Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

Crystal and Molekular Structure of Piperidinium-acet-p-Cl-anilide-chloride

Piperidinium-acet-p-Cl-anilide-chloride crystallizes in the triclinic space group P 1 with 2 formula units C₁₃H₁₈ON₂Cl₂ in the unit cell. The lattice constants are a = 10.471 Å, b = 12.545 Å, c = 6.149 Å, α = 72.14°, β = 105.70° and γ = 105.21°. Bond lengths, bond angles and the conformational flexibility were determined by X-ray structure analysis. The crystal structure contains dimeres consisting of drug molecules connected by hydrogen bonds.     

Crystal and Molecular Structure of Non-hydrated and Hydrated Piperidinium-acet-o-Cl-anilide-chloride

Crystallizations from water and alcoholic solution respectively yield different crystal and molecular structures of Piperidinium-acet-o-Cl-anilide-chloride. The non-hydrated compound crystallizes from alcoholic solution in the space group P 2₁/c with 4 formula units C₁₃H₁₈N₂OCl₂ in the unit cell of dimensions a = 12.352 Å, b = 6.864 Å, c = 19.018 Å and β = 113.98°. The hydrated modification has the space group C 2/c with 8 formula units C₁₃H₁₈N₂OCl₂ and 8 H₂O molecules in the unit cell. The lattice constants are a = = 24.159 Å, b = 8.966 Å, c = 14.179 Å and β = 90.50°. The X-ray structure analyses were carried out to investigate the hydrogen bonds and the change of the molecular conformation caused by linking of water molecules to the drug molecules.     

The Crystal and Molecular Structure of the Complex Diaquatetrakis(imidazole)copper(II) Terephthalate Crystal Structure Containing Cu(II) Him and TA

The title compound has been synthesized and its crystals structure determined at room temperature. MW = 536.01, monoclinic, space group C2/c, Z = 4, a = 22.193(5) Å, b = 8.038(2) Å, c = 15.699(4) Å, β = 119.64(2)°. The crystal structure consists of repeated [Cu(Him)₄(H₂O)₂] (Him = imidazole) cations and non-coordinated terephthalato dianions. The copper(II) ion displays an elongated octahedral coordination being linked to the four nitrogen atoms of the four imidazole ligands and to the two oxygen atoms of the two water molecules. The terephthalato dianions are hydrogen bonded to the four water molecules and four imidazole groups.     

The Crystal and Molecular Structure of 4'-Cyanophenyl-4-n-Pentylbenzoate

The crystal and molecular structure of the title compound with the formula C₅H¹¹—C₆H₄—COO—C₆H₄—CN (CPPB) has been determined by X-ray diffraction methods. CPPB crystallizes in the monoclinic space group P2₁/n with eight molecules in a unit cell of dimensions a = 15.268(2) Å, b = 9.165(1) Å, c = 24.031(3) Å, β = 94.67(1)°. The structure has been solved by direct methods and refined to an R value of 0.070.

The CPPB molecules adopt a stretched form and are packed in an approximate parallel imbricated mode, the molecular long axes making an angle of about 5° with the crystal c axis. The molecular geometry and packing are discussed in relation to the mesomorphic behavior of CPPB.     

The Crystal and Molecular Structure of Mesogenic Malonates (II)

The crystal and molecular structures of three diethyl-2-{n-[4-(4-nitrophenylazo)-phenoxy]alkyl}malonate with n = 5 (5 PhNO₂), 7 (7PhNO₂), 9 (9 PhNO₂) and an analogous diethyl-2-[4(4-cyanophenylazo)phenoxy]pentylmalonate (5 PhCN) have been determined with CuK_a or MoK_a: 5 PhNO₂: a = 8.007(6) Å, b = 11.960(8) Å, c = 13.516(9) Å, α = 77.10(6)°, β = 81.80(5)°, γ = 83.15(5)°; R = 0.053; 7PhNO₂: a = 8.074(4) Å, b = 11.592(5) Å, c = 14.422(7) Å, α = 87.43(3)°, β = 82.46(3)°, γ = 85.43(3)°; R = 0.072; 9 PhNO₂: a = 5.520(5) Å, b = 13.628(9) Å, c = 20.220(11) Å, α = 100.02(4)°, β = 95.49(4)°, γ = 101.02(4)°; R = 0.042; 5 PhCN: a = 8.018(6) Å, b = 11.960(8) Å, c = 13.566(7) Å, α = 77.82(5)°, β = 81.89(5)°, γ = 82.69(5)°; R = 0.067 (isotropically refined). All these structures belong to the triclinic space groups P1 . The arrangements of the molecules in the crystal of the homologous series of nPhNO₂ suggest two different types of packing independent of n even, odd or large, small. 5 PhCN represents an isomorphous structure to 5 PhNO₂. Isomophism between 7 PhNO₂ and 7 PhCN was confirmed by cocrystallization of these two compounds whose crystal structure was also determined.     

The Crystal and Molecular Structure of the Smectogenic Compound 5-Hexyl-2-(4-bromophenyl)-1,3-dioxane

The title compound with the formula C₆H₁₃ C₄O₂H₆ C₆H ₄Br (HBPD) crystallizes in the monoclinic space group C 2/c with lattice parameters a = 28.48 Å, b = 5.71 Å, c = 20.19 Å, β = 97.4° and molecules per unit cell. The structure has been solved by the heavy atom method and refined to a final R value of 0.094. – The HBPD molecules adopt a fully stretched form, both the alkyl and phenyl substituent are in equatorial position with respect to the chair-shaped dioxane ring. The orientation of the phenyl group is an intermediate between the perpendicular and parallel conformation. The molecules show a nearly perfect parallel arrangement in the crystal lattice.     

A Novel Coordination Structure of Dichromates Bonding to Copper (II): [Cu(bipy)2(Cr2O7)] · 2 H2O

Dark-green multimetal compound crystal [Cu(bipy)₂(Cr₂O₇)]· 2 H₂O was obtained from aqueous solution of Cu(NO₃)₂, K₂Cr₂O₇ and bipyridine. The crystal structure was determined by X-ray crystallography: triclinic P1 , a = 7.716(3) Å, b = 9.656(3) Å, c = 15.517(5)Å, α = 77.41(3)°, β = 81.04(3)°, γ = 82.33(3)°, Z = 2. In this compound, two chromium atoms and a copper atom are linked by two oxo bridges (Cu(II) O Cr(VI) O Cr(VI)). The copper coordination polyhedron corresponds to a five-coordinated distorted trigonal bipyramid.     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Structure Study of the Complex [Cu2 (μ–C2O4) (C10H8N2)2(H2O)2] (C6H4COSO2N)2 Crystal Structure Containing Cu (II) Bipy Oxalato and Saccharin

The title compound has been synthesized and its crystal structure determined at room temperature. MW = 927.86, monoclinic, space group P2₁/c, Z = 2, a = 9.283(1) Å, b = 16.239(2) Å, c = 12.209(1) Å, β = 99.848(9)°. The crystal structure consists of repeated [Cu₂(μ–C₂O₄)(C₁₀H₈N₂)₂ · (H₂O)₂]₂ cations and non-coordinated saccharin anions. Each copper ion is in a square pyrimidal environment with two oxalate oxygen and two bipyridine nitrogen atoms as a base and one water molecule at the apex. The two copper ions are bridged by oxalato and the distance is 5.138 Å.     

The Crystal and Molecular Structure of 4-Hydroxy-4′-nitro- biphenyl and its Potassium Salt

The crystal and molecular structures of the title compounds have been solved by single crystal X-ray analysis. 4-Hydroxy-4′-nitro-biphenyl (NBO) crystallizes in the centrosymmetric, monoclinic space group P2₁/n with a = 6.036(4) Å, b = 12.392(3) Å, c = 13.346(8) Å, β = 96.46(3)° and 4 molecules in the unit cell. Its potassium salt (NBOK) similarly belongs to P2₁/a with a = 11.277(2) Å, b = 7.3606(6) Å, c = 14.383(3) Å, β = 107.804(7)° and also 4 molecules in the unit cell. The structure of NBO was refined by full matrix least-squares calculation to R = 0.043 for 1105 observed reflections, the structure of NBOK to R = 0.041 for 2288 observed reflections, respectively. NBO and NBOK crystallize in layer-like structures. The biphenyl molecules of NBO are arranged as corrugated ribbons in layers. The ionic and polar moiety of NBOK (potassium, oxygen, and crystal water) are separated by biphenyl units to form layers. The almost planar biphenyl units of NBOK are arranged in pairs and exhibit a short molecular distance of 3.08 Å within one pair.     

Structural Properties of S-alkylated Dithiolene Chelates (I). Crystal and Molecular Structures of Bis(S-ethyl-ethene-1,2- dithiolato)palladium (II) and Bis(S-ethyl-ethene-1,2-dithiolato) platinum (II)

Bis(S-ethyl-ethene-1,2-dithiolato)palladium(II), Pd(S₂C₄H₇)₂, is monoclinic, P 2₁/n, with a = 7.598(1) Å, b = 10.445(2) Å, c = 8.031(1) Å, β = 95.3(1)° and Z = 2. The structure was determined by 893 independent reflections and refined by the block-diagonal leastsquares method to R = 0.12. The chelate molecule is nearly planar and the palladiumsulfur distances are 2.278(6) Å and 2.403(6) Å. Bis(S-ethyl-ethene-1,2-dithiolato)platinum(II), Pt(S₂C₄H₇)₂, is monoclinic, P 2₁/a, with a 13.114(2) Å, b = 12.873(2) Å, c = 7.446(2) Å, β = 96.1(1)° and Z = 4. The structure was solved from 2040 independent reflections. The compound is not isomorphic with the isomeric palladium complex. In the unit cell there exist two symmetry independent molecules. The platinum-sulfur distance is 2.280 (6) Å.     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Crystal and Molecular Structure of 1-Ethyl-3-[tris(trimethylsiloxanyl)silyl]pyrrolinium Hydrochloride

The crystal and molecular structure of 1-Ethyl-3[tris(trimethylsiloxyl)silyl]pyrrolinium hydro-chloride (C₁₅H₃₈N⁺O₃Si₄ · C¹⁻) has been determined by direct methods. The title compound crystallizes in the monoclinic space group C2/c with a = 20.640(3), b = 19.494(2), c = 27.34(3) Å, β = 90.60(4)°, V = 11000(13) ų, Z = 16, D_x = 1.034 Mg m⁻³. There are two molecules with different conformations in the crystal. The pyrroline rings are non-planar.-The Si O Si angles range from 149(1)° to 163(1)°. Two of the SiMe₃ groups are disordered. All molecules are connected by C¹⁻ – N⁺ contacts and C¹⁻ - HN⁺ hydrogen bonds to form double chains.     

Powder study of propanthioamide dervative C8H6N2S2

The crystal structure of 2‐cyano‐3‐(2‐thienyl)prop‐2‐enethioamide (C₈H₆N₂S₂), a propanethioamide derivative was solved from high resolution laboratory X‐ray powder diffraction data collected at ambient conditions. Structure determination was performed by means of the global optimization method of simulated annealing at a resolution of 1.5 Å. Rietveld refinement yielded an R_WP value of 4.02% (P2₁/a, a = 15.8174(2) Å, b = 5.6502(1) Å, c = 11.0952(1) Å, β = 116.9923(7)°, V = 883.6(5) ų, Z = 4). The molecules are stacked in parallel layers and are stabilized by hydrogen bonds. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Two organic‐inorganic hybrids with Keggin polyanions

Two new Keggin polyoxometalates [Co(phen)₃]₂[SiW₁₂O₄₀]·6H₂O (1) and (ppy)₆ H₄SiMo₁₂O₄₀·0.4H₂O (2) (phen = 1,10′‐phenanthroline, ppy = 4‐(5‐phenylpyridin‐2‐yl)pyridine) have been synthesized by the hydrothermal method. Single crystal X‐ray analysis revealed that compound 1 crystallizes in the monoclinic crystal system with cell parameters of a = 13.344(2) Å, b = 17.191(3) Å, c = 22.002(4) Å, α = 90.00°, β = 99.566(2)°, γ = 90.00°, V = 4977 ų, Z = 2, and compound 2 crystallizes in the triclinic crystal system with cell parameters of a = 11.297(2) Å, b = 12.341(3) Å, c = 19.354(4) Å, α = 107.60(3)°, β = 95.80(3)°, γ = 94.16(3)°, V = 2543.7(9) ų, Z = 1. Both 1 and 2 represent organic ligand molecules and inorganic Keggin anions, which are further interconnected to a 3D framework by supramolecular interactions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of piperidinium-acet-p-Cl-anilide-bromide

The crystal structure of piperidinium-acet-p-Cl-anilide-bromide is monoclinic, space group P 2₁/n with 8 formula units C₁₃H₁₈N₂OBrCl in the unit cell. The lattice constants are a = 7.337(2), b = 17.865(4), c = 22.822(5) Å, and β = 94.66(1)°. The title compound is not isomorphous to the corresponding chloride. Br ions are linked to the molecules by hydrogen bonds forming chains in the crystal structure.     

Structure of a liquid crystal of 4-cyano-4′-n-octyloxybiphenyl

The structure of a liquid crystal of 4-cyano-4′-n-octyloxybiphenyl (C₂₁H₂₅NO) is determined by X-ray diffraction analysis. The compound crystallizes in the triclinic crystal system with unit cell parameters a = 7.322(1) Å, b = 12.693(3) Å, c = 20.393(2) Å, α = 92.45(1)°, β = 99.96(1)°, γ = 99.35(2)°, and space group $P\bar 1$ . The structure is solved by the direct method and refined to R = 0.057. Two independent molecules are located in the asymmetric unit. No short intermolecular contacts are observed in the crystal packing.     

α-substituted Phosphoryl Compounds (I). The Crystal and Molecular Structure of Diethyl[5,6-dichloro-1,3-benzodioxol-(2)]-phosphonate,C11H13O5PCl2

Diethyl[5,6-dichloro- 1,3-benzodioxol-(2)]-phosphonate crystallizes in the triclinic space group P l̄ with two molecules per unit cell. The lattice parameters are a = 11.716 Å, b = 8.471 Å, c = 7.644 Å; α = 82.47° β = 95.81°, γ = 95.89°. With X-ray diffraction data collected on an automatic four circle diffractometer, the crystal structure was solved by direct methods and refined by least squares methods to an R value of 0.12 for 2374 measured reflections. The crystal used was im perfect. The substance is a derivative of acetales of formyl phosphoneacid esters. The aim is to find a correlation between the geometry of the structure and NMR data.     

The Molecular and Crystal Structure of 3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin

3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin crystallizes in the monoclinic space group P 2₁ with two molecules C₃₂H₄₈O₈ per unit cell and the lattice constants a = 7.865, b = 6.470, c = 29.803 Å, β = 93.95°. The structure was solved by direct methods of phases determination and subsequently refined by least squares technique to the final R-value 0.06. The position of the lactone ring is disordered in the crystal.