Journal of Crystallography The latest articles from Hindawi © 2017 , Hindawi Limited . All rights reserved. Rapid Creation of Three-Dimensional, Tactile Models from Crystallographic Data Sun, 14 Aug 2016 14:17:04 +0000 A method for the conversion of crystallographic information framework (CIF) files to stereo lithographic data files suitable for printing on three-dimensional printers is presented. Crystallographic information framework or CIF files are capable of being manipulated in virtual space by a variety of computer programs, but their visual representations are limited to the two-dimensional surface of the computer screen. Tactile molecular models that demonstrate critical ideas, such as symmetry elements, play a critical role in enabling new students to fully visualize crystallographic concepts. In the past five years, major developments in three-dimensional printing has lowered the cost and complexity of these systems to a level where three-dimensional molecular models may be easily created provided that the data exists in a suitable format. Herein a method is described for the conversion of CIF file data using existing free software that allows for the rapid creation of inexpensive molecular models. This approach has numerous potential applications in basic research, education, visualization, and crystallography. Nathan B. Fisher, John C. Charbonneau, and Stephanie K. Hurst Copyright © 2016 Nathan B. Fisher et al. All rights reserved. Finite Element Simulation and X-Ray Microdiffraction Study of Strain Partitioning in a Layered Nanocomposite Sun, 26 Jun 2016 09:37:30 +0000 The depth-dependent strain partitioning across the interfaces in the growth direction of the NiAl/Cr(Mo) nanocomposite between the Cr and NiAl lamellae was directly measured experimentally and simulated using a finite element method (FEM). Depth-resolved X-ray microdiffraction demonstrated that in the as-grown state both Cr and NiAl lamellae grow along the direction with the formation of as-grown distinct residual ~0.16% compressive strains for Cr lamellae and ~0.05% tensile strains for NiAl lamellae. Three-dimensional simulations were carried out using an implicit FEM. First simulation was designed to study residual strains in the composite due to cooling resulting in formation of crystals. Strains in the growth direction were computed and compared to those obtained from the microdiffraction experiments. Second simulation was conducted to understand the combined strains resulting from cooling and mechanical indentation of the composite. Numerical results in the growth direction of crystal were compared to experimental results confirming the experimentally observed trends. R. I. Barabash, V. Agarwal, S. Koric, I. Jasiuk, and J. Z. Tischler Copyright © 2016 R. I. Barabash et al. All rights reserved. Synthesis, Crystal Structure, and Characterization of Ternary Copper(II) Complex Derived from N-(salicylidene)-L-valine Mon, 20 Jun 2016 11:30:27 +0000 Ternary Schiff base copper(II) complex [CuL(tmpda)] (where H2L is N-(salicylidene)-L-valine; tmpda is N,N,N′,N′-tetramethyl-1,3-propanediamine) has been characterized by UV-Vis., FTIR, and single crystal XRD. The crystal structure displays a distorted square pyramidal geometry in which Schiff base is bonded to the Cu(II) ion via phenolate oxygen, imine nitrogen, and an oxygen atom of the carboxylate group through the basal plane and the chelating diamine, N,N,N′,N′-tetramethyl-1,3-propanediamine, displays an axial and equatorial mode of binding via NN-donor atoms. Sundaramurthy Santha Lakshmi and Kannappan Geetha Copyright © 2016 Sundaramurthy Santha Lakshmi and Kannappan Geetha. All rights reserved. Structure and Properties of 9,14,15,16,17,18,19,20-Octahydro-9,14[1′,4′]-benzenobenzo[b]triphenylene Mon, 20 Jun 2016 07:07:42 +0000 The compound 9,14,15,16,17,18,19,20-octahydro-9,14[1′,4′]-benzenobenzo[b]triphenylene, C28H24, was prepared by hydrogenation of the photocycloadduct of dibenz[a,c]anthracene and 1,3-cyclohexadiene with Pt/C in ethyl acetate. The X-ray diffraction analysis shows that the compound crystallizes in the monoclinic space group with the geometric parameters of = 11.0090(17) Å, = 13.733(2) Å, = 13.091(2) Å, and = 109.583(13)°. In addition to several close intramolecular contacts involving hydrogens derived from the dibenzanthracene moiety, long interannular C–C single bonds of about 1.593 Å are present. These bonds are shorter by about 0.18 Å than the corresponding bonds in the unsaturated precursor, which can be attributed to reduced strain in the more saturated polycyclic ring system. Anisotropic shielding of the four endo-methylene hydrogens in the 1H NMR spectrum is larger for the two hydrogens lying above the phenanthrene unit, which resonate at 1.03 ppm, than those above the benzenoid ring, which resonate at 1.24 ppm. Theoretical calculations reproduce the geometry with good agreement. Michelle E. Masnovi, John Masnovi, and Steven M. Schildcrout Copyright © 2016 Michelle E. Masnovi et al. All rights reserved. The X-Ray Structure of the Ligand-Free Antibiotic Ristocetin-A Reveals the Role of the Monomer/Dimer Equilibrium in Its Binding Mode Mon, 13 Jun 2016 07:18:45 +0000 Ristocetin-A belongs to the group of the glycoheptapeptide antibiotics. The sulfate salt of ristocetin-A was crystallized in the P21 monoclinic space group with a homodimer in the asymmetric unit. The two subunits are linked back-to-back like the other members of the family via four peptide bonds forming a twisted β-sheet and exposing the binding pockets to the exterior. The two tetrasaccharide parts of this ligand-free antibiotic are in the anti/anti orientations contrary to what was found in the mono- and diliganded ristocetin-A/-(D-Ala-D-Ala) complexes in which the two tetrasaccharides of the dimer are syn/anti. The ligand-free dimer shows however some conformational differences between the two subunits, particularly in the terminal arabinose leading to one extended and one bent conformation of the tetrasaccharide moiety. Comparison between this structure and the two available mono- and diliganded structures confirms that the anti/anti to syn/anti flipping of the tetrasaccharide is a key step in the binding to the D-Ala-D-Ala-containing target sequence and cannot proceed without displacement of the monomer/dimer equilibrium. Thierry Prangé and William B. T. Cruse Copyright © 2016 Thierry Prangé and William B. T. Cruse. All rights reserved. Synthesis and Crystal Structure of C1-Symmetric 3,3′-Bi(1,1′-dinaphthyl-camphopyrazole) Tue, 31 May 2016 13:09:40 +0000 The compound 3,3′-bi(1,1′-dinaphthyl-camphopyrazole) 1, C42H42O4, was obtained in good yield and structurally characterized by 1H and 13C NMR spectroscopy, elemental analysis, and X-ray diffraction. It consists of a 3,3′-bipyrazole group with each pyrazole ring containing a fused camphor group and a naphthalene ring bonded to the adjacent nitrogen atom in the ring. Both of the trimethyl, 5-membered rings of the fused camphor group form an envelope with the apex carbon atom as the flap in each case. In the crystal, weak stacking interactions are observed between nearby 6-carbon rings of the two naphthalene rings linking the molecules into extended chains. Weak π–ring intermolecular interactions are also observed between naphthalene atoms and pyrazole rings from each of the groups helping to stabilize the crystal packing. No classical hydrogen interactions are formed. Jannis Barrera, Victoria A. Smolenski, Jerry P. Jasinski, and Jesús Pastrán Copyright © 2016 Jannis Barrera et al. All rights reserved. Solid State Structure of Bis[(bromo)(dicyclopentadienyl)vanadium(μ2-fluoro)][(bromo)(cyclopentadienyl)vanadium][tetrafluoroborate] Sun, 29 Nov 2015 12:04:03 +0000 The new complex [V(C5H5)2Br]2(μ2-F)2[V(C5H5)Br]+[BF4]− has been isolated from the reaction of vanadocene monobromide with the ferrocenium cation. The complex is a mixed valence compound composed of two V(IV) and one V(III) centers. The V(III) center has one cyclopentadienyl ligand in its coordination sphere, as well as a bromide and two fluoride ligands. Each fluoride ligand is also attached to one of the V(IV) centers, which additionally is coordinated by a bromide and two cyclopentadienyl ligands. The complex crystallizes in the monoclinic space group , with (10) Å, (2) Å, (2) Å, and (8)° at 150(1) K. Lisa M. Chan, Atta M. Arif, and Richard D. Ernst Copyright © 2015 Lisa M. Chan et al. All rights reserved. Crystal Structure, Spectroscopy, SEM Analysis, and Computational Studies of N-(1,3-Dioxoisoindolin-2yl)benzamide Sun, 06 Sep 2015 06:55:57 +0000 The compound N-(1,3-dioxoisoindolin-2yl)benzamide, C15H10N2O3, was prepared by the heating of an ethanolic solution of 2-hydroxy-1H-isoindole-1,3(2H)-dione and 4-chloroaniline. The product was characterised using a combination of IR spectroscopy, SEM, and single crystal X-ray diffraction techniques. In addition to the experimental analysis, theoretical calculations were used to investigate the crystal structure in order to compare experimental and theoretical values. The X-ray diffraction analysis shows that the compound crystallises in the monoclinic space group with the geometric parameters of , , , and °. The crystal structure is held together by a network of N-H⋯O hydrogen bonds involving the carboxamide group. Hakan Bülbül, Yavuz Köysal, Necmi Dege, Sümeyye Gümüş, and Erbil Ağar Copyright © 2015 Hakan Bülbül et al. All rights reserved. Crystal Structures of Two Macrocyclic Bischalcones Possessing 26-Membered Rings Wed, 05 Aug 2015 15:47:23 +0000 Single crystal X-ray diffraction of two macrocyclic bischalcones, namely, (2E,25E)-11,17,33,37-tetraoxapentacyclo[,10.018,23.027,32]dotetraconta-1(42),2,5,7,9,18,20,22,25,27,29,31,38,40-tetradecaene-4,24-dione(1) and (2E,24E)-11,16,32,37-tetraoxapentacyclo[,10.017,22.026,31]dotetraconta-1(42),2,5,7,9,17,19,21,24,26,28,30,38,40-tetradecaene-4,23-dione(2), each containing a 26-membered ring, has been studied. Compound 1 belongs to the monoclinic system, space group C2/c with a = 34.3615(9) Å, b = 12.7995(3) Å, c = 14.6231(3) Å, β = 96.912(2)°,  V = 6,384.6(3) Å3, and Z = 8. Compound 2 is triclinic, space group P-1 with a = 10.066(2) Å, b = 10.670(3) Å, c = 16.590(3) Å, α = 85.95(2), β = 89.244(14), γ = 62.211(13), V = 1572.0(6) Å3, and Z = 2. Intermolecular C–H⋯O hydrogen bonding interactions are present in both compounds. Rina Mondal, Nayim Sepay, Debajyoti Ghoshal, and Asok K. Mallik Copyright © 2015 Rina Mondal et al. All rights reserved. Synthesis and Molecular Structure of 4′,9′,4″,9″-Tetra-tert-butyl-1′,6′,1″,6″-tetramethoxy-2,5-dioxa[3.3]metabiphenylophane Sun, 23 Nov 2014 09:21:32 +0000 A large calixarene-like metacyclophane, 4′,9′,4″,9″-tetra-tert-butyl-1′,6′,1″,6″-tetramethoxy-2,5-dioxa[3.3]metabiphenylophane, was synthesized by an intermolecular condensation reaction of its corresponding bischloromethyl-biphenyl and bishydroxymethyl-biphenyl precursors. After molecular characterization by 1H NMR spectroscopy and mass spectrometry, the compound generated single crystals by recrystallization from a dichloromethane/hexane mixture, facilitating an exact conformational determination via X-ray diffraction analysis. The crystal was found to belong to the monoclinic space group with cell parameters a = 19.908(2) Å, b = 9.7193(11) Å, c = 23.350(3) Å, β = 109.594(1)°, and  g/cm3 at 90 K. The compound adopted quite strained 1,2-alternate-like conformations because its biphenyl parts displayed large dihedral angles and rigidity. The crystal did not incorporate any solvent molecule but its molecular cavity and crystal space were effectively filled by the substituents. Tetsuji Moriguchi, Tatsuya Egami, and Akihiko Tsuge Copyright © 2014 Tetsuji Moriguchi et al. All rights reserved. Synthesis and Molecular Structure of Chiral (2S, 5S)-tert-Butyl 3-Oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate Wed, 05 Nov 2014 08:16:16 +0000 The title compound (2S, 5S)-tert-butyl 3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate was synthesized as a chiral cyclic amino acid ester from the corresponding cis- and trans-5-hydroxypipecolic acid ethyl esters via an intramolecular lactonization reaction without using chiral catalyst or enzyme and without separation by chiral column chromatography. The chiral compound was characterized using 1H NMR spectroscopy and high-resolution mass spectrometry. Its exact structure was then determined via single crystal X-ray diffraction analysis of a single crystal obtained after recrystallization of the compound from ethyl acetate/diethyl ether. The crystal was found to be of the orthorhombic space group P212121 (No. 19, noncentrosymmetric, chiral) with  Å,  Å,  Å, 4 g/cm3, and a Flack parameter of 0.0(5) at 90 K. The compound has a bicyclo[2.2.2]octane structure comprised of lactone and piperidine groups. Tetsuji Moriguchi, Suvratha Krishnamurthy, Toru Arai, and Akihiko Tsuge Copyright © 2014 Tetsuji Moriguchi et al. All rights reserved. Synthesis, Characterization, and Crystal Structure of Pyridinium Tetrakis{1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedionato}lanthanate(III) Complex Tue, 30 Sep 2014 12:26:05 +0000 The reaction of 1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedione with lanthanum(III) trichloride in the presence of pyridine leads to halide ligand exchange, yielding a novel pyridinium tetrakis{1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedionato}lanthanate(III) complex with four polycyclic aromatic hydrocarbon moieties. This reaction easily proceeds under mild conditions (25°C, 24 h) producing the complex in a 90% isolated yield. The complex was characterized by infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, and positive fast atom bombardment mass spectrometry, and its precise structure was determined by single crystal X-ray diffraction. Ultraviolet-visible spectroscopy, fluorescence spectroscopy, and X-ray analysis demonstrated that the four pyrene moieties were independently oriented. Tetsuji Moriguchi, Kenji Yoza, and Akihiko Tsuge Copyright © 2014 Tetsuji Moriguchi et al. All rights reserved. Synthesis and Crystal Structure of Alkynylplatinum(IV) Complex Containing the Terpyridine Ligand Wed, 03 Sep 2014 08:30:11 +0000 Reaction of square planar [(C≡CPh)(tpy)]+ (tpy = 2,2′:6′,2′′-terpyridine) with bromine at low temperature provides a general route for the synthesis of octahedral alkynyl(terpyridine)platinum(IV) complex. In this first example of alkynyl(terpyridine)platinum(IV) complex, the alkynyl group is situated in trans position relative to the central nitrogen atom of the terpyridine ligand, and the two bromido ligands are situated in trans positions; an X-ray structural analysis has been completed for trans(Br)-[Br2(C≡CPh)(tpy)]+. Tsugiko Takase and Dai Oyama Copyright © 2014 Tsugiko Takase and Dai Oyama. All rights reserved. Synthesis, Characterization, and Crystal Structure of [Co4(CH3CO2)2L4]2[BPh4]40.5H2O, Where HL = 4-(Salicylaldiminato)antipyrine Wed, 27 Aug 2014 00:00:00 +0000 The title complex was isolated as a red solid from the reaction of 4-(salicylaldiminato)antipyrine, HL, and cobalt (II) acetate in ethanol. The complex has been characterized by elemental analysis, FTIR, UV-Vis, and X-ray single crystal diffraction. Two crystallographically different cationic units, A and B, of the title complex are found. Both units are essentially isostructural; nevertheless, small differences exist between them. Both units contain four cobalt atoms arranged at the corners of distorted cubane-like core alternatively with phenoxy oxygen of the Schiff base. In both cases, one cobalt binds to three coordinated sites from the corresponding tridentate Schiff base ligand, and the fourth one was bonded by the acetate oxygen, and the fifth and the sixth donor sites come from the phenolate oxygen of another Schiff base ligand. Ramadan M. El-mehdawi, Abdussalam N. EL-dewik, Mufida M. Ben-Younes, Fathia A. Treish, Ramadan G. Abuhmaiera, Dejan Poleti, and Jelena Rogan Copyright © 2014 Ramadan M. El-mehdawi et al. All rights reserved. Molecular Structure and Crystal Packing of n-Type Semiconducting Material 3′,3′-(1,4-Phenylene)bis{2′-(4′′-trifluoromethyl)phenyl}acrylonitrile Tue, 19 Aug 2014 00:00:00 +0000 The exact molecular structure and the crystal packing of the n-type semiconducting material 3′,3′-(1,4-phenylene)bis{2′-(4′′-trifluoromethyl)phenyl}acrylonitrile was determined by a single crystal X-ray diffraction with twin treatment technique. The air-stable product was crystallized from dichloromethane-hexane mixed solution. The solid-state structure is the example of a typical π-π stacking with side intermolecular CN–H short contact networks. Tetsuji Moriguchi, Shuichi Nagamatsu, Tatsuo Okauchi, Akihiko Tsuge, Wataru Takashima, and Shuji Hayase Copyright © 2014 Tetsuji Moriguchi et al. All rights reserved. Synthesis and Molecular Structure of tert-Butyl 3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate Sun, 17 Aug 2014 12:18:32 +0000 The compound tert-butyl 3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate was synthesized as a cyclic amino acid ester from the corresponding ethyl 2-amino-4-(2-oxiranyl)butanoate HCl salt via an intramolecular lactonization reaction and was characterized by using 1H NMR spectroscopy and high-resolution mass spectrometry. The product was then recrystallized from dichloromethane/diethyl ether and its structure was determined via single crystal X-ray diffraction analysis. The crystal was found to be of the monoclinic space group P21/c (no. 14) with  Å,  Å,  Å, β = 114.186(13)°, and = 1.350 g/cm3 at 123 K. The compound has bicyclo[2.2.2]octane structure including a lactone moiety and a piperidine ring, and the two diastereomers of the molecules are present in a 1 : 1 ratio in the crystal. Tetsuji Moriguchi, Suvratha Krishnamurthy, Toru Arai, Taisuke Matsumoto, Koji Araki, Akihiko Tsuge, and Norikazu Nishino Copyright © 2014 Tetsuji Moriguchi et al. 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.