Crystal structure of 3-phenyl-7-bromoisoxazolo[4,5-d]pyridazin-4(5H)-one

The crystal and molecular structure of 3-phenyl-7-bromoisoxazolo[4,5-d]-pyridazin-4(5H-one, C₁₁H₆BrN₃O₂, has been determined from two- and three-dimensional X-ray data and refined by Fourier and least-squares methods toR = 0·101 for 1187 observed reflexions. Crystals of 3-phenyl-7-bromoisoxazolo-[4, 5-d]pyridazin-4(5H)-one are monoclinic:a = 7·67,b = 6·84,c = 20·52 Å, = 91·5 °,Z = 4, space groupP2₁/c. The benzene ring makes an angle of 4·5 ° with the plane of the isoxazole ring, and the other part of the molecule is slightly non-planar. The bond distances and angles compare well with those of other similar molecules. Two N-H...O hydrogen bonds join the two molecules related by a centre of symmetry. Close molecular packing is found in layers parallel to (100).     

Crystal and molecular structure of triphenyl[2-(p-tolylthio)ethyl]tin

The crystal and molecular structure of Ph₃SnCH₂CH₂SC₆H₄Me-p has been determined by X-ray crystallography. In each of the two independent molecules in the asymmetric unit the tin atom has an irregular tetrahedral geometry, with C–Sn–C valency angles ranging from 104.1(5) to 114.7(5)° in molecule (1) and from 104.6 to 112.7(6)° in molecule (2). The bond lengths, C_alkyl–Sn are 2.18(1) and 2.17(2)Å (in molecules (1) and (2), respectively) while the C_aryl–Sn bond lengths range from 2.11(1) to 2.13(1)Å in molecule (1) and from 2.09(1) to 2.14(1)Å in molecule (2). The Sn–C–C–S torsion angle, 172(1)° is the same for both molecules. NMR spectral data are presented; the¹H NMR spectrum in solution of the central-CH₂–CH₂-unit suggests that each of the protons on each of the CH₂ groups is magnetically distinct and that rotations about the C–C bond are slow on the NMR time scale. Comparisons with similar molecules are made and conformations discussed in terms of steric effects.     

Crystal and molecular structure of 3-tert-butyl-1-ethyl-1-[(4-chlorobenzene) sulfonyl] urea

The crystal structure of the title compound, C₁₃H₁₉SN₂O₃Cl, has been solved by direct methods with X-ray diffraction data collected using Cu K radiation. The crystals are monoclinic, witha=9.415(2),b=9.836(3),c=16.928(3)Å,=95.77(3)° and space groupP2₁/c. The structure was refined with 1806 observed [I>2(I)] unique reflections measured on Siemens AED single Crystal diffractometer equipped with a IBM PS2/30 personal computer, to a finalR value of 0.076. The molecule has similar geometrical and conformational features to those observed in 3-tert-butyl-1-methyl-1-[(4-chlorobenzene) sulfonyl] urea (Ghoshet al., 1992) and most of the sulfonamide structures.     

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 structure analyses of bis(triphenyl- phosphoranyliden)ammonium bis(pentafluoroethyl) argentate, [Ph3P=N=PPh3][Ag(C2F5)2] and bis[bis(triphenylphosphoranyliden)ammonium] tetrachloro-diargentate, [Ph3P=N=PPh3]2[ClAg(μ-Cl)2AgCl]

Bis(triphenylphosphoranyliden)ammonium bis(pentafluoroethyl)argentate, [Ph₃P=N= PPh₃][Ag(C₂F₅)₂] (1) and bis[bis(triphenylphosphoranyliden)ammonium]tetrachloro-diargentate, [Ph₃P=N=PPh₃]₂[ClAg(μ-Cl)₂AgCl] (2) were crystallized from the reaction mixture of pentafluoroethylsilver(I) and bis(triphenylphosphoranyliden)ammonium chlo-ride. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a = 17.083(2) Å, b = 11.600(2) Å, c = 19.833(2) Å, β = 109.66(1)°, V = 3700.8(7) ų, Z = 4. 2 crystallizes in the centrosymmetric orthorhombic space group Pbca (No. 61) with a = 19.540(1) Å, b = 15.926(1) Å, c = 20.160(1) Å, V = 6273.6(3) ų, Z = 8.     

Crystal and molecular structure of [Cu(pyrimidine)4]2BF4

The crystal structure of [Cu(pyrimidine)₄]2BF₄ was determined using single crystal X-ray diffraction. The compound crystallizes in the monoclinic space groupP2₁/n, with lattice parametersa=9.9736(8),b=13.872(1),c=16.568(1) Å. β=98.002(1), andZ=8, yielding a calculated density of 1.857 g/cm³. The Jahn-Teller distorted copper coordination sphere is composed of the four pyrimidine ligands in the equatorial positions (ave. Cu?N=2.02 Å) and the longer axial bonds from the copper to one fluorine (ave Cu?F=2.39 Å) on each of the BF ₄ ^? anions. The crystal structure features layers of molecules having interleaved pyrimidine rings: the layers are connected through intermolecular H … F hydrogen bonds.     

Crystal structure of 1-methyl-3-([2,2-dimethyl-4,6-dioxo-1,3-dioxane-5-ylidene]methyl)urea

The crystal structure of 1-Methyl-3-([2,2-dimethyl-4,6-dioxo-1,3-dioxane-5-ylidene]methyl)urea (C₉H₁₂N₂O₅) has been determined by single crystal X-ray diffraction analysis. The crystals are monoclinic, a = 5.3179(2), b = 18.6394(6), c =10.8124(3) Å, β = 100.015(2)°, Z = 4, sp. gr. P2₁/c, R = 0.0381 for 2537 reflections with I > 2σ(I). Except for C(CH₃)₂ group, the molecule is planar. The structure is stabilized by inter- and intramolecular N-H...O hydrogen bonds and weak C-H...O interactions.     

Crystal structure of (NH4)5Sc3F14

The equilibrium in the (NH₄)₃ScF₆-NH₄HF₂-H₂O system in the range of hydrodifluoride ammonium solution concentrations of 0.05–3.5 mol/L at temperatures of 18 and 90°C is studied. The composition of solid phases in equilibrium is analyzed using elemental analysis, X-ray diffraction, and neutron diffraction. A new phase, (NH₄)₅Sc₃F₁₄ with a tetragonal lattice (sp. gr. I4₁/a, unit-cell parameters a = 0.80843 nm and c = 2.5177 nm), is found at fluoride ion concentrations in the solution of ≤1.06 mol/L at 18°C and 2.92–3.01 mol/L at 90°C; the crystal structure of this phase is determined.     

Crystal structure of 4-[benzylideneamino]-3-thiophen-2-yl-methyl-4,5-dihydro-1H-[1,2,4]triazole-5-one

The crystal structure of the title compound C₁₄H₁₂N₄OS was determined by the X-ray diffraction method. The compound crystallizes in the triclinic space group $P\bar 1$ with Z = 2. The molecule is not planar: the dihedral angle between the triazole and thiophene rings is 73.98(2)°, and that between the triazole and benzene rings is 4.05(2)°. The thiophene ring is disordered over two positions, which are approximately parallel and oppositely oriented. The major component refined to a site-occupancy factor of 0.573(3). An intramolecular C-H...O hydrogen bond generates an S(6) ring motif. In the crystal, molecules are linked together by two pairs of N-H...O interactions (to the same O atom as acceptor), forming inversion dimers. The crystal packing is also stabilized by π-π interactions [centroid-centroid distance is 3.978 Å].     

Structure of ethyl(3-amino-5-nitrobenzo[b]thiophen)-2-carboxylate

The title compound was obtained as main product by the reaction of 3-chloro-5-nitro-1,2-benzisothiazole with diethyl malonate in sodium ethoxide. It crystallizes in the monoclinic space groupP2₁/n witha=12.143(5),b=11.172(4),c=8.567(3) Å,=95.51(2)°,Z=4. The structure was solved by direct methods and refined by full-matrix least-squares to a finalR value of 0.035 for 1217 reflections. The entire molecule is substantially planar except for the terminal methyl group. The amino group is involved in intra- and intermolecular hydrogen bonding.     

Molecular structure of (±)-5-benzylamino-endo-tricylo[5.2.1.02,6]dec-4-en-3-one

The crystal and molecular structure of (±)-5-benzylamino-endo-tricyclo[5.2.1.0^2.6]dec-4-en-3-one is described. The X-ray analysis revealed that the reduction of the norbornene double bond is an important process in the irradiation of the used enaminones. The structure was solved by direct methods and refined by least squares methods toR ₁=0.0468 for 2070 reflections (withI>2σ(I). Crystal data: C₁₇H₁₉NO, Orthorhombic, space groupPbcn, a=40.695 (1),b=6.6928 (1),c=10.2378(4)Å,V=2788.44(14)ų,Z=8.     

Crystal structure of the molecular adduct of 5-mono[(4-nitrophenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene with chloroform (1:1)

The crystal structure of the molecular adduct of 5-mono[(4-nitrophenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene (2) with chloroform (C₃₄H₂₇N₃O₆ CHCl₃) was determined by X-ray crystallographic analysis. It was found to possess a monoclinic space group P2(1)/n, with a = 15.9306(13) Å, b = 10.6293(9) Å, c = 20.3194(17) Å, = 110.480(2)° and D_calc = 1.428 Mg/m³ for _Z = 4. Crystal data indicated that the calix[4]arene moiety of 2 exists in a distorted-cone conformation with intramolecular hydrogen bonds.     

Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).     

Crystal structure of [Co(o-SC6H4NH2){P(OMe)3}3]PF6

A cobalt-thiolato-phosphite complex [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]PF₆ has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group with a = 10.590(4), b = 11.122(3), c = 13.577(5) Å, = 101.85(1), = 108.50(1), = 101.75(1)°, V = 1420.6(8) ų, and Z = 2. The structure comprises discrete [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]⁺ cations and PF ₆ ^– anions where the metal atom is coordinated in a highly distorted square-pyramidal environment by one chelate o-SC₆H₄NH ₂ ^– (abt) and two P(OMe)₃ ligands in the basal positions, and a third P(OMe)₃ in the axial site with Co–N,, 1.847(5), Co–S, 2.166(2), Co–P, 2.157(2), 2.147(2), and 2.125(2) Å.     

Crystal structure and phase transition in the compound [C6H5CH2NH(CH3)2]TlCl4

The N‐N dimethyl benzylammonium tetrachlorothallate (III) [C₆H₅CH₂NH(CH₃)₂]TlCl₄ crystallizes in the monoclinic system P2₁/n at room temperature with the following unit cell dimensions: a = 7.725(3) Å, b = 14.080(5) Å, c = 13.697(4) Å, β = 91.2(2)° with Z = 4. The structure shows a layer arrangement perpendicular to the b axis: planes of [TlCl₄]^‐ tetrahedra alternate with planes of [C₆H₅CH₂NH(CH₃)₂]⁺ cations. The cohesion of the atomic arrangement is ensured by hydrogen bonds N‐H…Cl. Differential scanning calorimetric and optical birefringence measurements reveals a phase transition at T = 339K. Raman spectroscopic study and dielectric measurements were performed to discuss the mechanism of the phase transition. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate

The crystal structure of the potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate has been determined. Potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate crystallizes in the orthorhombic space group Pca2₁ with the parameters a=30.7323(5) ?, b=8.3083(1) ? and c=9.2173(2) ?, V=2353.48(7) ?³ with Z=4. The crystal structure reveals the formation of continuous chains where two bidentate arms of the hydroborate ligand are coordinated to one potassium and the third to another cation. The structures of numerous transition metal and actinide salts have been reported during the last decades but no alkali metal complexes were available.