Journal of Crystallography The latest articles from Hindawi Publishing Corporation © 2014 , Hindawi Publishing Corporation . All rights reserved. Synthesis and Crystal Structure of 1-Methyl-3-(2-pyridyl)imidazolium Hexafluorophosphate Thu, 17 Jul 2014 08:07:20 +0000 Compound 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate was crystallized in monoclinic system with space group and unit cell parameters , , , , and  . The obtained solid state structure of 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate shows CH⋯F type weak interactions and was analyzed. Elango Kandasamy Copyright © 2014 Elango Kandasamy. All rights reserved. Synthesis, Crystal Structure, and Electrical Properties of a New Molybdylarsenate LiNa5K3Mo11As3O45 Sun, 13 Jul 2014 00:00:00 +0000 LiNa5K3Mo11As3O45 is a new inorganic compound. It was synthesized by a solid state method. The crystal structure has been studied by single crystal X-ray analysis. The R-values reached 2.8%. The title compound crystallizes in the triclinic system, space group P-1, with a = 10.550 (2) Å, b = 11.723 (2) Å, c = 17.469 (3) Å, α = 102.35 (3)°, β = 87.61 (2)°, and γ = 111.03 (3)°. The anionic unit [Mo11As3O45]9− is formed by nine MoO6 octahedra, two MoO5 trigonal bipyramids, and three AsO4 tetrahedra. The association of [Mo11As3O45]9− units, running along [010], leads to a one-dimensional framework. Li, K, and Na are located in the space surrounding the anionic ribbons. This material was characterized by SEM microscopy, IR spectroscopy, and powder X-ray diffraction. The electrical conductivity was investigated from 528 K to 673 K by impedance complex followed by DSC spectroscopy. Hamadi Hamza, Mohamed Faouzi Zid, and Ahmed Driss Copyright © 2014 Hamadi Hamza et al. All rights reserved. Quantitative Crystal Structure Analysis of (E)-1-[(2-Chloro-1,3-thiazol-5-yl)methyl]-3-methyl-2-nitroguanidine Sun, 15 Jun 2014 10:51:19 +0000 The crystal structure of a biologically active (E)-1-[(2-chloro-1,3-thiazol-5-yl)methyl)]-3-methyl-2-nitroguanidine with molecular formula C6H8N5O2ClS has been investigated based on the molecular conformation and the supramolecular packing in terms of intermolecular interactions involving N–H⋯O, N–H⋯N, and C–H⋯O–N (nitro group), C–H⋯N (thiazol) hydrogen bonds, offset π–π stacking, C–H⋯π and N(–NO2)⋯C=N intermolecular interactions. Furthermore, a short C–Cl⋯O–N contact is also present which contributes towards the crystal packing. The lattice energy of the title compound has been calculated using the PIXEL approach (the Coulomb-London-Pauli (CLP) model) and compared with periodic calculations performed using CRYSTAL09. In addition, Hirshfeld surface analysis and fingerprint plots provide a platform for the evaluation of the contribution of different intermolecular interactions towards the packing behaviour. Dhananjay Dey, Chetan S. Shripanavar, Kaushik Banerjee, and Deepak Chopra Copyright © 2014 Dhananjay Dey et al. All rights reserved. () and ()-1,4-Diphenyl-2-(2-phenyl-1-benzo[]imidazol-1-yl)but-2-ene-1,4-dione Tue, 27 May 2014 05:57:31 +0000 The title compound C29H20N2O2 adopts and geometry about olefinic C14–C22 bond, where the benzoyl group at C22 and benzimidazole group at C14 lie on the opposite sides and on the same side across the olefinic bond, respectively. In configuration the phenyl groups of both benzoyl moieties are almost perpendicular to benzimidazole ring while the phenyl of benzimidazole at C7 is oriented at an angle of 30.76 (5)° to the mean plane of the benzimidazole ring. On the other hand in configuration the phenyl group at C7 of benzimidazole ring is oriented at an angle of 38.44 (7)° to the mean plane of the benzimidazole ring while the phenyl rings of benzoyl moieties at C15 and C23 lie at an angle of 16.07 (9)° and 40.29 (6)°, respectively, to the mean plane of the benzimidazole ring. The observed bond distances and bond angles fall within the normal accepted range of values. Sarfaraz Ahmed, Niyaz A. Mir, Tariq A. Shah, Waseem Raza, M. Muneer, and Nigam P. Rath Copyright © 2014 Sarfaraz Ahmed et al. All rights reserved. Synthesis, Characterization, and Crystal Structure of Negundoside (2′-p-Hydroxybenzoyl Mussaenosidic Acid) Sun, 25 May 2014 11:23:02 +0000 The structure of title compound Negundoside (2′-p-hydroxybenzoyl mussaenosidic acid) was established by spectral and X-ray diffraction studies. The compound crystallizes in the monoclinic crystal system with space group P21 having unit cell parameters: (5) Å, (4) Å, (5) Å, (4)°, and . The crystal structure was solved by direct method using single crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R value of 0.0520 for 3389 observed reflections. Suresh Sharma, B. D. Gupta, Rajni Kant, and Vivek K. Gupta Copyright © 2014 Suresh Sharma et al. All rights reserved. Crystal Structure, Spectral Studies, and Hirshfeld Surfaces Analysis of 5-Methyl-5H-dibenzo[b,f]azepine and 5-(4-Methylbenzyl)-5H-dibenzo[b,f]azepine Mon, 19 May 2014 08:47:23 +0000 The compounds, 5-methyl-5H-dibenzo[b,f]azepine (1) and 5-(4-methylbenzyl)-5H-dibenzo[b,f]azepine (2), were synthesized and characterized by spectral studies, and finally confirmed by single crystal X-ray diffraction method. The compound 1 crystallizes in the orthorhombic crystal system in Pca21 space group, having cell parameters (18) Å, (18) Å, (13) Å, and and (3) Å3. And the compound 2 crystallizes in the orthorhombic crystal system and space group Pbca, with cell parameters (5) Å, (2) Å, (7) Å, and and (16) Å3. The azepine ring of both molecules 1 and 2 adopts boat conformation with nitrogen atom showing maximum deviations of 0.483 (2) Å and 0.5025 (10) Å, respectively. The C–H⋯π short contacts were observed. The dihedral angle between fused benzene rings to the azepine motif is 47.1 (2)° for compound 1 and 52.59 (6)° for compound 2, respectively. The short contacts were analyzed and Hirshfeld surfaces computational method for both molecules revealed that the major contribution is from C⋯H and H⋯H intercontacts. Madan Kumar Shankar, Basavapattana C. Manjunath, Koravangala Shivakumar Vinay Kumar, Kudigana J. Pampa, Marilinganadoddi P. Sadashiva, and Neartur K. Lokanath Copyright © 2014 Madan Kumar Shankar et al. All rights reserved. Crystal Structures of Ethyl 4-(4-Florophenyl)-6-phenyl-2-substituted-3-pyridinecarboxylates Sun, 04 May 2014 08:15:12 +0000 Three substituted pyridinecarboxylates were synthesized; (I) ethyl 2-bromo-4-4(fluorophenyl)-6-phenyl-3-pyridinecarboxylate, C20H15BrFNO2, (II) ethyl 4-(4-fluorophenyl)-2-(4-morpholinyl)-6-phenyl-3-pyridinecarboxylate, C24H23FN2O3, and (III) ethyl 4-(4-fluorophenyl)-6-phenyl-2-(1-piperidinyl)-3-pyridinecarboxylate, C25H25FN2O2. It was found that compound (I) belongs to the orthorhombic system with space group P212121, compound (II) to the monoclinic system with space group P21/c, and compound (III) to the monoclinic system with space group C2/c. The morpholine ring in (II) and piperidine ring in (III) have the shape of the distorted chair configuration. ElSayed M. Shalaby, Aisha M. Moustafa, Adel S. Girgis, and Aida M. ElShaabiny Copyright © 2014 ElSayed M. Shalaby et al. All rights reserved. Synthesis, Characterization, and X-Ray Structure of Bis(O-butyldithiocarbonato)bis(3-ethyl pyridine)nickel(II) Wed, 30 Apr 2014 08:39:31 +0000 A new series of additional complexes of bis(O-butyldithiocarbonato)nickel(II) with ethylpyridines have been prepared and characterized by physicochemical techniques like elemental analysis, molar conductance measurements, TGA-DTA and UV-visible electronic spectroscopy, and IR-spectral data. The structure of [Ni(S2COC4H9)2(C7H9N)2] has been established by X-ray crystallography. The complex crystallizes in the monoclinic space group P1/n with unit cell parameters , , and  Å and , , and °. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. Crystal structure was solved by direct methods and refined by full matrix least squares procedures to a final -value of 0.0545 for 1984 observed reflections. The butyl chain is disordered over two sets of sites, with occupancy ratio of 0.572 : 0.427. Inderjeet Kaur, Kuldeep Singh, Gurvinder Kaur, Renu Sachar, Vivek K. Gupta, and Rajni Kant Copyright © 2014 Inderjeet Kaur et al. All rights reserved. Crystal Structure and Molecular Mechanics Modelling of 2-(4-Amino-3-benzyl-2-thioxo-2,3-dihydrothiazol-5-yl)benzoxazole Sun, 27 Apr 2014 10:05:14 +0000 The crystal structure of the title compound, 2-(4-amino-3-benzyl-2-thioxo-2,3-dihydrothiazol-5-yl)benzoxazole, was determined. The crystal has P1 space group and triclinic system with unit cell parameters a = 5.174(3) Å, b = 6.411(6) Å, c = 12.369(10) Å, α = 86.021(4)°, β = 84.384(5)°, and γ = 77.191(5)°. The structure consists of benzoxazole group connected with benzyl via thiazole (attached with amino and thione). Benzoxazole and thiazole rings are almost planar (maximum deviation at C1, −0.013(3) Å, and C10, 0.0041(3) Å, resp.). The phenyl ring is nearly perpendicular to both thiazole and benzoxazole rings. A network of intermolecular hydrogen bonds and intermolecular interactions stabilizes the structure, forming parallel layers. The molecular geometry obtained using single crystal analysis is discussed along with results of the molecular mechanics modeling (MM), and the results showed the same cis conformation between benzoxazole nitrogen atom and the amino group. Ahmed F. Mabied, Elsayed M. Shalaby, Hamdia A. Zayed, Esmat El-Kholy, and Ibrahim S. A. Farag Copyright © 2014 Ahmed F. Mabied et al. All rights reserved. Synthesis, X-Ray Crystallography, Thermal Analysis, and DFT Studies of Ni(II) Complex with 1-Vinylimidazole Ligand Mon, 14 Apr 2014 16:20:47 +0000 The paper presents a combined experimental and computational study of hexa(1-vinylimidazole)Ni(II) perchlorate complex. The complex was prepared in the laboratory and crystallized in the monoclinic space group P21/n with (5), (8), (9) Å, , (5), and . The complex has been characterized structurally (by single-crystal X-Ray diffraction) and its molecular structure in the ground state has been calculated using the density functional theory (DFT) methods with 6-31G(d) and LanL2DZ basis sets. Thermal behaviour and stability of the complex were studied by TGA/DTA analyses. Besides, the nonlinear optical effects (NLO), molecular electrostatic potential (MEP), frontier molecular orbitals (FMO), and the Mulliken charge distribution were investigated theoretically. Fatih Şen, Ramazan Şahin, Muharrem Dinçer, Ömer Andaç, and Murat Taş Copyright © 2014 Fatih Şen et al. All rights reserved. Crystallographic and DFT Studies on Pyrrolo[1,2-c]imidazole Scaffolds Mon, 14 Apr 2014 13:48:01 +0000 The crystal structures of the compounds C15H14N4O2 (1) and C16H16N4O4 (2) are reported and analyzed by single crystal X-ray diffraction technique. Compounds (1) and (2) crystallized in monoclinic space group P21/c and Cc with four molecules in the unit cell, respectively. The unit cell parameters for compound (1) are = 11.4501(15) Å, = 9.7869(11) Å, = 12.3653(15) Å, β = 90.997(11)°, and Volume = 1385.5(3) Å3 and for compound (2) are = 13.865(2) Å, = 6.9538(8) Å, = 16.841(2) Å, β = 98.602(11)°, and Volume = 1605.4(4) Å3. In both compounds (1) and (2), the pyrrolidine ring adopts half-chair conformation. Moreover, both inter- and intramolecular N–H⋯O hydrogen bonds stabilize the crystal structure and play a crucial role in crystal packing. This intermolecular interaction alone constructs chain motif in both compounds. It is also supported by weak intermolecular π-π interaction which is essential for the stability of the crystal packing. Further, the Density Functional Theory (B3LYP) method with standard 6-31G basis set was used in the calculation and calculated geometrical parameter is correlated with the corresponding experimental data. The obtained HOMO and LUMO energies are in negative values indicating that the compounds are in stable state. Manikandan Jayaraman, Rajarathinam Balakrishnan, Kannan Muthu, Manivel Panneerselvam, Vasuki Gnanasambandam, and Krishna Ramadas Copyright © 2014 Manikandan Jayaraman et al. All rights reserved. Synthesis, Crystal Structure, and Hirshfeld Surface Analysis of Ciprofloxacin-Salicylic Acid Molecular Salt Mon, 07 Apr 2014 13:46:38 +0000 In the present study, ciprofloxacin-salicylic acid molecular salt has been synthesized and preliminarily characterized by FT-IR spectroscopy. The single crystal X-ray diffraction (SCXRD) reveals the proton transfer from carboxylic acid group of salicylic acid to piperazine moiety in ciprofloxacin confirming the formation of new molecular salt. The molecular packing of the molecular salt is mainly supported by N+–H⋯O−, O–H⋯O, C–H⋯F, C–H⋯, and interactions. The 3D Hirshfeld surfaces and the associated 2D fingerprint plots were investigated for intermolecular hydrogen bonding interactions. Ravikumar Nagalapalli and Shankar Yaga Bheem Copyright © 2014 Ravikumar Nagalapalli and Shankar Yaga Bheem. All rights reserved. Synthesis and Structural Study of the (N,N,N′,N′-Tetraethylethylenediamine)CdFe(CO)4 Dimer Mon, 07 Apr 2014 06:28:14 +0000 The new [(teeda)CdFe(CO)4]2 complex has been isolated from the reaction of with tetraethylethylenediamine. Unlike previous structural reports of ligand adducts of complexes, which have all been trimeric species composed of six-membered Cd3Fe3 rings, the teeda complex crystallized as a dimer, analogous to [(2,2-bpy)ZnFe(CO)4]2. As in the zinc dimer, significant distortion arises from steric interactions between the axial carbonyl ligands on opposing iron centers. The complex sits on an inversion center, leading to two independent Cd–Fe distances, 2.7244(6) and 2.7433(6) Å, and crystallizes in the monoclinic space group P21/a with a = 14.8546(2) Å, b = 15.1647(3) Å, c = 15.5252(3) Å, β = 90.9517, and = 1.719 g/cm3 at 150(1) K. Torsten Kolb, Atta M. Arif, and Richard D. Ernst Copyright © 2014 Torsten Kolb et al. All rights reserved. Crystallographic and Computational Study of Purine: Caffeine Derivative Sun, 30 Mar 2014 07:31:10 +0000 The crystal structure of substituted purine derivative, 8-(3-butyl-4-phenyl-2,3-dihydrothiazol-2-ylidene)hydrazino-3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-diones, caffeine derivative, has been determined. It crystallized in monoclinic system and space group P21/c with unit cell parameters a = 15.2634 (9), b = 13.4692 (9), c = 11.9761 (7) Å, and β = 108.825 (3)°. Although each constituting moiety of the structure individually is planar, nonplanar configuration for the whole molecule was noticed. Molecular mechanics computations indicated the same nonplanar feature of the whole molecule. A network of intermolecular hydrogen bonds contacts and π interactions stabilized the structure. Ahmed F. Mabied, Elsayed M. Shalaby, Hamdia A. Zayed, and Ibrahim S. A. Farag Copyright © 2014 Ahmed F. Mabied et al. All rights reserved. Crystal and Molecular Structure of 1,1-Bis(methylthio)-5-(4-chlorophenyl)-1,4-pentadien-3-one Wed, 26 Mar 2014 11:59:15 +0000 The 1,1-bis(methylthio)-5-(4-chlorophenyl)-1,4-pentadien-3-one compound crystallizes in the space group C2/c with unit cell parameters  Å,  Å,  Å, and ∘. The structure was solved by direct methods and refined to an R-factor of 0.0593. Due to the steric interaction between the two methyl groups, one of the methylthio groups is in cis conformation with C11–C10 double bond and the other is in trans conformation. The cinnamoyl group on the carbonyl carbon atom effects more delocalization of the electrons within the molecule so that the structure is highly conjugated and planar. Bubbly S. Gudennavar, Shivappa B. Gudennavar, and Viswam Dhanya Copyright © 2014 Bubbly S. Gudennavar et al. All rights reserved. Synthesis and Structural Study of the Bis(ethylenediamine)CdFe(CO)4 Monomer Tue, 25 Mar 2014 11:15:22 +0000 The new complex has been isolated from the crystallization of from ethylenediamine (en). The cadmium center bears square-pyramidal coordination, with the iron atom occupying the apical position. The iron coordination may be described either as trigonal bipyramidal, with the cadmium atom being in an axial position, or as monocapped (by cadmium) tetrahedral. The Cd-Fe distance was found to be 2.6250(2) Å. The complex crystallizes in the monoclinic space group with  Å,  Å,  Å, and at 150(1) K. Marcus Tofanelli, Atta M. Arif, and Richard D. Ernst Copyright © 2014 Marcus Tofanelli et al. All rights reserved. Synthesis and Molecular Structure of cis-Tetracarbonyl[N-(diphenylphosphino-kP)-naphthalen-1-yl-P,P-diphenylphosphinous amide-kP]chromium(0) Mon, 24 Mar 2014 12:01:59 +0000 The reaction of N,N-bis(diphenylphosphanyl)naphthylamine C10H7-1-N(PPh2)2 with (C5H10NH)2Cr(CO)4 (1 : 1 molar ratio) in dichloromethane afforded cis-[Cr(CO)4C10H7-1-N(PPh2)2] (1). This complex was crystallized in the monoclinic space group P21/n. The structure was solved by direct methods and refined by full-matrix least squares techniques to an factor of 0.0313 for 6488 observed reflections. The Cr-metal is coordinated by four terminal CO molecules and a P,P′-bidentate N,N-bis(diphenylphosphanyl)naphthylamine ligand in a distorted octahedral array. The N-atom adopts a planar geometry with the two P-atoms and C-atom attached to it. The four-membered metallacycle ring P2CrN is nearly planar. Harbi Tomah Al-Masri Copyright © 2014 Harbi Tomah Al-Masri. All rights reserved. Crystallization and Structural Characterization of Dimeric and Trimeric Forms of (Neocuproine)CdFe(CO)4 Tue, 11 Mar 2014 15:45:23 +0000 The previously reported (neocuproine)CdFe(CO)4 has been found to crystallize as either a dimer or a trimer depending on the procedure used. These species exist as nearly planar four- and six-membered rings composed of alternating cadmium and iron atoms. The trimeric form is reasonably similar to its 2,2′-bipyridyl analogue, while the dimeric form had not been observed previously for a CdFe(CO)4 complex. The space group for the dimeric isomer is C2/c, with (3), (2), (2)  Å, and (11)°, while for the trimeric isomer the space group is P, with (1), (1), (2)  Å, (3)°, (4)°, and (5)°. Torsten Kolb, Atta M. Arif, and Richard D. Ernst Copyright © 2014 Torsten Kolb et al. All rights reserved. Synthesis and X-Ray Crystal Structure of Two Acridinedione Derivatives Thu, 27 Feb 2014 13:58:00 +0000 The two acridinedione derivatives 1 [3,3,6,6-tetramethyl-9-(4-methoxyphenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione (C24H29NO3)] and 2 [3,3,6,6-tetramethyl-9-(4-methylphenyl)-3,4,6,7,9,10-hexa-hydro-2H,5H-acridine-1,8-dione (C24H29NO2)] were synthesized and their crystal structures were determined by direct methods. The asymmetric unit of compound 1 contains two independent molecules. The 1,4-dihydropyridine (DHP) ring adopts boat conformation in both 1 and 2. In 1 the dione rings exist in sofa conformation (for both the crystallographically independent molecules) while the corresponding rings in 2 adopt half chair and sofa conformations, respectively. The crystal packing is stabilized by intermolecular N–H⋯O and C–H⋯O interactions in compound 1 and N–H⋯O interactions in compound 2. Dalbir Kour, D. R. Patil, M. B. Deshmukh, Vivek K. Gupta, and Rajni Kant Copyright © 2014 Dalbir Kour et al. All rights reserved. Synthesis, Characterization, and X-Ray Crystal Structure of Bis(O-amyl dithiocarbonato-κ2S,S′)bis(4-cyanopyridine-κN)nickel(II) Mon, 17 Feb 2014 14:30:06 +0000 The [Ni(S2CO-n-C5H11)2(C6H4N2)2] adduct of 4-cyanopyridine with [Ni(S2CO-n-C5H11)2] was synthesized and characterized by elemental analysis, magnetic susceptibility measurement, IR, electronic spectral data, and X-ray diffraction analysis. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. The title compound exhibits magnetic moment value (3.20 B.M) which is in agreement with magnetic moment values observed for paramagnetic octahedral complexes of nickel(II). The title complex crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 11.455(5), b = 9.602(4), and c = 26.374(1) Å. Crystal structure was solved by direct methods and refined by full matrix least-squares procedures to a final R value of 0.0499 for 2004 observed reflections. The amyl chain is disordered over two sets of sites, with occupancy ratios of 0.595 : 0.405. Infinite long chains of molecules are formed with the help of C–H⋯N hydrogen bond. Kuldeep Singh, Sanjay Kapoor, Renu Sachar, Vivek K. Gupta, and Rajni Kant Copyright © 2014 Kuldeep Singh et al. All rights reserved. Structural Studies of and Thu, 13 Feb 2014 10:07:21 +0000 The structures of and have been determined (py = pyridine; THF = tetrahydrofuran). Each is composed of a six-membered ring having alternating cadmium and iron centers. The presence of the more strongly basic amine ligands in the former led to a greater contribution of an ionic resonance form, which resulted in overall longer Cd–Fe bonds and a greater contribution of a bicapped tetrahedral coordination geometry about iron. Thus, the Cd–Fe distances range from 2.5679(4) to 2.6501(1) Å for the THF complex versus 2.6445(8) to 2.6833(7) Å for the py complex. Similarly, the Fe–Cd–Fe and Cd–Fe–Cd angles for the THF complex fell in respective ranges of 139.03(2)–157.27(2)° and 84.41(1)–99.79(1)°, as compared to 135.31(3)–139.51(4)° and 102.52(3)–104.62(4)° for the py complex. The space group for the former compound is Pbcn, with = 12.2678(2), = 22.4601(5), and = 17.0039(4) Å, while for the THF complex, the space group is , with = 10.7297(2), = 20.4961(2), = 18.7464(3) Å, and = 94.2715(6)°. Bryce Anderson, Atta M. Arif, and Richard D. Ernst Copyright © 2014 Bryce Anderson et al. All rights reserved. Hydrogen Bonds between Acidic Protons from Alkynes (C–H···O) and Amides (N–H···O) and Carbonyl Oxygen Atoms as Acceptor Partners Sun, 12 Jan 2014 09:46:17 +0000 Crystals of tert-butyl (2S)-2-(prop-2-yn-1-ylcarbamoyl)pyrrolidine-1-carboxylate (Boc-L-Pro-NHCH2CCH) have been obtained. The title compound crystallizes easily as sharp needles in orthorhombic system, space group P 21 21 21 with a = 9.2890(2), b = 9.7292(2), c = 15.7918(4) Å, V = 1427.18(6) Å3, and Z = 4. The main feature of the structure is the orientation of the carbamate and amide. Their dipoles add up and the molecule displays an electric dipole moment of 5.61 D from B3LYP/6-31G(d) calculations. The antiparallel H bonding of amides and the alignment of dipoles induce columnar stacking (the dipole moment along the columnar a axis is 4.46 D for each molecule). The other components across the other axes are, therefore weaker, (3.17 D and 1.23 D along the b and c axes, resp.). The resulting anisotropic columns pack side by side, in an antiparallel fashion mostly by (alkyne) CH···O=C (carbamate) interactions. Pierre Baillargeon, Tommy Lussier, and Yves L. Dory Copyright © 2014 Pierre Baillargeon et al. All rights reserved. Structure of N-(3,4-Dimethoxyphenyl)pyrido[3′,2′:4,5]-thieno[3,2-d]pyrimidin-4-amine, a New Inhibitor of CLK1 and DYRK1A Kinases Mon, 23 Dec 2013 14:37:59 +0000 The complete crystal structure of N-(3,4-dimethoxyphenyl)pyrido[3′,2′:4,5]thieno[3,2-d]pyrimidin-4-amine, synthesized via a Dimroth rearrangement and designed as new inhibitor of CLK1 and DYRK1A kinases, was established by a single-crystal X-ray diffraction. The crystal is orthorhombic, space group Pca21; , ,  Å, °,  Å3, and , C17H14N4O2S. Solid-state data could be used to enlighten the biological mechanism of action. Jean Guillon, Mathieu Marchivie, Yvonnick Loidreau, Noël Pinaud, and Thierry Besson Copyright © 2013 Jean Guillon et al. All rights reserved. Molecular Structure of 1,2-Dibenzoyl-1′,2′,3′,4′,5′-pentamethylruthenocene Dioxime Hydrochloride Tue, 10 Dec 2013 08:32:07 +0000 The dioxime of 1,2-dibenzoylpentamethylruthenocene is synthesized from its parent diketone and hydroxylamine under standard basic conditions. The slightly air-sensitive product is crystallized in the form of its monohydrochloride. The solid-state structure is the first example of a dioxime monohydrochloride showing a typical metallocene core with peripheral intramolecular N–H–N and O–H–Cl hydrogen bonding. Stefan Vanicek, Daniela Eisenstecken, Holger Kopacka, Klaus Wurst, and Benno Bildstein Copyright © 2013 Stefan Vanicek et al. All rights reserved. Synthesis and Crystal Structure of trans-Diiodobis(piperidine-1-carbonitrile)platinum(II) Wed, 04 Dec 2013 09:33:21 +0000 Treatment of dichlorobis(piperidine-1-carbonitrile)platinum(II) with potassium iodide in water/methanol mixture results in the halide ligand exchange giving novel trans-diiodobis(piperidine-1-carbonitrile)platinum(II) complex. The reaction proceeds under mild conditions (20°C, 40 min) giving trans-[PtI2(NCNC5H10)2] in 70% isolated yield. The iodide complex was characterized by IR, 1H and 13C NMR spectroscopies, and high resolution ESI-MS, and its structure was determined by a single crystal X-ray diffraction. Aleksey L. Mindich, Matti Haukka, and Nadezhda A. Bokach Copyright © 2013 Aleksey L. Mindich et al. All rights reserved. The Use of a Flexible Calix[4]arene Template to Stabilize a Cyclooctatetraindiyl Samarium-Potassium Complex Tue, 26 Nov 2013 10:35:44 +0000 A sandwich compound of cyclooctatetraendiyl (COT)2− samarium-potassium was synthesized and analyzed using a flexible calix[4]arene dianion. This compound, [p-tBu-calix[4]-(OMe)2(O)2]arenediyl-samarium-(η8-cyclooctatetraendiyl)-potassium (tetrahydrofurane)3, is constructed as a linear sequence L-Sm--K-, where L, , and are specific ligands with L = O,O-dimethyl-calix[4]arene2−, = cyclo-octatetraendiyl, and = tetrahydrofurane templates. Geoffroy Guillemot, Euro Solari, Carlo Floriani, and Thierry Prangé Copyright © 2013 Geoffroy Guillemot et al. All rights reserved. 16α-Hydroxyfriedelin and 3-Oxo-16-methylfriedel-16-ene as Building Blocks: Crystal Structure and Hirshfeld Surfaces Decoding Intermolecular Contacts Thu, 24 Oct 2013 11:32:59 +0000 In this paper the importance of C–H⋯O intermolecular hydrogen bonds and van der Waals forces in crystal packing stabilization of 16α-hydroxyfriedelin (1) and 3-oxo-16-methylfriedel-16-ene (2) is described. Compound 1 is a natural product isolated from the hexane extract of Salacia elliptica branches, whereas compound 2 is obtained from compound 1 after dehydration accompanied by methyl migration of C-17 to C-16. The single-crystal X-ray diffraction experiments for 1 and 2 were carried out at 150 K, and the crystallographic study demonstrated that these compounds crystallize in noncentrosymmetric space groups, with 1 showing an orthorhombic P212121 space group and 2 a monoclinic P21 one. Compounds 1 and 2 are composed of five fused six-membered rings presenting a chair conformation, except for the central ring of 2, which adopts a half-chair conformation. In addition, the intra- and intermolecular parameters were studied using CCDC MOGUL analyses and Hirshfeld surfaces. Rodrigo S. Corrêa, Lucienir P. Duarte, Grácia D. F. Silva, Djalma M. de Oliveira, Javier Ellena, and Antônio C. Doriguetto Copyright © 2013 Rodrigo S. Corrêa et al. All rights reserved. Crystal Structure of Apraclonidine Hydrochloride Wed, 23 Oct 2013 10:53:33 +0000 Apraclonidine is used for the treatment of postsurgical elevated intraocular pressure. The crystal structure of its hydrochloride, C9H10Cl2N4·HCl, was determined by X-ray analysis. The crystal belongs to space group with the cell dimensions , ,  Å, and °. The final (all reflections) value is 0.053. Apraclonidine has a more twisted structure than its related drug of clonidine. The nitrogen atom bridging the two rings is protonated. Noriaki Hirayama Copyright © 2013 Noriaki Hirayama. All rights reserved. Bis(ammonium) Zoledronate Dihydrate Thu, 03 Oct 2013 15:45:18 +0000 Neutralization of 2-(1-imidazole)-1-hydroxyl-1,1′-ethylidenediphosphonic acid (zoledronic acid) by an excess of ammonia yielded bis(ammonium) zoledronate dihydrate, {, 2(H4N+), 2(H2O)}. The product is readily soluble in water and forms monocrystals for which the X-ray structural analysis was carried out. The zoledronic anion is of double negative charge due to deprotonation of three P–OH groups and protonation of the nitrogen in the imidazole ring. The structure is stabilized by extensive network of N–H⋯O and O–H⋯O hydrogen bonds expanding through the crystal in plane (002). The imidazole ring is involved in - stacking interactions with its symmetry equivalents related by inversion centers at (1 0 0) and (1 1/2 0), with distances between centroids (Cg–Cg) of 3.819 (2) and 3.881 (2) Å, respectively. Małgorzata Sikorska and Jarosław Chojnacki Copyright © 2013 Małgorzata Sikorska and Jarosław Chojnacki. All rights reserved. Synthesis and Structural Study of Tris(-pyrazolyl)hexakis(pyrazole)dicobalt(III) Nitrate Sun, 29 Sep 2013 15:54:09 +0000 The new (Hpyz)3Co(μ2-pyz)3Co complex has been isolated as the nitrate salt through a reaction of Co(II) nitrate, Hpyz (pyrazole), triethylamine, and oxygen. The salt crystallizes in the monoclinic space group P21/m with a = 12.5977(3) Å, b = 15.3387(4) Å, c = 14.0800(3) Å, β = 93.0868(15)°, and = 1.464 g/cm3 at 150(1) K. The complex, with pseudo-octahedral coordination about the equivalent cobalt centers, has shorter Co–N distances for the bridging anionic pyz ligands as compared to the neutral Hpyz ligands, with the averages being 1.918(2) and 1.966(4), respectively. The Co–Co separation is 3.568 Å, reflecting the absence of any significant metal-metal interaction. Yifan Shi, Atta M. Arif, and Richard D. Ernst Copyright © 2013 Yifan Shi et al. All rights reserved.