MedWorm.com provides a medical RSS filtering service. Over 6000 RSS medical sources are combined and output via different filters. This feed contains the latest items from the 'Acta Crystallographica Section C' source. Thu, 09 Feb 2012 13:01:23 +0100 http://www.medworm.com/index.php?rid=5655925&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgg3269 The title compound, C48H20F19N4O3P, prepared by the nucleophilic attack of triethyl phosphite on one of the 4-fluoro atoms of 5,10,15,20-tetrakis(pentafluorophenyl)porphyrin, contains a single molecule in the asymmetric unit. The porphyrin unit is almost planar [largest non-H atom deviation = 0.174 (6) Å], and has the planes of the neighbouring benzene rings oriented at angles ranging from 64.3 (2) to 89.6 (3)° relative to the porphyrin core. The P=O group is almost coplanar with the attached benzene ring, subtending an angle of 4.0 (3)°. Several weak supramolecular interactions, namely C—H...Ï€, C—F...Ï€, P=O...Ï€, C—H...(O,F) and F...F contacts, contribute to the crystal packing. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655925 Fri, 03 Feb 2012 17:54:40 +0100 5655925 http://www.medworm.com/index.php?rid=5655924&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fwq3009 Dimethyl (3,4-dichlorobenzoyl)carbonohydrazonodithioate, C10H10Cl2N2OS2, (D1), dibenzyl (3,4-dichlorobenzoyl)carbonohydrazonodithioate, C22H18Cl2N2OS2, (D2), dimethyl (3,4-dichlorobenzoyl)-1-methylcarbonohydrazonodithioate, C11H12Cl2N2OS2, (D3), 3,4-dichloro-N′-(1,3-dithiolan-2-ylidene)-N-methylbenzohydrazide, C11H10Cl2N2OS2, (D4), were synthesized as potential tuberculostatics. Compound (D1) (with two molecules in the asymmetric unit) was the only one showing tuberculostatic activity of the same range as the common drugs isoniazid and pyrazinamide. The molecular structures of the studied compounds depend on the substitution at the N atom adjacent to the carbonyl group. In the case of the unsubstituted derivatives (D1) and (D2), their central frames are generally planar with a twist of t... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655924 Fri, 03 Feb 2012 17:54:40 +0100 5655924 http://www.medworm.com/index.php?rid=5655923&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3033 The structure of the title compound, [U(C14H9N3O2)O2(CH3OH)2]·CH3OH, is the first to be reported for an actinide complex including triazole ligands. The UVI atom exhibits a pentagonal–bipyramidal NO6 coordination environment, involving two axial oxide ligands [U=O = 1.766 (3) and 1.789 (3) Å], four equatorial O atoms [U—O = 2.269 (3)–2.448 (3) Å] from the ligand and the two coordinated methanol molecules, and one equatorial N atom [U—N = 2.513 (4) Å] from the ligand. In the crystal structure, the complex molecules are linked via intermolecular N—H...O and O—H...O hydrogen bonds to form a two-dimensional structure. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655923 Fri, 03 Feb 2012 17:54:40 +0100 5655923 http://www.medworm.com/index.php?rid=5655922&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3269 A novel CdII metal–organic framework, [Cd(C3H2O4)(NH3)]n, was synthesized by liquid diffusion conducted in the presence of ammonia. The CdII atom has seven-coordinate O6N pentagonal–bipyramidal geometry. Six CdII centers are joined by six malonate ligands to form an S6-symmetric [Cd6(malonate)6] metallomacrocycle, which is further extended through a side-on chelating malonate ligand to form a three-dimensional network. Topologically, each CdII center is connected to four others to yield an infinite three-periodic four-coordinated SOD (sodalite) network with point symbol {42·64}. The overall network structure in the crystal is maintained and stabilized by the presence of N—H...O hydrogen bonds. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655922 Fri, 03 Feb 2012 17:54:40 +0100 5655922 http://www.medworm.com/index.php?rid=5655921&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3062 The asymmetric unit of the title compound, {[La(C4H5O2)3(H2O)2]·C5H5N5·H2O}n, consists of an LaIII cation, three crotonate (but-2-enoate) anions and two coordinated water molecules forming the neutral complex, completed by an external adenine molecule and one hydration water molecule. The LaO10 coordination polyhedra, connected through the sharing of a single edge, form isolated chains running along the [100] direction. These one-dimensional structures are characterized by two different centrosymmetric La2O2 loops, with La...La distances of 4.5394 (6) and 4.5036 (6) Å. The unbound adenine and water solvent molecules form a highly planar hydrogen-bonded array parallel to (110) (r.m.s. deviation from the mean plane (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655921 Fri, 03 Feb 2012 17:54:40 +0100 5655921 http://www.medworm.com/index.php?rid=5655920&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3029 The title phase, first detected in the early 1980s but hitherto unpublished, has been resynthesized and structurally characterized. Unambiguous determination of the chemical composition was not possible by structure analysis alone, but required additional analytical methods. The complex structure shows a close similarity to the structures of two related compounds, one known by the formula Pb1.6In8Bi4S19 and the other being the ternary compound Pb6In10S21. This is despite the fact that the three phases correspond to very different Pb:Bi ratios. A geometric mechanism is described by which the three structures can be transformed into each other, provided that the heavy atoms Pb and Bi are treated as equivalent. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655920 Fri, 03 Feb 2012 17:54:40 +0100 5655920 http://www.medworm.com/index.php?rid=5655919&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3063 Work on the ternary Ni–Sn–Zn phase diagram revealed the existence of the title compound pentanickel tetratin zinc, Ni3.17Sn2.67Zn0.67 [Schmetterer et al. (2012). Intermetallics, doi:10.1016/j.intermet.2011.05.025]. It crystallizes in the Ni5Ga3Ge2 structure type (orthorhombic, Cmcm) and is related to the InNi2 type (hexagonal, P63/mmc) of the neighbouring Ni3Sn2 high-temperature (HT) phase, but is not a superstructure. The crystal structure was determined using single-crystal X-ray diffraction. Its homogeneity range was characterized using electron microprobe analysis. Phase analysis at various temperatures indicated that the phase decomposes between 1073 and 1173 K, where a more extended ternary solid solution of the Ni3Sn2 HT phase was found instead. (Source: Acta Crystallographica... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5655919 Fri, 03 Feb 2012 17:54:40 +0100 5655919 http://www.medworm.com/index.php?rid=5634980&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fky3008 Owing to increasing interest in the use of N-heterocyclic carbenes (NHCs) based on imidazolidinium ions as ligands in the design of highly efficient transition-metal-based homogeneous catalysts, the characterizations of the 1-ferrocenylmethyl-3-(2,4,6-trimethylbenzyl)imidazolidin-3-ium iodide salt, [Fe(C5H5)(C19H24N2)]I, (I), and the palladium complex trans-bis(3-benzyl-1-ferrocenylmethyl-1H-imidazolidin-2-ylidene)diiodidopalladium(II), [Fe2Pd(C5H5)2(C16H17N2)2I2], (II), are reported. Compound (I) has two iodide anions and two imidazolidinium cations within the asymmetric unit (Z′ = 2). The two cations have distinctly different conformations, with the ferrocene groups orientated exo and endo with respect to the N-heterocyclic carbene. Weak C—H donor hydrogen bonds to both the iodide an... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5634980 Wed, 25 Jan 2012 05:00:00 +0100 5634980 http://www.medworm.com/index.php?rid=5634979&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fwq3010 The title compound, {[Cu(NH3)4][Cu(CN)3]2}n, features a CuI–CuII mixed-valence CuCN framework based on {[Cu2(CN)3]−}n anionic layers and [Cu(NH3)4]2+ cations. The asymmetric unit contains two different CuI ions and one CuII ion which lies on a centre of inversion. Each CuI ion is coordinated to three cyanide ligands with a distorted trigonal–planar geometry, while the CuII ion is ligated by four ammine ligands, with a distorted square-planar coordination geometry. The interlinkage between CuI ions and cyanide bridges produces a honeycomb-like {[Cu2(CN)3]−}n anionic layer containing 18-membered planar [Cu(CN)]6 metallocycles. A [Cu(NH3)4]2+ cation fills each metallocyclic cavity within pairs of exactly superimposed {[Cu2(CN)3]−}n anionic layers, but there are no cations between th... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5634979 Wed, 25 Jan 2012 05:00:00 +0100 5634979 http://www.medworm.com/index.php?rid=5634978&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgg3267 The rigid organic ligand (pyridine-3,5-diyl)diphosphonic acid has been used to create the title novel three-dimensional coordination polymer, [Ca(C5H6NO6P2)2(H2O)]n. The six-coordinate calcium ion is in a distorted octahedral environment, formed by five phosphonate O atoms from five different (pyridin-1-ium-3,5-diyl)diphosphonate ligands, two of which are unique, and one water O atom. Two crystallographically independent acid monoanions, L1 and L2, serve to link metal centres using two different coordination modes, viz. η2μ2 and η3μ3, respectively. The latter ligand, L2, forms a strongly undulated two-dimensional framework parallel to the crystallographic bc plane, whereas the former ligand, L1, is utilized in the formation of one-dimensional helical chains in the [010] direction. The ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5634978 Wed, 25 Jan 2012 05:00:00 +0100 5634978 http://www.medworm.com/index.php?rid=5603502&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3419 Hydantoin-5-acetic acid [2-(2,5-dioxoimidazolidin-4-yl)acetic acid] and orotic acid (2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylic acid) each contain one rigid acceptor–donor–acceptor hydrogen-bonding site and a flexible side chain, which can adopt different conformations. Since both compounds may be used as coformers for supramolecular complexes, they have been crystallized in order to examine their conformational preferences, giving solvent-free hydantoin-5-acetic acid, C5H6N2O4, (I), and three crystals containing orotic acid, namely, orotic acid dimethyl sulfoxide monosolvate, C5H4N2O4·C2H6OS, (IIa), dimethylammonium orotate–orotic acid (1/1), C2H8N+·C5H3N2O4−·C5H4N2O4, (IIb), and dimethylammonium orotate–orotic acid (3/1), 3C2H8N+·3C5H3N2O4−·C5H4N2O4, (IIc). The ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5603502 Wed, 18 Jan 2012 05:00:00 +0100 5603502 http://www.medworm.com/index.php?rid=5603501&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3160 The title salt, C6H12NO2+·C6H7O4− or ISO+·CBDC−, is an ionic ensemble assisted by hydrogen bonds. The amino acid moiety (ISO or piperidine-4-carboxylic acid) has a protonated ring N atom (ISO+ or 4-carboxypiperidinium), while the semi-protonated acid (CBDC− or 1-carboxycyclobutane-1-carboxylate) has the negative charge residing on one carboxylate group, leaving the other as a neutral –COOH group. The –+NH2– state of protonation allows the formation of a two-dimensional crystal packing consisting of zigzag layers stacked along a separated by van der Waals distances. The layers extend in the bc plane connected by a complex network of N—H...O and O—H...O hydrogen bonds. Wave-like ribbons, constructed from ISO+ and CBDC− units and described by the graph-set symbols C33(10) ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5603501 Wed, 18 Jan 2012 05:00:00 +0100 5603501 http://www.medworm.com/index.php?rid=5592247&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3265 Recrystallization of the title compound, [Fe(C5H5)(C14H13N2O3)], from a mixture of n-hexane and dichloromethane gave the new polymorph, denoted (I), which crystallizes in the same space group (P\overline{1}) as the previously reported structure, denoted (II). The Fe—C distances in (I) range from 2.015 (3) to 2.048 (2) Å and the average value of the C—C bond lengths in the two cyclopentadienyl (Cp) rings is 1.403 (13) Å. As indicated by the smallest C—Cg1—Cg2—C torsion angle of 1.4° (Cg1 and Cg2 are the centroids of the two Cp rings), the orientation of the Cp rings in (I) is more eclipsed than in the case of (II), for which the value was 15.3°. Despite the pronounced conformational similarity between (I) and (II), the formation of self-complementary N—H...O hydrog... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5592247 Sat, 14 Jan 2012 05:00:00 +0100 5592247 http://www.medworm.com/index.php?rid=5592248&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fmx3062 4-Hydroxypyridine and terephthalic acid cocrystallize as a hydrate, 4-pyridone–terephthalic acid–water (2/1/2), 2C5H5NO·C8H6O4·2H2O, from a methanol–water solution. The molecules form a two-dimensional hydrogen-bonded network resulting in sheets of hydrogen-bonded molecules that lie parallel to the (10\overline 2) plane. In contrast, 3-hydroxypyridine and terephthalic acid form the salt bis(3-hydroxypyridinium) terephthalate, 2C5H6NO+·C8H4O42−, giving rise to two-dimensional hydrogen-bonded sheets extending through the lattice parallel to the (10\overline 2) plane. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5592248 Thu, 12 Jan 2012 05:00:00 +0100 5592248 http://www.medworm.com/index.php?rid=5592246&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3010 Solvothermal reaction between Cd(NO3)2, 1,4-phenylenediacetate (1,4-PDA) and 1,3-bis(pyridin-4-yl)propane (bpp) afforded the title complex, [Cd(C10H8O4)(C13H14N2)]n. Adjacent carboxylate-bridged CdII ions are related by an inversion centre. The 1,4-PDA ligands adopt a cis conformation and connect the CdII ions to form a one-dimensional chain extending along the c axis. These chains are in turn linked into a two-dimensional network through bpp bridges. The bpp ligands adopt an anti–gauche conformation. From a topological point of view, each bpp ligand and each pair of 1,4-PDA ligands can be considered as linkers, while the dinuclear CdII unit can be regarded as a 6-connecting node. Thus, the structure can be simplified to a two-dimensional 6-connected network. (Source: Acta Crystallograph... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5592246 Tue, 10 Jan 2012 05:00:00 +0100 5592246 http://www.medworm.com/index.php?rid=5576375&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3264 Single crystals of lithium iron tungstate, LiFe(WO4)2, were obtained using a high-temperature solution growth method. The analysis was conducted using the monoclinic space group C2/c, with β = 90.597 (2)°, giving R1 = 0.0177. The Li and Fe atoms lie on twofold axes. The structure can also be refined using the orthorhombic space group Cmcm, giving slightly higher residuals. The experimental value of β and the residuals mitigate in favour of the monoclinic description of the structure. Calculated bond-valence sums for the present results are closer to expected values than those obtained using the results of a previously reported analysis of this structure. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576375 Mon, 09 Jan 2012 21:28:53 +0100 5576375 http://www.medworm.com/index.php?rid=5576385&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3422 The title compounds, 2-carbamoylguanidinium hydrogen fluorophosphonate, C2H7N4O+·HFO3P−, (I), 2-carbamoylguanidinium–hydrogen fluorophosphonate–hydrogen phosphite (1/0.76/0.24), C2H7N4O+·0.76HFO3P−·0.24H2O3P−, (II), and 2-carbamoylguanidinium–hydrogen fluorophosphonate–hydrogen phosphite (1/0.115/0.885), C2H7N4O+·0.115HFO3P−·0.885H2O3P−, (III), are isostructural with guanylurea hydrogen phosphite, C2H7N4O+·H2O3P− [Fridrichová, NÄ›mec, CísaÅ™ová & NÄ›mec (2010). CrystEngComm, 12, 2054–2056]. They constitute structures where the hydrogen phosphite anion has been fully or partially replaced by hydrogen fluorophosphonate. The title structures are the fourth example of isostructural compounds which differ by the presence of hydrogen fluorophosphonate and hydrogen ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576385 Fri, 06 Jan 2012 05:00:00 +0100 5576385 http://www.medworm.com/index.php?rid=5576384&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3423 , 2C2H7N4O+·FO3P2−·2H2O, are presented. Polymorph (I), crystallizing in the space group Pnma, is slightly less densely packed than polymorph (II), which crystallizes in Pbca. In (I), the fluorophosphonate anion is situated on a crystallographic mirror plane and the O atom of the water molecule is disordered over two positions, in contrast with its H atoms. The hydrogen-bond patterns in both polymorphs share similar features. There are O—H...O and N—H...O hydrogen bonds in both structures. The water molecules donate their H atoms to the O atoms of the fluorophosphonates exclusively. The water molecules and the fluorophosphonates participate in the formation of R44(10) graph-set motifs. These motifs extend along the a axis in each structure. The water molecules are also acceptors of ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576384 Fri, 06 Jan 2012 05:00:00 +0100 5576384 http://www.medworm.com/index.php?rid=5576383&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3420 Polymorph (Ia) of eldoral [5-ethyl-5-(piperidin-1-yl)barbituric acid or 5-ethyl-5-(piperidin-1-yl)-1,3-diazinane-2,4,6-trione], C11H17N3O3, displays a hydrogen-bonded layer structure parallel to (100). The piperidine N atom and the barbiturate carbonyl group in the 2-position are utilized in N—H...N and N—H...O=C hydrogen bonds, respectively. The structure of polymorph (Ib) contains pseudosymmetry elements. The two independent molecules of (Ib) are connected via N—H...O=C(4/6-position) and N—H...N(piperidine) hydrogen bonds to give a chain structure in the [100] direction. The hydrogen-bonded layers, parallel to (010), formed in the salt diethylammonium 5-ethyl-5-(piperidin-1-yl)barbiturate [or diethylammonium 5-ethyl-2,4,6-trioxo-5-(piperidin-1-yl)-1,3-diazinan-1-ide], C4H12N+·C1... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576383 Fri, 06 Jan 2012 05:00:00 +0100 5576383 http://www.medworm.com/index.php?rid=5576382&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3027 The title molecular salts, N2H5+·C7H5O3−·C7H6O3 and N2H5+·C11H7O3−·C11H8O3, are acid adducts containing a hydrazinium cation, one molecule of a deprotonated acid and one molecule of a neutral acid. The two compounds contain essentially identical hydrogen-bond networks between the hydrazinium cation and the acid molecules, which define closely comparable two-dimensional layers in the structures. The planes of the aromatic rings within both structures are approximately parallel and the layers are stacked with comparable intermolecular interactions. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576382 Fri, 06 Jan 2012 05:00:00 +0100 5576382 http://www.medworm.com/index.php?rid=5576381&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3072 The triclinic structure of the title compound, C6H8N+·H2PO4−, with three symmetry-independent structural units (Z′ = 3), is formed of separate organic and inorganic layers alternating along the b axis. The building blocks of the inorganic layer are deformed H2PO4 tetrahedra assembled into infinite ladders by short and hence strong hydrogen bonds. The anilinium cations forming the organic layer are not hydrogen bonded to one another, but they are anchored by four N—H...O crosslinks between the dihydrogen phosphate chains of adjacent ladders. Two H atoms of each –NH3 group then form one normal and one bifurcated N—H...O hydrogen bond to the P=O oxygens of two tetrahedra of one chain, while the third H atom is hydrogen bonded to the nearest O atom of an adjacent chain belonging to ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576381 Fri, 06 Jan 2012 05:00:00 +0100 5576381 http://www.medworm.com/index.php?rid=5576380&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3159 This article also reviews structures having a P(O)NH group, with the aim of finding similar three-centre hydrogen bonds in the packing of phosphoramidate compounds. This analysis shows that the factors affecting the preference of the above-mentioned O atom to act as a double H-atom acceptor are: (i) a higher number of H-atom donor sites relative to H-atom acceptor centres in molecules with P(=O)(NH)3, (N)P(=O)(NH)2, C(=O)NHP(=O)(NH)2 and (NH)2P(=O)OP(=O)(NH)2 groups, and (ii) the remarkable H-atom acceptability of this atom relative to the other acceptor centre(s) in molecules containing an OP(=O)(NH)2 group, with the explanation that the N atom bound to the P atom in almost all of the structures found does not take part in hydrogen bonding as an acceptor. Moreover, the differences in the ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576380 Fri, 06 Jan 2012 05:00:00 +0100 5576380 http://www.medworm.com/index.php?rid=5576379&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3426 2-Ammonio-5-chloro-4-methylbenzenesulfonate, C7H8ClNO3S, (Ia), is an intermediate in the synthesis of lake red azo pigments. The present structure determination from single-crystal data confirms the results of a previous powder diffraction determination [Bekö, Thoms, Brüning, Alig, van de Streek, Lakatos, Glaubitz & Schmidt (2010). Z. Kristallogr. 225, 382–387]. The zwitterionic tautomeric form is confirmed. During a polymorph screening, two additional pseudopolymorphs were obtained, viz. 2-ammonio-5-chloro-4-methylbenzenesulfonate 1-methyl-2-pyrrolidone monosolvate, C7H8ClNO3S·C5H9NO, (Ib), and 2-ammonio-5-chloro-4-methylbenzenesulfonate dimethyl sulfoxide monosolvate, C7H8ClNO3S·C2H6OS, (Ic). The molecules of (Ib) have crystallographic m symmetry. The 1-methyl-2-pyrrolidone solvent... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576379 Fri, 06 Jan 2012 05:00:00 +0100 5576379 http://www.medworm.com/index.php?rid=5576378&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fcu3008 The structure of the metastable form I polymorph of the macrolide antibiotic clarithromycin, C38H69NO13, was determined by a powder diffraction method using synchrotron radiation. The space group of form I is P21212. The initial model was determined by a molecular replacement method using the structure of clarithromycin form 0 as a search model, and the final structure was obtained through Rietveld refinements. In the form I crystal structure, the clarithromycin molecules are aligned parallel along the a axis in a head-to-tail manner with intermolecular hydrogen bonds between the hydroxy O atoms. The dimethylamine groups of the clarithromycin molecule interdigitate between neighbouring head-to-tail clarithromycin alignments. The novel crystal packing found in form I provides a mechanism th... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576378 Fri, 06 Jan 2012 05:00:00 +0100 5576378 http://www.medworm.com/index.php?rid=5576377&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3074 Crystals of molecular complexes of dimethyl sulfoxide with trichloromethane (chloroform), (CH3)2SO·2CHCl3, (I), and dichloromethane, (CH3)2SO·CH2Cl2, (II), have been grown in situ. In both compounds, the components are linked together by (Cl)C—H...O interactions. The dimethyl sulfoxide molecules in (I) are bound into chains by C—H...O interactions. In (II), pairs of the components form centrosymmetric rings, linked into a three-dimensional network by C—H...O contacts and dipole–dipole interactions between dimethyl sulfoxide molecules. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576377 Fri, 06 Jan 2012 05:00:00 +0100 5576377 http://www.medworm.com/index.php?rid=5576376&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgz3204 Three alkaline earth metal salts of phenylacetic acid were examined and all were found to have similar structural types to analogous salts of benzoic and halobenzoic acids. Thus, a synchrotron study shows that the cations in catena-poly[[[tetraaquamagnesium(II)]-μ-phenylacetato-κ2O:O′] phenylacetate], {[Mg(C8H7O2)(H2O)4](C8H7O2)}n, form a one-dimensional coordination polymer that propagates through Mg—O—C—O—Mg interactions involving both crystallographically independent Mg centres (Z′ = 2) and through translation along the a axis. The polymeric chains pack to give alternate inorganic layers and organic bilayers. The Ca and Sr species catena-poly[[[diaqua(phenylacetato-κ2O,O′)calcium(II)]-μ3-phenylacetato-1′:1:1′′κ4O:O,O′:O′] monohydrate], {[Ca(C8H7O2)2(H2O)2]·... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5576376 Fri, 06 Jan 2012 05:00:00 +0100 5576376 http://www.medworm.com/index.php?rid=5542040&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fme0468 (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542040 Mon, 26 Dec 2011 06:13:26 +0100 5542040 http://www.medworm.com/index.php?rid=5542047&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3010 Crystals of bis(2-ethyl-3-hydroxy-6-methylpyridinium) succinate–succinic acid (1/1), C8H12NO+·0.5C4H4O42−·0.5C4H6O4, (I), and 2-ethyl-3-hydroxy-6-methylpyridinium hydrogen succinate, C8H12NO+·C4H5O4−, (II), were obtained by reaction of 2-ethyl-6-methylpyridin-3-ol with succinic acid. The succinate anion and succinic acid molecule in (I) are located about centres of inversion. Intermolecular O—H...O, N—H...O and C—H...O hydrogen bonds are responsible for the formation of a three-dimensional network in the crystal structure of (I) and a two-dimensional network in the crystal structure of (II). Both structures are additionally stabilized by π–π interactions between symmetry-related pyridine rings, forming a rod-like cationic arrangement for (I) and cationic dimers for (II).... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542047 Fri, 23 Dec 2011 05:00:00 +0100 5542047 http://www.medworm.com/index.php?rid=5542046&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffn3092 Chloroform was found to occupy the lattice of the protonated porphyrin and to promote crystallization of a different polymorphic form of a metalloporphyrin. The structure of 5,10,15,20-tetraphenylporphyrin-21,23-diium dichloride chloroform octasolvate, C44H32N42+·2Cl−·8CHCl3, (I), in the solid state is described and compared with related solvates. The porphyrin macrocycle displays a distorted saddle shape, with chloride anions above and below the ring. Seven chloroform molecules are bound via C—H...Cl hydrogen bonds, while the link with the eighth solvent molecule is weaker. A new monoclinic polymorph of (5,10,15,20-tetraphenylporphyrinato)copper(II), [Cu(C44H28N4)], (II), crystallized from chloroform, is also presented. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542046 Fri, 23 Dec 2011 05:00:00 +0100 5542046 http://www.medworm.com/index.php?rid=5542045&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fdt3009 Colourless crystals of the title compound, [Cd2(C7H4IO2)4(C12H10N2)(H2O)2]n, were obtained by the self-assembly of Cd(NO3)2·4H2O, 1,2-bis(pyridin-4-yl)ethene (bpe) and 4-iodobenzoic acid (4-IBA). Each CdII atom is seven-coordinated in a pentagonal–bipyramidal coordination environment by four carboxylate O atoms from two different 4-IBA ligands, two O atoms from two water molecules and one N atom from a bpe ligand. The CdII centres are bridged by the aqua molecules and bpe ligands, which lie across centres of inversion, to give a two-dimensional net. Topologically, taking the CdII atoms as nodes and the μ-aqua and μ-bpe ligands as linkers, the two-dimensional structure can be simplified as a (6,3) network. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542045 Fri, 23 Dec 2011 05:00:00 +0100 5542045 http://www.medworm.com/index.php?rid=5542044&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3030 The triclinic structure of the title compound, cyclo-tetrakis(μ-1,1-dioxo-1λ6,2-benzothiazole-3-thiolato-κ2S:S)tetrakis[(triphenylphosphane-κP)silver(I)], [Ag4(C7H4NO2S2)4(C18H15P)4], is a polymorph of the previously reported monoclinic structure [Dennehy, Mandolesi, Quinzani & Jennings (2007). Z. Anorg. Allg. Chem. 633, 2746–2752]. In both polymorphs, the complex lies on a crystallographic inversion centre and the bond distances are closely comparable. Some differences can be found in the interatomic angles and torsion angles involving the inner Ag4S4 skeleton. The polymorphs contain essentially identical two-dimensional layers, but with different layer stacking arrangements. In the triclinic form, all layers are related by lattice translation, while in the monoclinic form they are ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542044 Fri, 23 Dec 2011 05:00:00 +0100 5542044 http://www.medworm.com/index.php?rid=5542043&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3028 The title compound, MgCl2·4H2O, was crystallized at 403 K and its structure determined at 200 K. The structure is built up from MgCl2(H2O)4 octahedra with a trans configuration. Each complex is situated on a crystallographic twofold axis, with the rotation axis aligned along one H2O—Mg—OH2 axis. They are connected by a complex network of O—H...Cl hydrogen bonds. The structure contains two-dimensional sections that are essentially identical to those in the reported tetrahydrates of CrCl2, FeCl2, FeBr2 and CoBr2, but they are stacked in a different manner in MgCl2·4H2O compared with the transition metal structures. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542043 Fri, 23 Dec 2011 05:00:00 +0100 5542043 http://www.medworm.com/index.php?rid=5542042&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3070 The asymmetric unit of the title compound, lead(II) dicalcium octaaluminate, contains one Pb, one Ca, four Al and eight O atoms, with the Pb atom and one O atom situated on mirror planes. Three Al atoms exhibit slightly distorted tetrahedral coordinations with a mean Al—O bond length of 1.76 Å. The fourth Al atom is in a considerably distorted trigonal–bipyramidal coordination with a mean Al—O bond length of 1.89 Å. One AlO4 tetrahedron forms infinite chains parallel to [100] via corner-sharing. These chains are linked by parallel chains of edge-sharing AlO5 trigonal bipyramids into layers A of six-membered double rings extending parallel to (010). The second layer B is made up of the remaining two AlO4 tetrahedra. These tetrahedra share corners, resulting in likewise six-membe... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542042 Fri, 23 Dec 2011 05:00:00 +0100 5542042 http://www.medworm.com/index.php?rid=5542041&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fme0460 (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5542041 Thu, 22 Dec 2011 05:00:00 +0100 5542041 http://www.medworm.com/index.php?rid=5520137&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffn3087 (Acetonitrile-1κN)[μ-1H-benzimidazole-2(3H)-thione-1:2κ2S:S][1H-benzimidazole-2(3H)-thione-2κS]bis(μ-1,1-dioxo-1λ6,2-benzothiazole-3-thiolato)-1:2κ2S3:N;1:2κ2S3:S3-dicopper(I)(Cu—Cu), [Cu2(C7H4NO2S2)2(C7H6N2S)2(CH3CN)] or [Cu2(tsac)2(Sbim)2(CH3CN)] [tsac is thiosaccharinate and Sbim is 1H-benzimidazole-2(3H)-thione], (I), is a new copper(I) compound that consists of a triply bridged dinuclear Cu—Cu unit. In the complex molecule, two tsac anions and one neutral Sbim ligand bind the metals. One anion bridges via the endocyclic N and exocyclic S atoms (μ-S:N). The other anion and one of the mercaptobenzimidazole molecules bridge the metals through their exocyclic S atoms (μ-S:S). The second Sbim ligand coordinates in a monodentate fashion (κS) to one Cu atom, while an acetonitr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520137 Tue, 13 Dec 2011 05:00:00 +0100 5520137 http://www.medworm.com/index.php?rid=5520140&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3425 A crystallization series of tizanidine hydrochloride, used as a muscle relaxant for spasticity acting centrally as an α2-adrenergic agonist, yielded single crystals of the free base and the hydrochloride salt. The crystal structures of tizanidine [systematic name: 5-chloro-N-(imidazolidin-2-ylidene)-2,1,3-benzothiadiazol-4-amine], C9H8ClN5S, (I), and tizanidine hydrochloride {systematic name: 2-[(5-chloro-2,1,3-benzothiadiazol-4-yl)amino]imidazolidinium chloride}, C9H9ClN5S+·Cl−, (II), have been determined. Tizanidine crystallizes with two almost identical molecules in the asymmetric unit (r.m.s. deviation = 0.179 Å for all non-H atoms). The molecules are connected by N—H...N hydrogen bonds forming chains running along [2\overline{1}1]. The present structure determination corrects... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520140 Fri, 09 Dec 2011 05:00:00 +0100 5520140 http://www.medworm.com/index.php?rid=5520139&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Feg3079 The title compounds, C66H46, (I), and C66H42F4, (II), are polyphenylated arylenes synthesized by one-step Diels–Alder cycloaddition reactions. In both structures, all molecules lie on crystallographic inversion centers. In the case of (I), there are two half-molecules present in the asymmetric unit, (IA) and (IB); the geometry of each half-molecule differs principally in the magnitudes of the dihedral angles between mean planes fitted through the central aryl ring and the pendant phenyl rings. The crystal used was a non-merohedral twin, with a refined twin scale factor of 0.460 (8). The dihedral angle between the plane of the central tetrafluorinated ring and the adjacent tetraphenylated ring in (II) is 83.87 (4)°, significantly greater than the dihedral angles of 49.89 (12) and 5... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520139 Fri, 09 Dec 2011 05:00:00 +0100 5520139 http://www.medworm.com/index.php?rid=5520138&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3263 In the crystal structure of the title compound, C20H18N2O2S, molecules are linked by bifurcated C—H...O hydrogen-bond interactions, giving rise to chains whose links are composed of alternating centrosymmetrically disposed pairs of molecules and characterized by R22(10) and R22(20) hydrogen-bonding motifs. Also, N—H...S hydrogen bonds form infinite zigzag chains along the [010] direction, which exhibit the C(4) motif. Hirshfeld surface and fingerprint plots were used to explore the intermolecular interactions in the crystal structure. This analysis confirms the important role of C—H...O hydrogen bonds in the molecular conformation and in the crystal structure, providing a potentially useful tool for a full understanding of the intermolecular interactions in acylthiourea derivatives. ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520138 Fri, 09 Dec 2011 05:00:00 +0100 5520138 http://www.medworm.com/index.php?rid=5520136&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3009 4-Hydroxypyridine-2,6-dicarboxylic acid (chelidamic acid, cdaH3) reacts with MnCl2·2H2O in the presence of 2-amino-4-methylpyrimidine in water to afford the tetranuclear title complex, [Mn4(C8H3NO5)4(H2O)10]·3.34H2O, built through carboxylate bridging. The tetranuclear complex sits on a centre of inversion at (1 \over 2, 1 \over 2, 1 \over 2). In the crystal, discrete undecameric (H2O)10.34 water clusters (involving both coordinated and uncoordinated water molecules, with one site of an uncoordinated water molecule not fully occupied) assemble these tetranuclear MnII complex units via an intricate array of hydrogen bonding into an overall three-dimensional network. The degree of structuring of the (H2O)10.34 supramolecular association of water molecules observed in the present compound, ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520136 Fri, 09 Dec 2011 05:00:00 +0100 5520136 http://www.medworm.com/index.php?rid=5520135&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3053 , poly[μ3-succinato-calcium(II)], [Ca(C4H5O4)]n, was synthesized by reaction of CaCl2·2H2O and succinic acid in an aqueous medium under hydrothermal microwave conditions. The structure contains infinite layers of edge-sharing calcium pentagonal–bipyramidal polyhedra forming six-membered rings connected through succinate ligands. Such an assembly of inorganic building units is unique for calcium metal–organic framework-type structures. Adjacent layers are packed into a final pseudo-three-dimensional structure through weak C—H...O hydrogen bonds. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5520135 Fri, 09 Dec 2011 05:00:00 +0100 5520135 http://www.medworm.com/index.php?rid=5482579&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3424 The molecule of the title compound, [AuCl(C27H36N2)], which belongs to a class of potentially catalytically active N-heterocyclic carbene complexes, has crystallographic C2 symmetry and approximate C2v symmetry. The structure is isostructural with the CuI and AgI analogues. A previous report of the structure of the title compound as its toluene solvate [Fructos et al. (2005). Angew. Chem. Int. Ed. 44, 5284–5288] has inaccurate geometry for the complex molecule as a consequence of probable incorrect refinement in the space group Cc, instead of C2/c [Marsh (2009). Acta Cryst. B65, 782–783]. The Au—C bond length of 1.998 (4) Å in the title compound is more consistent with the mean distance of 1.979 (14) Å found in 52 other reported [AuCl(carbene)] complexes than with the short... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5482579 Thu, 08 Dec 2011 06:52:23 +0100 5482579 http://www.medworm.com/index.php?rid=5482582&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3009 Six closely related pyrazolo[3,4-b]pyridine derivatives, namely 6-chloro-3-methyl-1,4-diphenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C20H14ClN3O, (I), 6-chloro-3-methyl-4-(4-methylphenyl)-1-phenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C21H16ClN3O, (II), 6-chloro-4-(4-chlorophenyl)-3-methyl-1-phenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C20H13Cl2N3O, (III), 4-(4-bromophenyl)-6-chloro-3-methyl-1-phenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C20H13BrClN3O, (IV), 6-chloro-4-(4-methoxyphenyl)-3-methyl-1-phenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C21H16ClN3O2, (V), and 6-chloro-3-methyl-4-(4-nitrophenyl)-1-phenylpyrazolo[3,4-b]pyridine-5-carbaldehyde, C20H13ClN4O3, (VI), which differ only in the identity of a single small substituent on one of the aryl rings, crystallize in four different ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5482582 Tue, 06 Dec 2011 05:00:00 +0100 5482582 http://www.medworm.com/index.php?rid=5482581&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ftp3005 Methyl β-d-galactopyranosyl-(1→4)-β-d-xylopyranoside, C12H22O10, (II), crystallizes as colorless needles from water with positional disorder in the xylopyranosyl (Xyl) ring and no water molecules in the unit cell. The internal glycosidic linkage conformation in (II) is characterized by a ϕ′ torsion angle (C2′Gal—C1′Gal—O1′Gal—C4Xyl) of 156.4 (5)° and a ψ′ torsion angle (C1′Gal—O1′Gal—C4Xyl—C3Xyl) of 94.0 (11)°, where the ring atom numbering conforms to the convention in which C1 denotes the anomeric C atom, and C5 and C6 denote the hydroxymethyl (–CH2OH) C atoms in the β-Xyl and β-Gal residues, respectively. By comparison, the internal linkage conformation in the crystal structure of the structurally related disaccharide, methyl β-lactoside [methy... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5482581 Tue, 06 Dec 2011 05:00:00 +0100 5482581 http://www.medworm.com/index.php?rid=5482580&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3004 Weakly diffracting crystals of benz[cd]indol-2(1H)-one (naphtholactam), C11H7NO, were unsuitable for data collection by early photographic methods. However, a diffractometer data set collected at room temperature in 1989 was solved and refined. The peak scans were broad, and the results indicated disorder or a satellite crystal. Recent data collection (on another crystal from the same sample) with an area detector at 100 K revealed the same disorder, and made it possible to refine two different, more complete, disorder models. Both models assume an occasional 180° rotation of the nearly planar centrosymmetric cis-lactam dimer. The refinements differ, especially in the anisotropic displacement parameters for the –C(=O)—NH– portion of the molecule. Both models at 100 K give a C—... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5482580 Tue, 06 Dec 2011 05:00:00 +0100 5482580 http://www.medworm.com/index.php?rid=5464714&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fme0465 (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5464714 Fri, 02 Dec 2011 07:05:10 +0100 5464714 http://www.medworm.com/index.php?rid=5464717&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fov3009 The title salt, (C2H8NO3S)[SbF6], which contains the protonated form of taurine (2-aminoethanesulfonic acid), was synthesized in anhydrous hydrofluoric acid and recrystallized as colourless block-shaped crystals from liquid SO2. In the solid state, a three-dimensional network is observed. This is formed by intra- and intermolecular N—H...O, N—H...F and O—H...F hydrogen bonds. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5464717 Wed, 30 Nov 2011 05:00:00 +0100 5464717 http://www.medworm.com/index.php?rid=5464716&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3235 The title compound, {(C3H10N)4[Ni3Cl10]}n, contains zigzag layers of tri-μ-chlorido-bridged linear 2/m-symmetric Ni3Cl12 segments, linked by mono-μ-chlorido quasi-linear bridges to two other segments at each end. These inorganic layers are interleaved with interdigitated bilayers of mirror-symmetric n-propylammonium cations, the ammonium head groups of which are directed into the inorganic layers to form multiple N—H...Cl hydrogen bonds, while the propyl tail groups pack together in a tongue-and-groove manner in the center of the bilayer. The propyl groups are ordered at 100 K but disordered with opposite conformations on the mirror plane at 240 K. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5464716 Wed, 30 Nov 2011 05:00:00 +0100 5464716 http://www.medworm.com/index.php?rid=5464715&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffn3089 In the complex salt [η6-1-chloro-2-(pyrrolidin-1-yl)benzene](η5-cyclopentadienyl)iron(II) hexafluoridophosphate, [Fe(C5H5)(C10H12ClN)]PF6, (I), the complexed cyclopentadienyl and benzene rings are almost parallel, with a dihedral angle between their planes of 2.3 (3)°. In a related complex salt, (η5-cyclopentadienyl){2-[η6-2-(pyrrolidin-1-yl)phenyl]phenol}iron(II) hexafluoridophosphate, [Fe(C5H5)(C16H17NO)]PF6, (II), the analogous angle is 5.4 (1)°. In both complexes, the aromatic C atom bound to the pyrrolidine N atom is located out of the plane defined by the remaining five ring C atoms. The dihedral angles between the plane of these five ring atoms and a plane defined by the N-bound aromatic C atom and two neighboring C atoms are 9.7 (8) and 5.6 (2)° for (I) and (II), res... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5464715 Wed, 30 Nov 2011 05:00:00 +0100 5464715 http://www.medworm.com/index.php?rid=5447183&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3057 New ternary dodecalithium dodecacopper tetradecaaluminium, Li12Cu12.60Al14.37 (trigonal, R\overline{3}m, hR39), crystallizes as a new structure type and belongs to the structural family that derives from binary Laves phases. The Li atoms are enclosed in 15- and 16-vertex and the Al3 atom in 14-vertex pseudo-Frank–Kasper polyhedra. The polyhedra around the statistical mixtures of (Cu,Al)1 and (Al,Cu)2 are distorted icosahedra. The electronic structure was calculated by the TB–LMTO–ASA (tight-binding linear muffin-tin orbital atomic spheres approximation) method. The electron localization function, which indicates bond formation, is mostly located at the Al atoms. Thus, Al—Al bonding is much stronger than Li—Al or Cu—Al bonding. This indicates that, besides metallic bonding which... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5447183 Sat, 26 Nov 2011 06:49:36 +0100 5447183 http://www.medworm.com/index.php?rid=5447184&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3112 Two polymorphs of 2,5-diphenyl-1,3,4-selenadiazole, C14H10N2Se, denoted (Ia) and (Ib), and a new polymorph of 2,5-bis(thiophen-2-yl)-1,3,4-selenadiazole, C10H6N2S2Se, (IIb), form on crystallization of the compounds, prepared using Woollins' reagent (2,4-diphenyl-1,3-diselenadiphosphetane 2,4-diselenide). These compounds, along with 2-(4-chlorophenyl)-5-phenyl-1,3,4-selenadiazole, C14H9ClN2Se, (III), and 2-(furan-2-yl)-5-(p-tolyl)-1,3,4-selenadiazole, C13H10N2OSe, (IV), show similar intermolecular interactions, with π–π stacking, C—H...Ï€ interactions and weak hydrogen bonds typically giving rise to molecular chains. However, the combination of interactions differs in each case, giving rise to different packing arrangements. In polymorph (Ib), the molecule lies across a crystallograph... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5447184 Sat, 26 Nov 2011 05:00:00 +0100 5447184 http://www.medworm.com/index.php?rid=5436941&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fuk3034 The title compound, C7H12N4O2, was obtained by nitrosation of the aminal cage (2R,7R,11S,16S)-1,8,10,17-tetraazapentacyclo[8.8.1.18,17.02,7.011,16]icosane. The crystal structure is a racemic mixture of RR and SS enantiomers. The asymmetric unit contains two crystallographically independent half-molecules, one having two partially occupied conformers with refined occupancy factors of 0.747 (3) and 0.253 (3). The molecules sit across twofold axes. The unique molecules each form chains parallel to [001], with molecules connected by intermolecular C—H...O hydrogen bonds. The bonding between adjacent chains is weak. The analysis of eight different crystals confirmed the presence of disordered and nondisordered molecules in the same structure as a regular feature. (Source: Acta Crystallogr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5436941 Tue, 22 Nov 2011 05:00:00 +0100 5436941 http://www.medworm.com/index.php?rid=5427740&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3233 In the four compounds of chloranilic acid (2,5-dichloro-3,6-dihydroxycyclohexa-2,5-diene-1,4-dione) with pyrrolidin-2-one and piperidin-2-one, namely, chloranilic acid–pyrrolidin-2-one (1/1), C6H2Cl2O4·C4H7NO, (I), chloranilic acid–pyrrolidin-2-one (1/2), C6H2Cl2O4·2C4H7NO, (II), chloranilic acid–piperidin-2-one (1/1), C6H2Cl2O4·C5H9NO, (III), and chloranilic acid–piperidin-2-one (1/2), C6H2Cl2O4·2C5H9NO, (IV), the shortest interactions between the two components are O—H...O hydrogen bonds, which act as the primary intermolecular interaction in the crystal structures. In (II), (III) and (IV), the chloranilic acid molecules lie about inversion centres. For (III), this necessitates the presence of two independent acid molecules. In (I), there are two formula units in the asymme... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5427740 Sat, 19 Nov 2011 05:00:00 +0100 5427740 http://www.medworm.com/index.php?rid=5427739&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3111 The structure of a previously unreported polymorph of anhydrous theophylline (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione), C7H8N4O2, has been determined at 100 K and shown to have monoclinic symmetry with Z′ = 2. The structure is named form IV and experimental observation indicates that this is the stable form of the material. The molecular packing consists of discrete hydrogen-bonded dimers similar to that observed in the monohydrate structure. The structure of form I has also been determined and consists of hydrogen-bonded chains. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5427739 Sat, 19 Nov 2011 05:00:00 +0100 5427739 http://www.medworm.com/index.php?rid=5427738&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3421 The title metal–organic framework, [Cd3(C12H9O6)2(C10H8N2)2]n, has been synthesized by a solvothermal reaction. The CdII ions are located in CdO4N2 and CdO6 six-coordinated environments, with the latter CdII ion lying on an inversion centre. The 2,4,6-trimethylbenzene-1,3,5-tricarboxylate ligand (TMBTC) connects the CdII ions to form a two-dimensional sheet incorporating hourglass-like [Cd3(COO)6] secondary building units (SBUs). Topologically, taking the TMBTC ligand and the [Cd3(COO)6] SBU as 3- and 6-connected nodes, respectively, the overall two-dimensional sheet can be simplified to a rare (3,6)-connected 2-nodal kgd (Kagomé dual) net with a short Schläfli vertex notation of {43}2{46.66.83}, which further stacks into a three-dimensional supramolecular framework through π–π sta... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5427738 Sat, 19 Nov 2011 05:00:00 +0100 5427738 http://www.medworm.com/index.php?rid=5416934&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3008 The title racemic heterometallic dinuclear compound, [MnSn(C2H2O2S)3(H2O)5], (I), contains one main group SnIV metal centre and one transition metal MnII centre, and, by design, links the MnII centre to the building unit of the (Δ/Λ) [SnL3]2− complex anion (L is the 2-sulfidoacetate dianion). In this cluster, the SnIV centre of the (Δ/Λ) [SnL3]2− unit is coordinated by three O atoms and three S atoms from three L ligands to form an [SnO3S3] octahedral coordination environment. The MnII centre is in an [MnO6] octahedral coordination environment, with five O atoms from five water molecules and the sixth from the μ2-L ligand of the (Δ/Λ) [SnL3]2− unit. Between adjacent dinuclear molecules, there are many hydrogen-bond interactions of O—H...O, O—H...S, C—H...O and C—H...S ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5416934 Wed, 16 Nov 2011 05:00:00 +0100 5416934 http://www.medworm.com/index.php?rid=5416933&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3054 Poly[bis(3,3′,5,5′-tetramethyl-4,4′-bi-1H-pyrazole-2,2′-diium) γ-octamolybdate(VI) dihydrate], {(C10H16N4)2[Mo8O26]·2H2O}n, (I), and bis(3,3′,5,5′-tetramethyl-4,4′-bi-1H-pyrazole-2,2′-diium) α-dodecamolybdo(VI)silicate tetrahydrate, (C10H16N4)2[SiMo12O40]·4H2O, (II), display intense hydrogen bonding between the cationic pyrazolium species and the metal oxide anions. In (I), the asymmetric unit contains half a centrosymmetric γ-type [Mo8O26]4− anion, which produces a one-dimensional polymeric chain by corner-sharing, one cation and one water molecule. Three-centre bonding with 3,3′,5,5′-tetramethyl-4,4′-bi-1H-pyrazole-2,2′-diium, denoted [H2Me4bpz]2+ [N...O = 2.770 (4)–3.146 (4) Å], generates two-dimensional layers that are further linked by hydrogen ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5416933 Wed, 16 Nov 2011 05:00:00 +0100 5416933 http://www.medworm.com/index.php?rid=5396030&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3006 The reaction of the μ3-oxido-centred trinuclear isobutyrate cluster [Fe3O(O2CCHMe2)6(H2O)3]+ with an excess of phenol (PhOH) in chloroform produces a novel octanuclear FeIII cluster, cyclo-tetra-μ2-hydroxido-dodeca-μ2-isobutyrato-κ24O:O′-octa-μ2-phenolato-κ16O:O′-octairon(III) phenol hexasolvate monohydrate, [Fe8(C4H7O2)12(C6H5O)8(OH)4]·6C6H5OH·H2O. The neutral cluster is located about a centre of inversion and consists of a planar ring of eight FeIII centres with two types of bridges between adjacent Fe atoms: each Fe atom is bridged to one of its neighbours by a μ-hydroxide and two 1,3-bridging carboxylates, or by two phenolate and one 1,3-bridging isobutyrate ligand. The cavity within the {Fe8} wheel is occupied by a disordered water molecule. Intermolecular O—H...O hydro... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396030 Fri, 11 Nov 2011 07:00:02 +0100 5396030 http://www.medworm.com/index.php?rid=5396035&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fuk3036 The title compound, C28H20N2O2, forms two conformational polymorphs, (I) and (II), where the molecular structures are similar except for the orientation of the two hydroxy groups. In (I), which was obtained by slow evaporation from chloroform, the two hydroxy groups have an anti conformation. The molecules form a sheet structure within the ac plane, where the hydroxy groups form zigzag hydrogen bonds. In (II), which was obtained by slow evaporation from acetonitrile, the two hydroxy groups have a syn conformation. The molecules form a double-sheet structure within the ab plane, where the hydroxy groups form 4-helix hydrogen bonds. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396035 Sat, 05 Nov 2011 04:00:00 +0100 5396035 http://www.medworm.com/index.php?rid=5396034&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3006 The X-ray crystal structures of solvates of sulfapyridine have been determined to be conformational polymorphs. 4-Amino-N-(1,2-dihydropyridin-2-ylidene)benzenesulfonamide (polymorph III), C11H11N3O2S, (1), 4-amino-N-(1,2-dihydropyridin-2-ylidene)benzenesulfonamide 1,3-dioxane monosolvate, C11H11N3O2S·C4H8O2, (2), and 4-amino-N-(1,2-dihydropyridin-2-ylidene)benzenesulfonamide tetrahydrofuran monosolvate, C11H11N3O2S·C4H8O, (3), crystallized as the imide form, while piperidin-1-ium 4-amino-N-(pyridin-2-yl)benzenesulfonamidate, C5H12N+·C11H10N3O2S−, (4), crystallized as the piperidinium salt. The tetrahydrofuran and dioxane solvent molecules in their respective structures were disordered and were refined using a disorder model. Three-dimensional hydrogen-bonding networks exist in all str... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396034 Sat, 05 Nov 2011 04:00:00 +0100 5396034 http://www.medworm.com/index.php?rid=5396033&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgg3264 Two polymorphs of 2,6-dichloropurine, C5H2Cl2N4, have been crystallized and identified as the 9H- and 7H-tautomers. Despite differences in the space group and number of symmetry-independent molecules, they exhibit similar hydrogen-bonding motifs. Both crystal structures are stabilized by intermolecular N—H...N interactions that link adjacent molecules into linear chains, and by some nonbonding contacts of the C—Cl...Ï€ type and by π–π stacking interactions, giving rise to a crossed two-dimensional herringbone packing motif. The main structural difference between the two polymorphs is the different role of the molecules in the π–π stacking interactions. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396033 Sat, 05 Nov 2011 04:00:00 +0100 5396033 http://www.medworm.com/index.php?rid=5396032&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3236 In 3-tert-butyl-1-(4-chlorophenyl)-4-phenylindeno[1,2-b]pyrazolo[4,3-e]pyridin-5(1H)-one, C29H22ClN3O, (I), inversion-related pairs of molecules are linked by C—H...O hydrogen bonds to form R22(18) dimers, which are themselves linked into a chain by a π–π stacking interaction between inversion-related pairs of molecules. In 3-tert-butyl-1-(4-chlorophenyl)-4-(4-methoxyphenyl)indeno[1,2-b]pyrazolo[4,3-e]pyridin-5(1H)-one, C30H24ClN3O2, (II), which crystallizes in the space group P\overline{1}, with Z′ = 2 and with different orientations for the methoxy groups in the two independent molecules, a combination of C—H...O and C—H...Ï€(arene) hydrogen bonds links the molecules into chains of rings, which are further linked into sheets by a π–π stacking interaction. (Source: Acta Cr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396032 Sat, 05 Nov 2011 04:00:00 +0100 5396032 http://www.medworm.com/index.php?rid=5396031&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fmx3053 The molecular geometry of the tetragonal crystal structure of the title compound, [Ru(NO2)2(C5H5N)4]·2H2O, differs from that previously determined by powder diffraction [Schaniel et al. (2010). Phys. Chem. Chem. Phys. 12, 6171–6178]. In the [Ru(NO2)(C5H5N)4] molecule, the Ru atom lies at the intersection of three twofold axes (Wyckoff position 8b). It is coordinated by four N atoms of the pyridine rings, as well as by two N atoms of N-nitrite groups. The last two N atoms are located on a twofold axis (Wyckoff position 16f). The O atoms of the water molecules are situated on a twofold axis (Wyckoff position 16e). Short intermolecular contacts are observed in the crystal structure, viz. N—O...OW and N—O...H—OW contacts between nitrite and water, and weak C—H...OW hydrogen bonds be... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5396031 Sat, 05 Nov 2011 04:00:00 +0100 5396031 http://www.medworm.com/index.php?rid=5354800&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Feg3076 Diels–Alder reaction between maleimides featuring 3,5-di-, 2,4,6-tri- and pentafluorinated N-phenyl substituents and anthracene yields the corresponding pentacyclic ethanoanthracenedicarboximide compounds, namely N-(3,5-difluorophenyl)-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboximide, C24H15F2NO2, (IIa), N-(2,4,6-trifluorophenyl)-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboximide, C24H14F3NO2, (IIb), N-(2,3,4,5,6-pentafluorophenyl)-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboximide, C24H12F5NO2, (IIc). The crystal structures of (IIa)–(IIc) reveal an expected molecular geometry with a `V'-shape of the anthracene-derived tricyclic moiety. The crystal packings of (IIa) and (IIb) are dominated by π–π and C—H...O/F interactions, while F...F and C—H...Ï€ contacts are ab... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5354800 Tue, 25 Oct 2011 04:00:00 +0100 5354800 http://www.medworm.com/index.php?rid=5354799&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fqs3005 The title compounds, trans-bis(1H-benzimidazole-2-carboxylato-κ2N3,O)bis(ethanol-κO)cadmium(II), [Cd(C8H5N2O2)2(C2H6O)2], (I), and trans-bis(1H-benzimidazole-κN3)bis(1H-benzimidazole-2-carboxylato-κ2N3,O)nickel(II), [Ni(C8H5N2O2)2(C7H6N2)2], (II), are hydrogen-bonded supramolecular complexes. In (I), the CdII ion is six-coordinated by two O atoms from two ethanol molecules, and by two O and two N atoms from two bidentate benzimidazole-2-carboxylate (HBIC) ligands, giving a distorted octahedral geometry. The combination of O—H...O and N—H...O hydrogen bonds results in two-dimensional layers parallel to the ab plane. In (II), the six-coordinated NiII atom, which lies on an inversion centre, shows a similar distorted octahedral geometry to the CdII ion in (I); two benzimidazole molecu... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5354799 Tue, 25 Oct 2011 04:00:00 +0100 5354799 http://www.medworm.com/index.php?rid=5343155&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3055 In the title polymeric compound, [Cu(C9H6O4)(C3H4N2)2]n, the copper(II) cation occupies an N2O3 coordination sphere defined by two 1H-imidazole (imid) ligands in trans positions and three carboxylate O atoms from three different 2-(carboxylatomethyl)benzoate (hpt2−) dianions. The geometry is that of a square pyramid with one of the O atoms at the apex, bridging neighbouring metal centres into an [–ON2CuO2CuN2O–] dinuclear unit. These units are in turn connected by hpt anions into a reticular mesh topologically characterized by two types of loops, viz. a four-membered Cu2O2 diamond motif and a 32-membered Cu4O8C20 ring. The imid groups do not take part in the formation of the two-dimensional structure, but take part in the N—H...O interactions. These arise only within individual pla... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5343155 Sat, 22 Oct 2011 04:00:00 +0100 5343155 http://www.medworm.com/index.php?rid=5320985&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3227 In the crystal structures of the conformational isomers hydrogen {phosphono[(pyridin-1-ium-3-yl)amino]methyl}phosphonate monohydrate (pro-E), C6H10N2O6P2·H2O, (Ia), and hydrogen {phosphono[(pyridin-1-ium-3-yl)amino]methyl}phosphonate (pro-Z), C6H10N2O6P2, (Ib), the related hydrogen {[(2-chloropyridin-1-ium-3-yl)amino](phosphono)methyl}phosphonate (pro-E), C6H9ClN2O6P2, (II), and the salt bis(6-chloropyridin-3-aminium) [hydrogen bis({[2-chloropyridin-1-ium-3-yl(0.5+)]amino}methylenediphosphonate)] (pro-Z), 2C5H6ClN2+·C12H16Cl2N4O12P42−, (III), chain–chain interactions involving phosphono (–PO3H2) and phosphonate (–PO3H−) groups are dominant in determining the crystal packing. The crystals of (Ia) and (III) comprise similar ribbons, which are held together by N—H...O interactio... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5320985 Sat, 15 Oct 2011 04:00:00 +0100 5320985 http://www.medworm.com/index.php?rid=5320982&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3109 The two isomorphous title compounds, [1,5,9-tris(2-aminoethoxy)-3,7,11-trihydroxy-3,7,11-tribora-1,5,9-triborata-2,4,6,8,10,12-hexaoxa-13-oxoniatricyclo[7.3.1.05,13]tridecane]cobalt(II), [Co(C6H21B6N3O13)] or Co{B6O7(OH)3[O(CH2)2NH2]3}, and the NiII analogue, [Ni(C6H21B6N3O13)], each consist of an MII cation and an inorganic–organic hybrid {B6O7(OH)3[O(CH2)2NH2]3}2− anion. The MII cation lies on a crystallographic threefold axis (as does one O atom) and is octahedrally coordinated by three N atoms from the organic component. Three O atoms covalently link the B–O cluster and the organic component. Molecules are connected to one another through N—H...O and O—H...O hydrogen bonds, forming a three-dimensional supramolecular network. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5320982 Sat, 15 Oct 2011 04:00:00 +0100 5320982 http://www.medworm.com/index.php?rid=5320984&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffn3090 The crystal structures of 4,5-bis(bromomethyl)-1,3-dithiol-2-one, C5H4Br2OS2, (I), and 4,5-bis[(dihydroxyphosphoryl)methyl]-1,3-dithiol-2-one, C5H8O7P2S2, (II), occur with similar unit cells in the same monoclinic space group. Both molecules reside on a twofold symmetry axis coincident with the C=O bond, so that the substituents in the 4- and 5-positions project above and below the plane of the 1,3-dithiol-2-one ring. In both structures, the molecules align themselves in a head-to-tail fashion along the b axis, and these rows of molecules then stack, with alternating directionality, along the c axis. For (II), an extensive network of intermolecular hydrogen bonds occurs between molecules within the same stack and between adjacent stacks. Each –CH2P(O)(OH)2 group participates in four hydr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5320984 Tue, 11 Oct 2011 04:00:00 +0100 5320984 http://www.medworm.com/index.php?rid=5320983&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3414 In order to investigate the relative stability of N—H...O and N—H...S hydrogen bonds, we cocrystallized the antithyroid drug 6-propyl-2-thiouracil with two complementary heterocycles. In the cocrystal pyrimidin-2-amine–6-propyl-2-thiouracil (1/2), C4H5N3·2C7H10N2OS, (I), the `base pair' is connected by one N—H...S and one N—H...N hydrogen bond. Homodimers of 6-propyl-2-thiouracil linked by two N—H...S hydrogen bonds are observed in the cocrystal N-(6-acetamidopyridin-2-yl)acetamide–6-propyl-2-thiouracil (1/2), C9H11N3O2·2C7H10N2OS, (II). The crystal structure of 6-propyl-2-thiouracil itself, C7H10N2OS, (III), is stabilized by pairwise N—H...O and N—H...S hydrogen bonds. In all three structures, N—H...S hydrogen bonds occur only within R22(8) patterns, whereas N—H...... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5320983 Tue, 11 Oct 2011 04:00:00 +0100 5320983 http://www.medworm.com/index.php?rid=5292440&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3110 The title compound, [Mg2(C12H14O4)2]n, is the first example of an s-block metal adamantanedicarboxylate coordination polymer. The asymmetric unit comprises two crystallographically unique MgII centers and two adamantane-1,3-dicarboxylate ligands. The compound is constructed from a combination of chains of corner-sharing magnesium-centered polyhedra, parallel to the a axis, connected by organic linkers to form a layered polymer. The two MgII centers are present in distorted tetrahedral and octahedral coordination environments derived from carboxylate O atoms. Tetrahedrally coordinated MgII centers have been reported in organometallic compounds, but this is the first time that such coordination has been observed in a magnesium-based coordination polymer. The bond valance sums of the two MgII... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5292440 Fri, 07 Oct 2011 06:00:26 +0100 5292440 http://www.medworm.com/index.php?rid=5292443&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3158 The conversion of myo-inositol to epi-inositol can be achieved by the hydride reduction of an intermediate epi-inosose derived from myo-inositol. (−)-epi-Inosose, (I), crystallized in the monoclinic space group P21, with two independent molecules in the asymmetric unit [Hosomi et al. (2000). Acta Cryst. C56, e584–e585]. On the other hand, (2RS,3SR,5SR,6SR)-epi-inosose, C6H10O6, (II), crystallized in the orthorhombic space group Pca21. Interestingly, the conformation of the molecules in the two structures is nearly the same, the only difference being the orientation of the C-3 and C-4 hydroxy H atoms. As a result, the molecular organization achieved mainly through strong O—H...O hydrogen bonding in the racemic and homochiral lattices is similar. The compound also follows Wallach's rul... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5292443 Thu, 06 Oct 2011 04:00:00 +0100 5292443 http://www.medworm.com/index.php?rid=5292442&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3416 Due to its donor–acceptor–donor site, the antimalarial drug pyrimethamine [systematic name: 5-(4-chlorophenyl)-6-ethylpyrimidine-2,4-diamine] is a potential component of a supramolecular synthon. During a cocrystallization screen, one new polymorph of solvent-free pyrimethamine, C12H13ClN4, (I), and two pseudopolymorphs, pyrimethamine dimethyl sulfoxide monosolvate, C12H13ClN4·C2H6OS, (Ia), and pyrimethamine N-methylpyrrolidin-2-one monosolvate, C12H13ClN4·C5H9NO, (Ib), were obtained. In (I), (Ia), (Ib) and the previously reported polymorph, the pyrimethamine molecules exhibit similar conformations and form R22(8) dimers stabilized by a pair of N—H...N hydrogen bonds. However, the packing arrangements are completely different. In (I), the dimers are connected by two additional N—... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5292442 Thu, 06 Oct 2011 04:00:00 +0100 5292442 http://www.medworm.com/index.php?rid=5292441&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3066 The title compound, C21H14N4O2S, belongs to a family of molecules possessing nonlinear optical properties in solution. Its structure has been solved from laboratory X-ray powder diffraction data using a new direct-space structure solution method, where the atomic coordinates are directly used as parameters and the molecular geometry is described by restraints. The molecular packing is controlled by two systems of π–π interactions and one weak edge-to-face interaction. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5292441 Thu, 06 Oct 2011 04:00:00 +0100 5292441 http://www.medworm.com/index.php?rid=5280949&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fem3044 The basic building unit in the structure of the title compound, C14H14FNO3, is pairs of molecules arranged in an antiparallel fashion, enabling weak C—H...O interactions. Each molecule is additionally involved in π–π interactions with neighbouring molecules. The pairs of molecules formed by the C—H...O hydrogen bonds and π–π interactions form ribbon-like chains running along the c axis. Theoretical calculations based on these pairs showed that, although the main intermolecular interaction is electrostatic, it is almost completely compensated by an exchange–repulsion contribution to the total energy. As a consequence, the dominating force is a dispersion interaction. The F atoms form weak C—F...H—C interactions with the H atoms of the neighbouring ethyl groups, with H...F ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280949 Thu, 29 Sep 2011 04:00:00 +0100 5280949 http://www.medworm.com/index.php?rid=5280948&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3157 The title compound, C9H14N+·CHB11Cl11−, was obtained in the course of our continuing studies of the low-melting salts of closo- and nido-carborane cage anions with alkylpyridinium and dialkylimidazolium cations. The title compound is the first example of a pyridinium salt of a perchlorinated carborane anion. The structure consists of one N-butylpyridinium cation counterbalanced by one perchlorinated carborane cage anion per asymmetric unit. By changing the counter-ion, different packings are observed, and to try to understand this the new structure is compared with five similar compounds. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280948 Thu, 29 Sep 2011 04:00:00 +0100 5280948 http://www.medworm.com/index.php?rid=5280947&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3021 The molecule of the title compound (systematic name: 6-chloroindolin-2-one), C8H6ClNO, is almost planar, with a dihedral angle of 1.13 (9)° between the planes of the constituent pyrrolidine and benzene rings. Centrosymmetric dimers are formed in the crystal structure by N—H...O hydrogen bonds, and these dimers are additionally linked by Cl...Cl and C—H...O interactions. Density functional theory (DFT) calculations at the B3LYP/6-31 G(d,p) level of theory were used to optimize the molecular structure and the geometry was best reproduced by optimization of two interacting molecules. The bond orders in the molecule, estimated using the natural bond orbitals (NBO) formalism, are consistent with the observed bond lengths. In particular, the contribution of the lone pair of electrons on... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280947 Thu, 29 Sep 2011 04:00:00 +0100 5280947 http://www.medworm.com/index.php?rid=5280946&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3259 The stereochemistry of the iridoid plumeridoid C, C15H18O7, was established by X-ray single-crystal structure analysis, giving (2′R,3R,4R,4aS,7aR)-methyl 3-hydroxy-4′-[(S)-1-hydroxyethyl]-5′-oxo-3,4,4a,7a-tetrahydro-1H,5′H-spiro[cyclopenta[c]pyran-7,2′-furan]-4-carboxylate. The absolute structure of the title compound was determined on the basis of the Flack x parameter and Bayesian statistics on Bijvoet differences. The hydrogen-bond donor and acceptor functions of the two hydroxy groups are employed in the formation of O—H...O-bonded helical chains. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280946 Thu, 29 Sep 2011 04:00:00 +0100 5280946 http://www.medworm.com/index.php?rid=5280945&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3260 The title compound, C8H4Br6, (I), initially crystallized from deuterochloroform as the comcomitant polymorphs (Ia) (prisms, space group P21/n, Z = 2) and (Ib) (hexagonal plates, space group C2/c, Z = 4). The molecules in both forms display crystallographic inversion symmetry. All further attempts to crystallize the compound led exclusively to (Ib), so that (Ia) may be regarded as a `disappearing polymorph'. Surprisingly, however, the density of (Ia) is greater than that of (Ib). The only significant difference between the molecular structures is the orientation of the CBr3 groups. The molecular packing of both structures is largely determined by Br...Br interactions, although (Ia) also displays a C—H...Br hydrogen bond and both polymorphs display one Br...Ï€ contact. For (Ia), six of the... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280945 Wed, 28 Sep 2011 04:00:00 +0100 5280945 http://www.medworm.com/index.php?rid=5280944&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3415 The title compound, C7H4N2O6, (I), crystallizes in P\overline{1} with Z′ = 4, but with no approximate or pseudosymmetry. The crystals were nonmerohedrally twinned, with at least four twin components related to the major moiety by 180° rotations around the real b and c axes, and by 180° rotation around the a* axis. The excessive twinning is not caused by a phase change from an untwinned room-temperature higher-symmetry polymorph. The molecules are planar chiral and, owing to the tilt angle of the nitro groups and the position of protonation, there are altogether eight conformers possible. Six of these theoretically possible eight conformers are realized in the solid-state structure of (I). Packing analysis and force-field calculations indicate that the largest part of the packing intera... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280944 Wed, 28 Sep 2011 04:00:00 +0100 5280944 http://www.medworm.com/index.php?rid=5280943&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fmx3055 The title compound, C20H32B2N4, is monoclinic at ambient temperature but triclinic (pseudo-monoclinic) below 150 K. The structures of the two phases, determined at 200 and 120 K, respectively, are very similar, the molecular symmetry being crystallographic C2 and approximate (local) C2, respectively. There is significant Ï€ conjugation within each N—B—N moiety, but none between them or between the N—B—N and arene moieties. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280943 Wed, 28 Sep 2011 04:00:00 +0100 5280943 http://www.medworm.com/index.php?rid=5280942&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3005 Two mononuclear copper complexes, {bis[(3,5-dimethyl-1H-pyrazol-1-yl-κN2)methyl]amine-κN}(3,5-dimethyl-1H-pyrazole-κN2)(perchlorato-κO)copper(II) perchlorate, [Cu(ClO4)(C5H8N2)(C12H19N5)]ClO4, (I), and {bis[(3,5-dimethyl-1H-pyrazol-1-yl-κN2)methyl]amine-κN}bis(3,5-dimethyl-1H-pyrazole-κN2)copper(II) bis(hexafluoridophosphate), [Cu(C5H8N2)2(C12H19N5)](PF6)2, (II), have been synthesized by the reactions of different copper salts with the tripodal ligand tris[(3,5-dimethyl-1H-pyrazol-1-yl)methyl]amine (TDPA) in acetone–water solutions at room temperature. Single-crystal X-ray diffraction analysis revealed that they contain the new tridentate ligand bis[(3,5-dimethyl-1H-pyrazol-1-yl)methyl]amine (BDPA), which cannot be obtained by normal organic reactions and has thus been captured in... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5280942 Wed, 28 Sep 2011 04:00:00 +0100 5280942 http://www.medworm.com/index.php?rid=5232678&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3107 The title compound {systematic name: trimethyl[2-({4-oxo-4-[2-(trimethylazaniumyl)ethoxy]butanoyl}oxy)ethyl]azanium diiodide}, C14H30N2O42+·2I−, is a salt of the succinylcholinium cation. There is one formula unit in the asymmetric unit, represented by two anions and two halves of two cations which lie on centres of inversion. The component species are stabilized by electrostatic interactions, and C—H...I and C—H...O hydrogen bonds are also present. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232678 Sat, 17 Sep 2011 04:00:00 +0100 5232678 http://www.medworm.com/index.php?rid=5232674&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3023 The salts hexaaquamagnesium furan-2,5-dicarboxylate, [Mg(H2O)6](C6H2O5), (I), and hexaaquanickel furan-2,5-dicarboxylate, [Ni(H2O)6](C6H2O5), (II), provide the first crystallographic characterization of the furan-2,5-dicarboxylate dianion. Both structures exhibit extensive three-dimensional hydrogen-bonding networks between the octahedral coordinated hexaaquametal(II) ions and the dicarboxylate anions. Although the two structures are not isomorphous, they contain essentially identical two-dimensional slabs. The distinction between the structures is that these slabs are related by translation in (II), whereas adjacent slabs in (I) are reflected relative to each other by the action of a glide plane. The reflection occurs so that the local contacts between slabs are not changed, and thus the ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232674 Sat, 17 Sep 2011 04:00:00 +0100 5232674 http://www.medworm.com/index.php?rid=5232677&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3222 In situ cryocrystallization has been employed to grow single crystals of 4-methoxybenzaldehyde (anisaldehyde), C8H8O2, 2-hydroxybenzaldehyde (salicylaldehyde), C7H6O2, and (2E)-3-phenylprop-2-enal (cinnamaldehyde), C9H8O, all of which are liquids at room temperature. Several weak C—H...O interactions of the types Caryl—H...O, Cformyl—H...O and Csp3—H...O are present in these related crystal structures. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232677 Fri, 16 Sep 2011 04:00:00 +0100 5232677 http://www.medworm.com/index.php?rid=5232676&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fdn3164 In xanthinium nitrate hydrate [systematic name: 2,6-dioxo-1,2,3,6-tetrahydro-9H-purin-7-ium nitrate monohydrate], C5H5N4O2+·NO3−·H2O, (I), and xanthinium hydrogen sulfate hydrate [systematic name: 2,6-dioxo-1,2,3,6-tetrahydro-9H-purin-7-ium hydrogen sulfate monohydrate], C5H5N4O2+·HSO4−·H2O, (II), the xanthine molecules are protonated at the imine N atom with the transfer of an H atom from the inorganic acid. The asymmetric unit of (I) contains a xanthinium cation, a nitrate anion and one water molecule, while that of (II) contains two crystallographically independent xanthinium cations, two hydrogen sulfate anions and two water molecules. A pseudo-quadruple hydrogen-bonding motif is formed between the xanthinium cations and the water molecules via N—H...O and O—H...O hydrogen ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232676 Thu, 15 Sep 2011 04:00:00 +0100 5232676 http://www.medworm.com/index.php?rid=5232675&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3258 The title compound, C20H25N3O, an important precursor for the preparation of benzovesamicol analogues for the diagnosis of Alzheimer's disease, has been synthesized and characterized by FT–IR, and 1H and 13C NMR spectroscopic analyses. The crystal structure was analysed using powder diffraction as no suitable single crystal was obtained. The piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. The crystal packing is mediated by weak contacts, principally by complementary intermolecular N—H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C—H...N contacts and by a weak intermolecular C—H...Ï€ interaction. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232675 Thu, 15 Sep 2011 04:00:00 +0100 5232675 http://www.medworm.com/index.php?rid=5232673&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fem3043 The asymmetric unit of the title compound, poly[{μ4-4-[(carboxylatomethyl)sulfanyl]benzoato}(N,N-dimethylformamide)zinc], [Zn(C9H6O4S)(C3H7NO)]n, consists of one crystallographically independent ZnII cation, one 4-[(carboxylatomethyl)sulfanyl]benzoate (L2−) ligand and one coordinated dimethylformamide (DMF) molecule. The zinc ion is coordinated by five O atoms from four separate L2− ligands and one DMF molecule, and the ZnO5 unit displays a distorted square-based-pyramidal geometry. Two ZnO5 units form a binuclear zinc–tetracarboxylate paddlewheel cluster, and these are bridged by L2− ligands to generate an intersecting helical chain (Zn2+ ions as nodes), which is composed of right-handed (P) and left-handed (M) helices. Weak C—H...O hydrogen bonds extend the one-dimensional coo... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232673 Thu, 15 Sep 2011 04:00:00 +0100 5232673 http://www.medworm.com/index.php?rid=5232672&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsq3296 The title compound, [Zn(C9H7N3)2(H2O)4](CF3O3S)2, contains an octahedral [ZnL2(H2O)4]2+ cationic complex with trans geometry (Zn site symmetry \overline{1}), and each 5-(3-pyridyl)pyrimidine (L) ligand is coordinated in a monodentate fashion through the pyridine N atom. In the extended structure, these complexes, with both hydrogen-bond acceptor (pyrimidine) and donor (H2O) functions, are linked to each other by intermolecular water–pyrimidine O—H...N hydrogen-bonding interactions, resulting in a double chain along the crystallographic a axis. The trifluoromethanesulfonate anions are integrated into the chains via O—H...O hydrogen bonds between the coordinated water and sulfonate O atoms. These double chains are associated into a novel three-dimensional network through interchain wat... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232672 Thu, 15 Sep 2011 04:00:00 +0100 5232672 http://www.medworm.com/index.php?rid=5232671&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3065 In the present tetragonal modification of dysprosium orthomolybdate, Dy2(MoO4)3, the Dy, one Mo and one O atom are located on a mirror plane with Wyckoff symbol 4e, while another Mo atom is located on a fourfold inverse axis, Wyckoff symbol 2a. A single crystal was selected from a polycrystalline mixture of the Dy2O3–ZrO2–MoO3 system and was stable at room temperature for at least three months. The structure refinement does not indicate the presence of Zr on the Dy sites (to within 1% accuracy). Thus, the stabilization of the tetragonal form is due to disordered positions for a second O atom and split positions for a third O atom that also maintain the DyO7 coordination, which is not expected for short Dy—O distances [2.243 (6)–2.393 (5) Å]. (Source: Acta Crystallographica S... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5232671 Thu, 15 Sep 2011 04:00:00 +0100 5232671 http://www.medworm.com/index.php?rid=5190775&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3063 The crystal structure of ammonium rubidium nonaoxotetratellurate(IV) dihydrate has been studied as a function of pressure up to 7.40 GPa. The ambient-pressure structure is characterized by the co-existence of three different Te—O polyhedra (TeO3, TeO4 and TeO5), which are connected to form layers. NH4+, H2O and Rb+ are incorporated between the layers. Both the Rb1 position, which is located on a twofold axis, and the Rb2 position are partially occupied. The three different types of coordination polyhedra around Te4+ are stable up to at least 5.05 GPa. No phase transition is observed. The fit of the unit-cell volume as a function of pressure gives a zero-pressure bulk modulus of 34 (1) GPa with a zero-pressure volume of V0 = 2620 (4) Å3 [B′ = 1.4 (2)]. (Source: Acta Cryst... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5190775 Sun, 04 Sep 2011 01:27:59 +0100 5190775 http://www.medworm.com/index.php?rid=5190776&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ftp3002 The title compounds, p-phenetidinium hydrogen phthalate (or 4-ethoxyanilinium 2-carboxybenzoate), C8H12NO+·C8H5O4−, (I), and cyclohexylaminium hydrogen phthalate hemihydrate (or cyclohexylaminium 2-carboxybenzoate hemihydrate), C6H14N+·C8H5O4−·0.5H2O, (II), form two- and one-dimensional supramolecular networks, respectively. In (I), the anionic–cationic network consists of R32(6) and R44(16) hydrogen-bonded rings forming a two-dimensional sheet along the (001) plane. In (II), O—H...O hydrogen bonds connect the glide-related anions, generating a supramolecular chain running parallel to [001] to which the cations are linked to form one-dimensional channels along [001]. The solvent water molecules, which reside on twofold axes, are trapped inside the molecular channels by N—H...O... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5190776 Thu, 01 Sep 2011 23:00:00 +0100 5190776 http://www.medworm.com/index.php?rid=5168401&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsq3295 The title compound, {[Ag(C13H14N2)](C10H6O6S2)0.5·2H2O}n, (I), features a three-dimensional supramolecular sandwich architecture that consists of two-dimensional cationic layers composed of polymeric chains of silver(I) ions and 1,3-bis(4-pyridyl)propane (bpp) ligands, linked by Ag...Ag and π–π interactions, alternating with anionic layers in which uncoordinated naphthalene-1,5-disulfonate (nds2−) anions and solvent water molecules form a hydrogen-bonded network. The asymmetric unit consists of one AgI cation linearly coordinated by N atoms from two bpp ligands, one bpp ligand, one half of an nds2− anion lying on a centre of inversion and two solvent water molecules. The two-dimensional {[Ag(bpp)]+}n cationic and {[(nds)·2H2O]2−}n anionic layers are assembled into a three-dimen... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5168401 Thu, 25 Aug 2011 23:00:00 +0100 5168401 http://www.medworm.com/index.php?rid=5168400&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbi3020 The reaction of (Et4N)[Tp*WS3] [Tp* = hydrogen tris(3,5-dimethylpyrazol-1-yl)borate] with one or two equivalents of CuBr afforded the [1 + 1] and [1 + 2] addition products (Et4N)[Tp*WS(μ-S)2(CuBr)] {or (C8H20N)[CuWBr(C15H22BN6)S3], (I)} and (Et4N)[Tp*W(μ3-S)(μ-S)2(CuBr)2] {or (C8H20N)[Cu2WBr2(C15H22BN6)S3], (II)}. The anion of (I) contains a [W(μ-S)2Cu] core formed by the addition of one CuBr unit to the [Tp*WS3] species. The anion of (II) has a butterfly-shaped [W(μ3-S)(μ-S)2Cu2] core formed by the addition of two CuBr units to the [Tp*WS3] species. The [Tp*WS3] sections of each complex exhibit approximate C3v point symmetry and have closely comparable geometry. In (II), both the anion and cation lie on a crystallographic mirror plane. The structure of (I) is noncentrosymmet... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5168400 Thu, 25 Aug 2011 23:00:00 +0100 5168400 http://www.medworm.com/index.php?rid=5168399&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3223 A new triclinic polymorph of the title compound, [PdCl2(C18H15P)2], has two independent molecules in the unit cell, with the Pd atoms located on inversion centres. One molecule has an eclipsed conformation, whereas the second molecule adopts a gauche conformation. The molecules with a gauche conformation are involved in weak intermolecular C—H...Cl—Pd interactions with symmetry-related molecules. It is suggested that C—H...Cl—Pd interactions are mainly responsible for the existence of conformational differences, which contribute to the polymorph formation. In the crystal, there are layers of eclipsed and gauche molecules separated by normal van der Waals interactions. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5168399 Thu, 25 Aug 2011 23:00:00 +0100 5168399 http://www.medworm.com/index.php?rid=5168398&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbg3140 The environment of the U atom in the title compound, (C4H12N)4[UO2(CO3)3]·8H2O, presents a typical hexagonal bipyramidal geometry found in many actinide complexes. It is a model for actinide species and consists of common environmental moieties (carbonate, water and ammonia species). The structure displays a sheet-like hydrogen-bonding network formed from crystallization water molecules and carbonate ligands. The compound is isomorphous with a previously described Np isolog [Grigorev et al. (1997). Radiokhimiya (Russ. Radiochem.), 39, 325–329]. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5168398 Thu, 25 Aug 2011 23:00:00 +0100 5168398 http://www.medworm.com/index.php?rid=5137441&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fem3042 The interaction of the antifungal pharmaceutical agent fluconazole with salicylic acid in acetonitrile solution yields the 1:1 cocrystal 2-(2,4-difluorophenyl)-1,3-bis(1H-1,2,4-triazol-1-yl)propan-2-ol–2-hydroxybenzoic acid (1/1), C13H12F2N6O·C7H6O3. The asymmetric unit consists of one molecule of fluconazole and one molecule of salicylic acid, both in their neutral forms. Both crystal agents form head-to-tail hydrogen-bonded dimers, which are further connected into hydrogen-bonded extended zigzag tapes propagating along the ac diagonal. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5137441 Tue, 16 Aug 2011 23:00:00 +0100 5137441 http://www.medworm.com/index.php?rid=5137439&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3256 The solid-state structures of three push–pull acceptor-Ï€-donor (A-Ï€-D) systems differing only in the nature of the Ï€-spacer have been determined. (E)-1-Nitro-4-[2-(3,4,5-trimethoxyphenyl)ethenyl]benzene, C17H17NO5, (I), and its `bridge-flipped' imine analogues, (E)-3,4,5-trimethoxy-N-(4-nitrobenzylidene)aniline, C16H16N2O5, (II), and (E)-4-nitro-N-(3,4,5-trimethoxybenzylidene)aniline, C16H16N2O5, (III), display different kinds of supramolecular networks, viz. corrugated planes, a herringbone pattern and a layered structure, respectively, all with zero overall dipole moments. Only (III) crystallizes in a noncentrosymmetric space group (P212121) and is, therefore, a potential material for second-harmonic generation (SHG). (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5137439 Tue, 16 Aug 2011 23:00:00 +0100 5137439 http://www.medworm.com/index.php?rid=5116666&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsu3071 The title compound, [Zn2(C9H4O6)2(C6H6N4)2], consists of two ZnII ions, two 5-carboxybenzene-1,3-dicarboxylate (Hbtc2−) dianions and two 2,2′-bi-1H-imidazole (bimz) molecules. The ZnII centre is coordinated by two carboxylate O atoms from two Hbtc2− ligands and by two imidazole N atoms of a bimz ligand, in a distorted tetrahedral coordination geometry. Two neighbouring ZnII ions are bridged by a pair of Hbtc2− ligands, forming a discrete binuclear [Zn2(Hbtc)2(bimz)2] structure lying across an inversion centre. Hydrogen bonds between carboxyl H atoms and carboxylate O atoms and between imidazole H atoms and carboxylate O atoms link the binuclear units. These binuclear units are further extended into a three-dimensional supramolecular structure through extensive O—H...O and N—H..... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5116666 Wed, 10 Aug 2011 23:00:00 +0100 5116666 http://www.medworm.com/index.php?rid=5116665&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsq3293 The title dinuclear complex, (aqua-1κO)tetrakis(μ-2,3-diphenylprop-2-enoato-1:2κ2O:O′)bis(2,3-diphenylprop-2-enoato)-1κO;2κO-(ethanol-2κO)bis(1,10-phenanthroline)-1κ2N,N′;2κ2N,N′-dilanthanum(III), [La2(C15H11O2)6(C12H8N2)2(C2H5OH)(H2O)], contains two similar LaIII centres with distorted [LaO6N2] bicapped triganol–prismatic coordination polyhedra formed by six phenylcinnamate (PCA− or 2,3-diphenylprop-2-enoate) ligands, two 1,10-phenanthroline (phen) ligands, a coordinating ethanol molecule and a coordinating water molecule. The two metal centres are bridged by four μ-PCA− ligands, with the remaining two PCA− ligands coordinated in a monodentate fashion. The noncoordinated carboxylate O atoms on the terminal PCA− ligands form O—H...O hydrogen bonds with the coordi... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5116665 Wed, 10 Aug 2011 23:00:00 +0100 5116665 http://www.medworm.com/index.php?rid=5102505&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3049 The green crystals of the title compound, [V(C22H18N2O2)O], represent a mononuclear oxovanadium complex. The central VIV centre has a distorted square-pyramidal coordination. Two N atoms and two O atoms of the Schiff base ligand define the base of the pyramid, and the oxide O atom is in the apical position. Density functional theory (DFT) calculations were performed to analyse the changes in the geometry of the ligand during the complex formation. The most significant changes are observed in the values of the torsion angles in the vicinity of the donor N atoms. The HOMA index (Harmonic Oscillator Model of Aromaticity) has been calculated to compare the aromaticity of the benzene rings in the complex and its ligand. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102505 Sun, 07 Aug 2011 03:56:04 +0100 5102505 http://www.medworm.com/index.php?rid=5102512&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3155 The title compound [systematic name (6S,12S)-methyl 6-(allyloxymethyl)-12-isopropyl-2,2,9,9-tetramethyl-4,7,10-trioxo-3-oxa-5,8,11-triazatridecan-13-oate], C21H37N3O7, containing the little studied O-allyl-l-serine residue [Ser(All)], crystallizes in the monoclinic space group C2 with one molecule in the asymmetric unit. The compound is an analogue of the Ser140-Val142 segment of the water channel aquaporin-4 (AQP4). It forms a distorted type-II β-turn with a PII–310L–PII backbone conformation (PII is polyproline II). The overall backbone conformation is markedly different from that of the CO(Pro139)–Val142 stretch of rat AQP4, but is quite similar to the corresponding segment of human AQP4, despite significant differences at the level of the individual residues. The side chain of t... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102512 Fri, 05 Aug 2011 23:00:00 +0100 5102512 http://www.medworm.com/index.php?rid=5102506&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fov3005 The reaction between [PtCl(terpy)]·2H2O (terpy is 2,2′:6′,2′′-terpyridine) and pyrazole in the presence of two equivalents of AgClO4 in nitromethane yields the title compound, [Pt(C3H4N2)(C15H11N3)](ClO4)2·CH3NO2, as a yellow crystalline solid. Single-crystal X-ray diffraction shows that the dicationic platinum(II) chelate is square planar with the terpyridine ligand occupying three sites and the pyrazole ligand occupying the fourth. The torsion angle subtended by the pyrazole ring relative to the terpyridine chelate is 62.4 (6)°. Density functional theory calculations at the LANL2DZ/PBE1PBE level of theory show that in vacuo the lowest-energy conformation has the pyrazole ligand in an orientation perpendicular to the terpyridine ligand (i.e. 90°). Seemingly, the stability ga... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102506 Fri, 05 Aug 2011 23:00:00 +0100 5102506 http://www.medworm.com/index.php?rid=5102511&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsu3068 Although having been described as a liquid in the literature for 41 years, 1,2-bis[(pyridin-2-ylmethyl)sulfanyl]ethane, C14H16N2S2, (I), has now been obtained as monoclinic crystals via a new and convenient method of purification. Molecules of (I) are located on crystallographic inversion centres and are held together by C—H...N and C—H...S interactions, resulting in the formation of a three-dimensional network structure. In addition, two polymorphs of the corresponding hydrochloride salt, 2-[({2-[(pyridin-1-ium-2-ylmethyl)sulfanyl]ethyl}sulfanyl)methyl]pyridin-1-ium dichloride, C14H18N2S22+·2Cl−, (II) and (III), have been isolated. Molecules of (II) and (III) have similar conformations and are located on inversion centres. Both polymorphs form three-dimensional networks through Nâ€... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102511 Thu, 04 Aug 2011 23:00:00 +0100 5102511 http://www.medworm.com/index.php?rid=5102510&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Feg3074 The title terephthalic acid derivatives, namely 2,5-dimethoxyterephthalic acid, C10H10O6, (I), and 2,5-diethoxyterephthalic acid, C12H14O6, (II), exhibit nearly planar molecular structures, with maximum deviations from the least-squares planes calculated for all non-H atoms of 0.0418 (6) and 0.0902 (10) Å for (I) and (II), respectively. The molecules of both title compounds contain an inversion centre and thus the asymmetric unit of both crystal structures consists of only half a molecule. It is a remarkable fact that a comparatively small change in the substitution of the terephthalic acid [dimethoxy in (I) versus diethoxy in (II)] causes major differences in the dominating supramolecular interactions. While in (II) the packing structure is stabilized by typical intermolecular hydr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102510 Thu, 04 Aug 2011 23:00:00 +0100 5102510 http://www.medworm.com/index.php?rid=5102509&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3003 In the crystal structures of the diastereoisomers of O-tosylcinchonidine [(9R)-cinchon-9-yl 4-methylbenzenesulfonate], (I), and O-tosylcinchonine [(9S)-cinchon-9-yl 4-methylbenzenesulfonate], (II), both C26H28N2O3S, both molecules are in an anti-closed conformation and, in each case, the position of the aryl ring of the tosylate system is influenced by an intramolecular C—H...O hydrogen bond. The molecular packing in (I) is influenced by weak intermolecular C—H...O and C—H...Ï€ interactions. The crystal structure of (II) features C—H...Ï€ interactions and van der Waals forces only. The computational investigations using RHF/6–31G** ab initio and AM1 semi-empirical methods performed for (I) and (II) and their protonated species show that the conformational and energetic parameters... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102509 Thu, 04 Aug 2011 23:00:00 +0100 5102509 http://www.medworm.com/index.php?rid=5102508&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsu3067 2,3,4,5,6-Pentafluorophenol (pFp), unlike phenol, forms cocrystals with the weak heteroaromatic base phenazine (phz). Two types of cocrystals were prepared, (I) with a high content of pFp, 2,3,4,5,6-pentafluorophenol–phenazine (5/1), 5C6HF5O·C12H8N2, and (II) with a 2:1 pFp–phz molar ratio, 2,3,4,5,6-pentafluorophenol–phenazine (2/1), 2C6HF5O·C12H8N2. In both forms, homostacks are formed by the heterocyclic base and phenol molecules and no aryl–perfluoroaryl stacking interactions occur. The arrangement of the molecules in the crystal of (I) is determined by strong O—H...N and O—H...O hydrogen bonds, weak O—H...F, C—H...F and C—H...O interactions, π–π stacking interactions between the phz molecules and C—F...Ï€F interactions within the pFp stacks. Among the specifi... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102508 Thu, 04 Aug 2011 23:00:00 +0100 5102508 http://www.medworm.com/index.php?rid=5102507&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsu3065 The asymmetric unit of the title compound, C10H10N22+·2C2HO4−, consists of one half of a 4,4′-bipyridinium cation, which has inversion symmetry, and a hydrogen oxalate anion, in which an intramolecular hydrogen bond exists. The cations and anions are connected by O—H...O, N—H...O and C—H...O hydrogen bonds, forming a two-dimensional network, whereas π–π stacking interactions involving the 4,4′-bipyridinium cations lead to the formation of a three-dimensional supramolecular structure. An unusual deca-atomic ring is formed between two hydrogen oxalate anions, which are linked side-to-side via O—H...O hydrogen-bonding interactions. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5102507 Thu, 04 Aug 2011 23:00:00 +0100 5102507 http://www.medworm.com/index.php?rid=5076000&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3225 In the structure of the title 1:1 proton-transfer compound of brucine with 2-(2,4,6-trinitroanilino)benzoic acid, C23H27N2O4+·C13H7N4O8−·H2O, the brucinium cations form classic undulating ribbon substructures through overlapping head-to-tail interactions, while the anions and the three related partial solvent water molecules (having occupancies of 0.73, 0.17 and 0.10) occupy the interstitial regions of the structure. The cations are linked to the anions directly through N—H...OCOO− hydrogen bonds and indirectly by the three water molecules, which form similar conjoint cyclic bridging units [graph set R24(8)] through O—H...OC=O and O—H...OCOO− hydrogen bonds, giving a two-dimensional layered structure. Within the anion, intramolecular N—H...OCOO− and N—H...Onitro hydroge... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5076000 Wed, 27 Jul 2011 23:00:00 +0100 5076000 http://www.medworm.com/index.php?rid=5075999&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3047 The title compound, C16H16Br2O4S2, which is a precursor for the synthesis of oligothiophenes and their substituted homologues, was synthesized and its X-ray crystal structure determined at 100 K. The experimental electron-density parameters for the available atom types were transferred from the ELMAM2 database. The compound lies about an inversion centre, which coincides with the mid-point of a C—C bond. The molecules in the crystal are linked by several types of weak interactions; the largest contact surfaces are for H...H and H...Br. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5075999 Wed, 27 Jul 2011 23:00:00 +0100 5075999 http://www.medworm.com/index.php?rid=5068343&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fmx3051 Crystals of 5-hydroxy-6-methyl-2-pyridone, (I), grown from a variety of solvents, are invariably trigonal (space group R\overline{3}); these are 5-hydroxy-6-methyl-2-pyridone acetone 0.1667-solvate, C6H7NO2·0.1667C3H6O, (Ia), and 6-methyl-5-hydroxy-2-pyridone propan-2-ol 0.1667-solvate, C6H7NO2·0.1667C3H8O, (Ib), and the forms from methanol, (Ic), water, (Id), benzonitrile, (Ie), and benzyl alcohol, (If). They incorporate channels running the length of the c axis that contain extensively disordered solvent molecules. A solvent-free sublimed powder of 5-hydroxy-6-methyl-2-pyridone microcrystals is essentially isostructural. Inversion-related host molecules interact via pairs of N—H...O hydrogen bonds to form R22(8) dimers. Six of these dimers form large R126(42) puckered rings, in which... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5068343 Tue, 26 Jul 2011 23:00:00 +0100 5068343 http://www.medworm.com/index.php?rid=5057029&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgt3033 The structures of three related keto diester and diester ylides, namely diethyl 3-oxo-2-(triphenylphosphoranylidene)glutarate, C27H27O5P, (I), diethyl 3-oxo-2-(triphenylphosphoranylidene)glutarate acetic acid monosolvate, C27H27O5P·C2H4O2, (II), and diethyl 2-(triphenylphosphoranylidene)succinate, C26H27O4P, (III), are presented. The syn-keto anti-ester conformations in the crystalline keto diesters are governed by electronic delocalization between the P—C and ylidic bonds and an acyl group, and by intra- and intermolecular interactions. There are also intramolecular attractive and repulsive interactions of different types (C—H...O and C—H...Ï€) controlling the molecular conformations. The mono-ylidic diester (III) has an anti-ester conformation, while those for (I) and (II) are rel... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5057029 Thu, 21 Jul 2011 23:00:00 +0100 5057029 http://www.medworm.com/index.php?rid=5057028&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fga3165 In the title coordination compound, [Cd(C8H3NO6)(C5H8N3)0.5(H2O)]n, each CdII atom is six-coordinated in a distorted octahedral environment surrounded by three carboxylate O atoms from two different 5-nitroisophthalate (5-NIP2−) ligands, two N atoms from two distinct 1,6-bis(1,2,4-triazol-1-yl)hexane (bth) ligands and one water molecule. The CdII centres are bridged by the bth ligands, which lie across centres of inversion, to give a honeycomb-like two-dimensional layer structure; the layers are further connected by the bridging 5-NIP2− ligands with a κ2;κ1-μ2 coordination mode to generate the final three-dimensional structure. Topologically, taking the the CdII atoms and the bth ligands as different four-connected nodes and the 5-NIP2− ligands as linkers, the three-dimensional st... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5057028 Thu, 21 Jul 2011 23:00:00 +0100 5057028 http://www.medworm.com/index.php?rid=5057027&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fga3164 Orange crystals of bis(acetonitrile-κN)bis[N,N-bis(diphenylphosphanyl)ethanamine-κ2P,P′]iron(II) tetrabromidoferrate(II), [Fe(CH3CN)2(C26H25NP2)2][FeBr4], (I), and red crystals of bis(acetonitrile-κN)bis[N,N-bis(diphenylphosphanyl)ethanamine-κ2P,P′]iron(II) μ-oxido-bis[tribromidoferrate(III)], [Fe(CH3CN)2(C26H25NP2)2][Fe2Br6O], (II), were obtained from the same solution after prolonged exposure to atmospheric oxygen, resulting in partial oxidation of the [FeBr4]2− anion to the [Br3FeOFeBr3]2− anion. The asymmetric unit of (I) consists of three independent cations, one on a general position and two on inversion centres, with two anions, required to balance the charge, located on general positions. The asymmetric unit of (II) consists of two independent cations and two anions, a... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5057027 Thu, 21 Jul 2011 23:00:00 +0100 5057027 http://www.medworm.com/index.php?rid=5026542&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Flg3062 The crystal structures of two p-substituted phenylformiminopyrrole derivatives, namely 2-[(4-fluorophenyl)iminomethyl]pyrrole, C11H9FN2, (1), and 2-[(1H-pyrrol-2-ylmethylidene)amino]benzonitrile, C12H9N3, (2), bear F and C[triple-bond]N electron-withdrawing groups, respectively. Both structures feature two independent molecules in the asymmetric unit forming dimers via N—H...N hydrogen bonds. In the case of (1), each dimer interacts with two other dimers via C—H...F contacts, thus forming one-dimensional chains in the b direction, whereas in the case of (2), a weak C—H...N interaction connects the dimers in one-dimensional chains in the (110) direction. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5026542 Wed, 13 Jul 2011 23:00:00 +0100 5026542 http://www.medworm.com/index.php?rid=5005927&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbm3106 The title compound, [Co(C5H7N6)2(H2O)4](C10H2O8)·4H2O, is an ionic structure comprising a [Co(Hdap)2(H2O)4]4+ cation (dap is 2,6-diaminopurine) in a general position, two benzene-1,2,4,5-tetracarboxylate (btc4−) anions straddling two different inversion centres and four solvent water molecules. The structure presents a remarkable degree of pseudosymmetry, with the CoII cation lying almost exactly on a noncrystallographic pseudo-inversion centre. The overall spatial arrangement can be described in terms of cationic and anionic chains running along the [111] direction and linked into a three-dimensional network by a very complex hydrogen-bonding scheme in which all the available N—H and O—H groups take part. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005927 Thu, 07 Jul 2011 20:04:46 +0100 5005927 http://www.medworm.com/index.php?rid=5005936&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsq3285 The structures of orthorhombic (E)-4-(2-{[amino(iminio)methyl]amino}vinyl)-3,5-dichlorophenolate dihydrate, C8H8Cl2N4O·2H2O, (I), triclinic (E)-4-(2-{[amino(iminio)methyl]amino}vinyl)-3,5-dichlorophenolate methanol disolvate, C8H8Cl2N4O·2CH4O, (II), and orthorhombic (E)-amino[(2,6-dichloro-4-hydroxystyryl)amino]methaniminium acetate, C8H9Cl2N4O+·C2H3O2−, (III), all crystallize with one formula unit in the asymmetric unit, with the molecule in an E configuration and the phenol H atom transferred to the guanidine N atom. Although the molecules of the title compounds form extended chains via hydrogen bonding in all three forms, owing to the presence of different solvent molecules, those chains are connected differently in the individual forms. In (II), the molecules are all coplanar, whi... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005936 Tue, 05 Jul 2011 23:00:00 +0100 5005936 http://www.medworm.com/index.php?rid=5005935&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fga3166 In the title cocrystal, 4-amino-N-(4,6-dimethylpyrimidin-2-yl)benzenesulfonamide–4-amino-N-(4,6-dimethyl-1,2-dihydropyrimidin-2-ylidene)benzenesulfonamide–1,3-dimethyl-7H-purine-2,6-dione (1/1/1), C7H8N4O2·2C12H14N4O2S, two sulfamethazine molecules cocrystallize with a single molecule of theophylline. Each molecule of sulfamethazine forms a hydrogen-bonded ribbon along the b axis crosslinked by further hydrogen bonding. The two sulfamethazine molecules exhibit a hydrogen-shift isomerization so that the crystal structure contains both tautomeric forms. Calculation of their relative energies showed that the tautomer protonated at the chain N atom is considerably more stable than the one where an N atom in the aromatic ring is protonated. The latter, here observed for the first time, is ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005935 Tue, 05 Jul 2011 23:00:00 +0100 5005935 http://www.medworm.com/index.php?rid=5005934&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgz3195 Two concomitant polymorphs, (I) and (II), of a β-benzyl-β-hydroxyaspartate analogue [systematic name: dibenzyl 2-benzyl-2-hydroxy-3-(4-methylphenylsulfonamido)succinate], C32H31NO7S, crystallize from a mixture of ethyl acetate and cyclohexane at ambient temperature. The structure of (I) has triclinic (P\overline{1}) symmetry and that of (II) monoclinic (P21/c) symmetry. Both crystal structures are made up of a stacking of homochiral racemic dimers (2S,3S and 2R,3R) which are internally connected by a similar R22(9) hydrogen-bonding pattern consisting of intermolecular N—H...O and O—H...O hydrogen bonds. The centroid of the racemic dimer lies on an inversion centre. The main structural difference between the two polymorphs is the conformational orientation of two of the four aromatic ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005934 Mon, 04 Jul 2011 23:00:00 +0100 5005934 http://www.medworm.com/index.php?rid=5005933&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fdt3003 Glycinium semi-malonate, C2H6NO2+·C3H3O4−, (I), and glutaric acid–glycine (1/1), C2H5NO2·C5H8O4, (II), are new examples of two-component crystal structures containing glycine and carboxylic acids. (II) is the first example of a glycine cocrystal which cannot be classified as a salt, as glutaric acid remains completely protonated. In the structure of (I), there are chains formed exclusively by glycinium cations, or exclusively by malonate anions, and these chains are linked with each other. Two types of very short O—H...O hydrogen bonds are present in the structure of (I), one linking glycinium cations with malonate anions, and the other linking malonate anions with each other. In contrast to (I), no direct linkages between molecules of the same type can be found in (II); all the hy... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005933 Mon, 04 Jul 2011 23:00:00 +0100 5005933 http://www.medworm.com/index.php?rid=5005932&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Feg3073 The title compound, C14H18F2O2·0.5H2O, a hemihydrate of a Cs-symmetric unsaturated difluorodiol, crystallizes in the centrosymmetric space group P2/m (Z = 4). The asymmetric unit contains two crystallographically independent difluorodiol half-molecules, occupying the mirror planes at (x, 0, z) and (x, {1\over 2}, z), and half a molecule of water, lying on the twofold axis at (0, y, 0). Four difluorodiol molecules self-assemble around each solvent water molecule via O—H...O hydrogen bonds in a near tetrahedral symmetry to generate a cylindrical column-like architecture. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005932 Mon, 04 Jul 2011 23:00:00 +0100 5005932 http://www.medworm.com/index.php?rid=5005931&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3390 The influence of the substituent at the C2 position on the hydrogen-bonding patterns is compared for a series of five related compounds, namely (±)-3-exo,6-exo-dibromo-5-endo-hydroxy-3-endo-nitrobicyclo[2.2.1]heptane-2-exo-carbonitrile, C8H8Br2N2O3, (II), (±)-3-exo,6-exo-dibromo-6-endo-nitro-5-exo-phenylbicyclo[2.2.1]heptan-2-endo-ol, C13H13Br2NO3, (III), (±)-methyl 3-exo,6-exo-dibromo-5-endo-hydroxy-3-endo-nitrobicyclo[2.2.1]heptane-2-exo-carboxylate, C9H11Br2NO5, (IV), (±)-methyl 3-exo,6-exo-dibromo-7-diphenylmethylidene-5-endo-hydroxy-3-endo-nitrobicyclo[2.2.1]heptane-2-exo-carboxylate, C22H19Br2NO5, (V), and (±)-methyl 3-exo,6-exo-dibromo-5-endo-hydroxy-3-endo-nitro-7-oxabicyclo[2.2.1]heptane-2-exo-carboxylate, C8H9Br2NO6, (VI). The hydrogen-bonding motif in all five compounds is ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005931 Mon, 04 Jul 2011 23:00:00 +0100 5005931 http://www.medworm.com/index.php?rid=5005930&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fjz3206 The title compound (systematic name: methyl 2-{2-[(tert-butoxycarbonyl)amino]-2-methylpropanamido}-2-methylpropanoate), C14H26N2O5, (I), crystallizes in the monoclinic space group P21/n in two polymorphic forms, each with one molecule in the asymmetric unit. The molecular conformation is essentially the same in both polymorphs, with the α-aminoisobutyric acid (Aib) residues adopting Ï• and ψ values characteristic of α-helical and mixed 310- and α-helical conformations. The helical handedness of the C-terminal residue (Aib2) is opposite to that of the N-terminal residue (Aib1). In contrast to (I), the closely related peptide Boc-Aib-Aib-OBn (Boc is tert-butoxycarbonyl and Bn is benzyl) adopts an αL-PII backbone conformation (or the mirror image conformation). Compound (I) forms hydroge... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005930 Mon, 04 Jul 2011 23:00:00 +0100 5005930 http://www.medworm.com/index.php?rid=5005929&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fjz3205 The title compound, C16H30N2O5, crystallizes with three molecules in the asymmetric unit, each adopting a β-strand/polyproline II backbone conformation. The main-chain functional groups are hydrogen bonded into tapes having the characteristics of parallel β-sheets. Each tape has a left-handed twist and thus forms a helix, with six peptide molecules needed to complete a full 360° rotation. A comparison of hydrogen-bond lengths and twisting modes is made with other related structures of protected dipeptides and with a hexapeptide derived from amyloid-β containing the Val–Val segment. Additionally, a comparison of the backbone conformation is made with that of the Val141–Val142 segment of the water channel aquaporin-4 (AQP4). (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005929 Mon, 04 Jul 2011 23:00:00 +0100 5005929 http://www.medworm.com/index.php?rid=5005928&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyp3005 In the solid state, 4-methoxy-N′-(2,2,2-trichloroethanimidoyl)benzene-1-carboximidamide, C10H10Cl3N3O, (I), N′-(2,2,2-trichloroethanimidoyl)benzene-1-carboximidamide, C9H8Cl3N3, (II), 4-chloro-N′-(2,2,2-trichloroethanimidoyl)benzene-1-carboximidamide, C9H7Cl4N3, (III), 4-bromo-N′-(2,2,2-trichloroethanimidoyl)benzene-1-carboximidamide, C9H7BrCl3N3, (IV), and 4-trifluoromethyl-N′-(2,2,2-trichloroethanimidoyl)benzene-1-carboximidamide, C10H7Cl3F3N3, (V), display strong intramolecular N—H...N hydrogen bonding across the chelate ring and also intramolecular N—H...Cl contacts. Additional intermolecular hydrogen bonds link the molecules into chains, double chains or sheets in all cases except for compound (V). For compound (II), there are three independent molecules per asymmetric u... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=5005928 Mon, 04 Jul 2011 23:00:00 +0100 5005928 http://www.medworm.com/index.php?rid=4983013&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyp3002 This article also reviews 102 similar structures deposited in the Cambridge Structural Database and with the International Union of Crystallography, with the aim of comparing hydrogen-bond strengths in the above-mentioned cyclic motifs. This analysis shows that the strongest N—H...O hydrogen bonds exist in the R22(8) rings of some molecules. The phosphoryl and carbonyl groups in each of compounds (I)–(III) are anti with respect to each other and the P atoms are in a tetrahedral coordination environment. In the crystal structures, adjacent molecules are linked via the above-mentioned hydrogen bonds in a linear arrangement, parallel to [010] for (I) and (III) and parallel to [100] for (II). Formation of the NC(O)NHP(O)—H...O=C instead of the NC(O)NHP(O)—H...O=P hydrogen bond is refle... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4983013 Tue, 28 Jun 2011 23:00:00 +0100 4983013 http://www.medworm.com/index.php?rid=4983012&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3395 Three potassium edta (edta is ethylenediaminetetraacetic acid, H4Y) salts which have different degrees of ionization of the edta anion, namely dipotassium 2-({2-[bis(carboxylatomethyl)azaniumyl]ethyl}(carboxylatomethyl)azaniumyl)acetate dihydrate, 2K+·C10H14N2O82−·2H2O, (I), tripotassium 2,2′-({2-[bis(carboxylatomethyl)amino]ethyl}ammonio)diacetate dihydrate, 3K+·C10H13N2O83−·2H2O, (II), and tetrapotassium 2,2′,2′′,2′′′-(ethane-1,2-diyldinitrilo)tetraacetate 3.92-hydrate, 4K+·C10H12N2O84−·3.92H2O, (III), were obtained in crystalline form from water solutions after mixing edta with potassium hydroxide in different molar ratios. In (II), a new mode of coordination of the edta anion to the metal is observed. The HY3− anion contains one deprotonated N atom coordinat... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4983012 Tue, 28 Jun 2011 23:00:00 +0100 4983012 http://www.medworm.com/index.php?rid=4983011&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3394 The seven isostructural complexes, [Cu5Ln(C2H4N2O2)5(SO4)(H2O)6.5]2(SO4)·6H2O, where LnIII = Pr, Nd, Sm, Eu, Gd, Dy and Ho, are representatives of the 15-metallacrown-5 family. Each dianion of glycinehydroxamic acid (GlyHA) links two CuII cations forming a cyclic [CuGlyHA]5 frame. The LnIII cations are located at the centre of the [CuGlyHA]5 rings and are bound by the five hydroxamate O atoms in the equatorial plane. Five water molecules are coordinated to CuII cations, and one further water molecule, located close to an inversion centre between two adjacent [Cu5Ln(GlyHA)5]2+ cations, is disordered around this inversion centre and coordinated to a CuII cation of either the first or second metallacrown ether. Another water molecule and one of the two crystallographically independent sulfat... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4983011 Tue, 28 Jun 2011 23:00:00 +0100 4983011 http://www.medworm.com/index.php?rid=4983010&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fwq3004 Post-metallation derivatives of the sodium dialkyl(amido)zincate reagent (TMEDA)Na(μ-TMP)Zn(tBu)2 (TMEDA is N,N,N′,N′-tetramethylethylenediamine and TMP is 2,2,6,6-tetramethylpiperidide) have been of structural interest due to the insight they give into aromatic metallation mechanisms. Here, the aromatic substrate is formally replaced with [ZnO]2 to give tetra-tert-butyldi-μ4-oxido-bis(tetramethylethylenediamine-κ2N,N′)bis(μ2-2,2,6,6-tetramethylpiperidin-1-ido-κ2N:N)disodiumtetrazinc hexane 0.59-solvate, [Na2Zn4(C4H9)4(C9H18N)2O2(C6H16N2)2]·0.59C6H14. The crystallographically centrosymmetric complex retains many of the structural features of its parent monomer but has an unusual dimeric structure, with a central planar Zn–O–Zn–O ring joined to two orthogonal near-planar Z... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4983010 Tue, 28 Jun 2011 23:00:00 +0100 4983010 http://www.medworm.com/index.php?rid=4983009&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fem3041 Poly[bis(μ3-trimethylsilylmethanolato)tetrakis(μ2-trimethylsilylmethyl)dimagnesiumdisodium], [Na2Mg2(C4H11OSi)2(C4H11Si)4]n, was obtained from the controlled exposure to oxygen of the unsolvated sodium magnesate [NaMg(CH2SiMe)3]n. Exhibiting a centrosymmetric (Z′ = 1 \over 2) dimeric core of a heterobimetallic eight-membered cationic ring, hosting two alkoxide ligands at its core, the title compound forms a two-dimensional coordination polymer in the crystallographic bc plane through Na...Me contacts. These contacts from Na to formally uncharged groups are only 0.06 Å longer than those between Na and the formally charged CH2R anions. The coordination polymers stack along the a direction to give a layer structure with alternating hydrophobic and hydrophilic regions. (Source: Acta Cry... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4983009 Tue, 28 Jun 2011 23:00:00 +0100 4983009 http://www.medworm.com/index.php?rid=4967209&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgg3253 Indolin-2-one (oxindole), (I), undergoes a Knoevenagel condensation with ferrocene-1,1′-dicarbaldehyde, (II), to afford the title complex 3,3′-[(E,E)-ferrocene-1,1′-diyldimethylidyne]diindolin-2-one dichloromethane disolvate, [Fe(C28H20N2O2)]·2CH2Cl2, (IV). The structure of (IV) contains two ferrocene complex molecules in the asymmetric unit and displays, as expected, intermolecular hydrogen bonding (N—H...O=C) between the indolin-2-one units. Intermolecular π–π stacking interactions are also observed. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4967209 Fri, 24 Jun 2011 23:00:00 +0100 4967209 http://www.medworm.com/index.php?rid=4959036&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fov3004 Single crystals of tribarium diyttrium hexaborate, which crystallized in the cubic system, have been obtained by spontaneous crystallization from a high-temperature melt using Li2O–BaO–B2O3 as flux. Its structure is composed of isolated [B2O5]4− groups, irregular BaO9 polyhedra and regular YO6 polyhedra which occupy alternate sites running along the [111] direction. Irregular BaO9 polyhedra and regular YO6 polyhedra construct a three-dimensional framework, which is reinforced by [B2O5]4− groups. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959036 Thu, 23 Jun 2011 05:46:42 +0100 4959036 http://www.medworm.com/index.php?rid=4959045&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsu3064 The structures of the 1:1 proton-transfer compounds of isonipecotamide (piperidine-4-carboxamide) with 4-nitrophthalic acid [4-carbamoylpiperidinium 2-carboxy-4-nitrobenzoate, C6H13N2O8+·C8H4O6−, (I)], 4,5-dichlorophthalic acid [4-carbamoylpiperidinium 2-carboxy-4,5-dichlorobenzoate, C6H13N2O8+·C8H3Cl2O4−, (II)] and 5-nitroisophthalic acid [4-carbamoylpiperidinium 3-carboxy-5-nitrobenzoate, C6H13N2O8+·C8H4O6−, (III)], as well as the 2:1 compound with terephthalic acid [bis(4-carbamoylpiperidinium) benzene-1,2-dicarboxylate dihydrate, 2C6H13N2O8+·C8H4O42−·2H2O, (IV)], have been determined at 200 K. All salts form hydrogen-bonded structures, viz. one-dimensional in (II) and three-dimensional in (I), (III) and (IV). In (I) and (III), the centrosymmetric R22(8) cyclic amide–am... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959045 Wed, 22 Jun 2011 23:00:00 +0100 4959045 http://www.medworm.com/index.php?rid=4959044&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3389 In 2-amino-6-methylpyridin-1-ium 2-carboxy-3,4,5,6-tetrachlorobenzoate, C6H9N2+·C8HCl4O4−, there are two perpendicular chains of hydrogen-bonded ions, one arising from the interaction between 2-carboxy-3,4,5,6-tetrachlorobenzoate ions and the other from the interaction between the 2-amino-6-methylpyridin-1-ium and 2-carboxy-3,4,5,6-tetrachlorobenzoate ions. These chains combine to form a two-dimensional network of hydrogen-bonded ions. Cocrystals of bis(2-amino-3-methylpyridin-1-ium) 3,4,5,6-tetrachlorophthalate–3,4,5,6-tetrachlorophthalic acid (1/1), 2C6H9N2+·C8Cl4O42−·C8H2Cl4O4, form finite aggregates of hydrogen-bonded ions. π–π interactions are observed between 2-amino-3-methylpyridin-1-ium cations. Both structures exhibit the characteristic R22(8) motif as a result of the... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959044 Wed, 22 Jun 2011 23:00:00 +0100 4959044 http://www.medworm.com/index.php?rid=4959043&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Feg3071 The title compound, C6H15N2+·C2H6NO4S2−, crystallizes as a 0.11-hydrate, (I), in the space group C2; the asymmetric unit consists of two cations (one of each enantiomer), one anion on a general position, two half anions, each with the N atom on a twofold axis, and approximately one fifth of a water molecule. The general anion departs significantly from the usual conformation: it lacks one of the typical `W'-shaped sequence of O—S—N—S—O atoms. The compound also crystallizes in the solvent-free form, (II), in the space group P21/c, with one formula unit in the asymmetric unit. Both compounds form ribbons of hydrogen-bonded cation dimers parallel to the b axis. In (I), there are two independent ribbons of opposite chirality, each involving one anion on a special position, and these... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959043 Wed, 22 Jun 2011 23:00:00 +0100 4959043 http://www.medworm.com/index.php?rid=4959042&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyp3004 The molecule of 3-(2-amino-6-chloropyrimidin-4-yl)-1,1-dimethylprop-2-yn-1-ol monohydrate, C9H10ClN3O·H2O, (I), shows a very polarized molecular–electronic structure, while the polarization is slight for 3-[2-amino-6-(3-hydroxy-3,3-dimethylprop-1-yn-1-yl)pyrimidin-4-yl]-1,1-dimethylprop-2-yn-1-ol, C14H17N3O2, (II). In the supramolecular structure of (I), a combination of hard N—H...N hydrogen bonds and soft C—H...N hydrogen bonds creates a molecular column. Aromatic π–π stackings between the pyrimidine rings stabilize the column with perpendicular and centroid–centroid distances of 3.283 (3) and 3.588 (1) Å, respectively. Short Cl...Cl contacts further link neighbouring molecular columns, creating a hydrophilic tube in which water molecules are fixed by various hydrogen... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959042 Wed, 22 Jun 2011 23:00:00 +0100 4959042 http://www.medworm.com/index.php?rid=4959041&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3050 The structure of β-carboline, also called norharman (systematic name: 9H-pyrido[3,4-b]indole), C11H8N2, has been determined at 110 K. Norharman is prevalent in the environment and the human body and is of wide biological interest. The structure exhibits intermolecular N—H...N hydrogen bonding, which results in a one-dimensional herringbone motif. The three rings of the norharman molecule collectively result in a C-shaped curvature of 3.19 (13)° parallel to the long axis. The diffraction data show shorter pyridyl C—C bonds than those reported at the STO-3G level of theory. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959041 Wed, 22 Jun 2011 23:00:00 +0100 4959041 http://www.medworm.com/index.php?rid=4959040&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fyf3004 Reactions of (Et4N)[Tp*WS3] [Tp* is hydridotris(3,5-dimethylpyrazol-1-yl)borate] with CuSCN in MeCN in the presence of melamine afforded the title neutral dimeric cluster [Cu4W2(C15H22BN6)2(NCS)2S6(C2H3N)2] or [Tp*W(μ2-S)2(μ3-S)Cu(μ2-SCN)(CuMeCN)]2, which has two butterfly-shaped [Tp*WS3Cu2] cores bridged across a centre of inversion by two (CuSCN)− anions. The S atoms of the bridging thiocyanate ligands interact with the H atoms of the methyl groups of the Tp* units of a neighbouring dimer to form a C—H...S hydrogen-bonded chain. The N atoms of the thiocyanate anions interact with the H atoms of the methyl groups of the Tp* units of neighbouring chains, affording a two-dimensional hydrogen-bonded network. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959040 Wed, 22 Jun 2011 23:00:00 +0100 4959040 http://www.medworm.com/index.php?rid=4959039&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgg3258 The structure of catena-poly[[{bis[4-(trimethylammonio)benzenethiolate-κS]mercury(II)}-μ-1,1′-(ethane-1,2-diyl)bis(1H-benzimidazole)-κ2N3:N3′] bis(hexafluoridophosphate) 0.25-hydrate], {[Hg(C16H14N4)(C9H13NS)2](PF6)2·0.25H2O}n, contains a one-dimensional zigzag chain. The HgII cation is coordinated by two S atoms of two 4-(trimethylammonio)benzenethiolate (Tab) ligands and by two N atoms from two different 1,1′-(ethane-1,2-diyl)bis(1H-benzimidazole) ligands, forming a distorted seesaw-shaped coordination geometry. The F atoms of the hexafluoridophosphate anion interact with the H atoms of the Tab ligand, generating a two-dimensional network. Furthermore, this layer is connected to neighbouring layers via H...Ï€ interactions, thereby forming a three-dimensional hydrogen-bonded str... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959039 Wed, 22 Jun 2011 23:00:00 +0100 4959039 http://www.medworm.com/index.php?rid=4959038&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffg3220 The title compound, [Ti2Cl6(C2H6N)2(C2H7N)2], is a binuclear octahedral complex lying about an inversion centre. There are four different chloride environments, two terminal [Ti—Cl = 2.2847 (5) and 2.3371 (5) Å] and two bridging [Ti—Cl = 2.4414 (5) and 2.6759 (5) Å], with the Ti—Cl distances being strongly influenced by both the ligand trans to the chloride and whether or not the chloride anion is bridging between the two TiIV centres. The compound forms a two-dimensional network in the solid state, with weak intermolecular C—H...Cl interactions giving rise to a planar network in the (10\overline{2}) plane. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959038 Wed, 22 Jun 2011 23:00:00 +0100 4959038 http://www.medworm.com/index.php?rid=4959037&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fku3048 A rhombohedral modification of europium pentanickel indide, r-EuNi5In, crystallizes in the R\overline{3}m space group and adopts the UCu5In structure type. The structure is closely related to the hexagonal, h-EuNi5In, form (CeNi5Sn type). Both EuNi5In modifications are composed of CaCu5 (EuNi5)-, MgCu2 (InNi2)- and NiAs (EuNi)-type slabs in a 1:2:1 ratio. The atoms in the structure have high coordination numbers, viz. 20 and 18 for europium, 14 for indium, and 12 and 10 for nickel. The structure features a two-dimensional network of 2∞[Ni8] tetrahedral clusters arranged in the ab plane. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4959037 Wed, 22 Jun 2011 23:00:00 +0100 4959037 http://www.medworm.com/index.php?rid=4944004&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3386 This study was undertaken in a search for relationships between activity and specific intramolecular interactions, especially conjugations and hydrogen-bond contacts, and the molecular structures were compared with respective amine analogues, also active against the pathogen. Despite the differences between the amine and carbonyl groups with opposite functions in the hydrogen bond, the two types of structure show a surprisingly similar planar geometry, mostly due to the conjugations aided by the bifurcated intramolecular hydrogen-bond contact between the N—H group of the central hydrazide group as donor and a pyrazine N atom and an S atom of the dithio function as acceptors. Planarity was suggested to be crucial for the tuberculostatic activity of these compounds. The N-methylated deriva... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4944004 Thu, 16 Jun 2011 23:00:00 +0100 4944004 http://www.medworm.com/index.php?rid=4944003&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fuk3030 In the title compound, C10H7NO3·H2O, the zwitterionic organic molecules and the water molecules are connected by N—H...O and O—H...O hydrogen bonds to form ribbons, and π–π stacking interactions expand these ribbons into a three-dimensional net. The energies of these hydrogen bonds adopt values typical for mildly weak interactions (3.33–7.75 kcal mol−1; 1 kcal mol−1 = 4.184 kJ mol−1). The total π–π stacking interactions between aromatic molecules can be classified as mildly strong (energies of 15.3 and 33.9 kcal mol−1), and they are made up of multiple constituent π–π interactions between six-membered rings. The short intermolecular C—H...O contact between two zwitterionic molecules is nonbonding in character. (Source: Acta Crystallographica Sec... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4944003 Thu, 16 Jun 2011 23:00:00 +0100 4944003 http://www.medworm.com/index.php?rid=4944002&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fbg3138 The novel title coordination polymer, {[Cu(C8H4O4)(C10H9N3)]·H2O}n, synthesized by the slow-diffusion method, takes the form of one-dimensional zigzag chains built up of CuII cations linked by benzene-1,3-dicarboxylate (ipht) anions. An exceptional characteristic of this structure is that it belongs to a small group of metal–organic polymers where ipht is coordinated as a bridging tridentate ligand with monodentate and chelate coordination of individual carboxylate groups. The CuII cation has a highly distorted square-pyramidal geometry formed by three O atoms from two ipht anions and two N atoms from a di-2-pyridylamine (dipya) ligand. The zigzag chains, which run along the b axis, further construct a three-dimensional metal–organic framework via strong face-to-face π–π interacti... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4944002 Thu, 16 Jun 2011 23:00:00 +0100 4944002 http://www.medworm.com/index.php?rid=4944001&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fky3002 The amino-functionalized helical chiral one-dimensional coordination polymer catena-poly[[bis(pyridine-κN)zinc(II)]-μ-2-aminobenzene-1,4-dicarboxylato-κ4O1,O1′:O4,O4′], [Zn(C8H5NO4)(C5H5N)2]n, has an extended structure that is assembled from 2-aminobenzene-1,4-dicarboxylate anions and Zn2+ cations and which presents a left-handed 43 helix with a pitch of 25.6975 (9) Å. All the pyridine rings and all the amino groups point away from the helix to generate a hollow tube with a cross-section of approximately 8 × 8 Å running parallel to the crystallographic c direction. Each single-stranded helix is interdigitated with four neighbouring helices via N—H...O hydrogen bonds, which gives rise to a dense homochiral three-dimensional supramolecular network. (Source: Acta Crystallogr... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4944001 Thu, 16 Jun 2011 23:00:00 +0100 4944001 http://www.medworm.com/index.php?rid=4944000&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsq3290 In the title cadmium(II) complex, [Cd(C8H4O5)(C14H14N4)(H2O)]n, the 5-hydroxybenzene-1,3-dicarboxylate (5-OH-1,3-bdc) and 1,4-bis(imidazol-1-ylmethyl)benzene (1,4,-bix) ligands bridge water-coordinated CdII atoms to generate a three-dimensional network. Two carboxylate groups from different ligands function as O,O′-chelates, while two imidazole N atoms from different ligands coordinate in a monodentate fashion, and one water molecule completes the seven-coordinate pentagonal bipyramid around the CdII atom, in which the N atoms occupy the axial sites and the O atoms occupy the equatorial sites. The overall architecture is a twofold interpenetrated CdSO4-type framework. The two crystallographically equivalent frameworks are linked by O—H...O hydrogen bonds between the water, hydroxy and ... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4944000 Thu, 16 Jun 2011 23:00:00 +0100 4944000 http://www.medworm.com/index.php?rid=4943999&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3411 The title compounds, [1,2-bis(isopropylsulfanyl)ethane-2κ2S,S′]octachlorido-1κ5Cl,2κ3Cl-μ-oxido-ditantalum(V), [Ta2Cl8O(C8H18S2)], (I), and μ-dimethyldiselane-κ2Se:Se′-μ-oxido-bis[tetrachloridotantalum(V)], [Ta2Cl8O(C2H6Se2)], (II), contain six-coordinate TaV centres linked by a nonlinear oxide bridge. Compound (I) contains one TaV centre bonded to a chelating dithioether and three terminal chloride ligands, with the second TaV centre bonded to five terminal chloride ligands. In (II), two tetrachloridotantalum(V) residues are bridged by the diselenide, giving a puckered five-membered Ta/O/Ta/Se/Se ring. The Ta—O distances in the bridges are short in both compounds, indicating that significant multiple-bond character is retained despite the deviation from linearity, and the bon... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4943999 Thu, 16 Jun 2011 23:00:00 +0100 4943999 http://www.medworm.com/index.php?rid=4900867&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsk3409 The solid-state structure of the title compound, [Cu(C19H13F2N2)(C5H9N)2], shows that the CuI centre adopts a distorted tetrahedral coordination geometry, being coordinated by two N atoms of the 6-aminofulvene-2-aldimine (AFA) chelating ligand and by the bridgehead C atoms of the two isocyanide ligands. The cyclopentadienyl and imine components of the AFA ligand are approximately coplanar, with an angle between the planes of 5.00 (3)°. The Cu atom lies 0.6460 (3) Å above the imine plane defined by the N and C atoms of the seven-membered metallocycle. There is also an uncommon C—H...Cu anagostic interaction, with an intramolecular Cu...H distance of 2.67 Å, which is less than the sum of the van der Waals radii. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4900867 Mon, 06 Jun 2011 17:25:51 +0100 4900867 http://www.medworm.com/index.php?rid=4900871&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fsf3150 Two arylsulfonamide derivatives, N-(4-acetylphenyl)benzenesulfonamide, C14H13NO3S, and N-(4-acetylphenyl)-2,5-dichlorobenzenesulfonamide, C14H11Cl2NO3S, differing by the absence or presence of two chloro substituents on one of the phenyl rings, were synthesized and characterized in order to establish structural relationships and the role of chloro substitution on the molecular conformation and crystal assembly. Both arylsulfonamides form inversion-related dimers through C—H...Ï€ and π–π interactions. These dimers pack in a similar way in the two structures. The substitution of two H atoms at the 2- and 5-positions of one phenyl ring by Cl atoms did not substantially alter the molecular conformation or the intermolecular architecture displayed by the unsubstituted sulfonamide. The str... Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4900871 Fri, 03 Jun 2011 23:00:00 +0100 4900871 http://www.medworm.com/index.php?rid=4900870&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Fgd3393 In the title racemic hemihydrated solvatomorph of carvedilol (carv), C24H26N2O4·0.5H2O, the asymmetric unit contains two independent organic moieties and one water molecule. Within this 2(carv)·H2O unit, the molecular components are strongly linked by hydrogen bonds and the unit acts as the basic building block for the crystal structure. Interactions parallel to (10\overline{1}) generate hydrogen-bonded layers which are further linked by much weaker C—H...N/O interactions. The conformations of the organic molecules, as well as the hydrogen-bonding interactions connecting them, are compared with other related structures in the literature. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4900870 Fri, 03 Jun 2011 23:00:00 +0100 4900870 http://www.medworm.com/index.php?rid=4900869&cid=s_37341_59_f&fid=37341&url=http%3A%2F%2Fscripts.iucr.org%2Fcgi-bin%2Fpaper%3Ffa3253 In the crystal structure of the title compound, 2C22H24P+·I82−, the I82− anion is located on a crystallographic inversion centre and consists of two tri-iodide anions linked by di-iodine at angles of 89.92 (4)° to form a planar `Z'-shaped dianion. The octaiodides are linked via long-range interactions [3.877 (11) Å] into infinite polyiodide ribbons. This is the first example of a structure containing an [(o-tolyl)3PMe]+ cation, and the CMe—P—C—CMe torsion angles of −54.0 (11), −51.3 (11) and −48.2 (11)° indicate that the configuration is exo3. (Source: Acta Crystallographica Section C) Acta Crystallographica Section C journals http://www.medworm.com/rss/comments.php?id=4900869 Fri, 03 Jun 2011 23:00:00 +0100 4900869