Crystal Structure of 4-(8-chloro-[1,2,4]triazolo[4,3-α]pyridin-3-yl)phenol

The title compound 4-(8-chloro-[1,2,4]triazolo[4,3-α]pyridin-3-yl)phenol was structurally characterized by X-ray crystal structural analysis. The crystals are triclinic, space group P-1 with a = 7.307(3), b = 11.792(4), c = 12.474(5) Å, α = 83.850(10), β = 87.148(13), γ = 77.691(11)°, V = 1043.6(6) ų, Z = 2, F(000) = 504, D_c = 1.564 g/cm³, μ = 0.350 mm^?1, the final R = 0.0433 and wR = 0.1232. A total of 10,746 reflections were collected, of which 4920 were independent (R_int = 0.0357). In the crystal packing diagram, intermolecular O-H…Cl and C-H…O hydrogen bonds stabilize the solid state of the title compound.     

Synthesis and crystal structure of a new inorganic – organic complex: (4‐ClC7H6NH3)9[Nd(P6O18)2]·9H2O

Single crystals of (4‐ClC₇H₆NH₃)₉[Nd(P₆O₁₈)₂]·9H₂O were synthesized in aqueous solution. This compound crystallizes in a triclinic P1 unit‐cell, with a = 14.898(6), b = 18.049(7), c = 20.695(6)Å, α = 102.04(3), β = 100.49(3), γ = 98.82(3)°, V = 5245(4) ų and Z = 2. The crystal structure has been solved and refined to R = 0.043 (Rw = 0.061) for 20420 observed reflections. The atomic arrangement of the title compound can be described as infinite layers built by complex of Neodyme [Nd(P₆O₁₈)₂] and nine water molecules. The organic cations are located in the space delimited by the successive inorganic layers. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)2

The crystal structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)₂ has been determined from three-dimensional X-ray diffraction data. The compound crystallizes in the triclinic space group P1 (no 2) with unit cell parameters α = 9.712(6) Å, β = 11.137(7) Å, c = 14.768(12) Å, α = 86.04(5), β = 80.36(4), γ = 65.70(4), Z = 2, V= 1435(2) ų. The structure was determined by direct methods which on refinement yielded a final value of R(F) index as 0.068.     

X-ray crystal structural analysis of 1,2-dihydro-3-methylpyrazole-5-one

The title compound 1,2-dihydro-3-methylpyrazole-5-one was determined by X-ray crystal structural analysis. The crystals are monoclinic, with space group P2(1)/n with a = 7.968(7), b = 6.502(6), c = 9.986(10) Å, α = 90°, β = 109.995(15)°, γ = 90°, V = 486.1(8) ų, Z = 4, F(000) = 208, D_c = 1.340 g cm^–3, μ = 0.100 mm^?1, and the final R = 0.0373 and wR = 0.0961. A total of 4776 reflections were collected, of which 1148 were independent (R_int = 0.0589). In the crystal packing diagram, intermolecular N?H···O hydrogen bonds and π?π stacking interactions stabilize the solid state of the title compound.     

Crystal structure of N,N ′-bis(cyclohexyl)-1-(N,N-dihexylamino)perylene-3,4:9,10-bis(dicarboximide)

An asymmetric dialkylamino-substituted perylene bisimide (1), N,N′-bis(cyclohexyl)-1-(N,N-dihexylamino)perylene-3,4:9,10-bis(dicarboximide), was synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P–1, with a = 9.8924(6), b = 14.6338(10), c = 15.6221(10) Å, α= 105.098(3)°, β = 103.386(2)°, γ = 107.772(3)°, and Z = 2. The central perylene core of 1 is twisted with dihedral angles of 14.9(3)° and 11.6(3)°; this twist configuration induces the axial chirality in this family of perylene bisimide dyes. In the crystal structure, the intermolecular C–H···O interaction links a pair of molecules into a cyclic centrosymmetric dimer that is connected to one another via the intermolecular π–π stacking, so linking the molecules into a continuous one-dimensional framework along the [100] direction.     

Crystal structure of the tetranickel complex with Ipropanethiolate

The title complex [Ni₄(SPrⁱ)₈] was confirmed by single crystal X-ray crystal diffraction analysis. The crystals are monoclinic, space group P2/n with a = 12.760(3), b = 10.059(2), c = 14.484(3) Å, α = 90, β = 93.70(3), γ = 90°, V = 1855.3(6) ų, Z = 4, F(000) = 880, D_c = 1.496 g/cm³, μ = 2.463 mm^?1, the final R = 0.0352 and wR = 0.0580. A total of 18,588 reflections were collected, of which 4404 were independent (R_int = 0.0631). In the crystal packing diagram, intermolecular C—H···Ni hydrogen bonds stabilize the solid state of the title complex.     

Crystal structure of low-symmetry rondorfite

The crystal structure of an aluminum-rich variety of the mineral rondorfite with the composition Ca₁₆[Mg₂(Si₇Al)(O₃₁OH)]Cl₄ from the skarns of the Verkhne-Chegemskoe plateau (the Kabardino-Balkarian Republic, the Northern Caucasus Region, Russia) was solved in the triclinic space group with the unit-cell parameters a = 15.100(2) Å, b = 15.110(2) Å, c = 15.092(2) Å, α = 90.06(1)°, β = 90.01(1)°, γ = 89.93(1)°, Z = 4, sp. gr. P1. The structural model consisting of 248 independent atoms was determined by the phase-correction method and refined to R = 3.8% with anisotropic displacement parameters based on all 7156 independent reflections with 7156 F > 3σ(F). The crystal structure is based on pentamers consisting of four Si tetrahedra linked by the central Mg tetrahedron. The structure can formally be refined in the cubic space group (a = 15.105 Å, sp. gr. Fd \(\overline 3 \), seven independent positions) with anisotropic displacement parameters to R = 2.74% based on 579 reflections with F > 3σ(F) without accounting for more than 1000 observed reflections, which are inconsistent with the cubic symmetry of the crystal structure.     

X-ray crystal structural analysis of dicyclohexylthiocarbamide

The title compound dicyclohexylthiocarbamide has been determined by single crystal X-ray crystal diffraction analysis. The crystals are monoclinic, space group P2(1)/c with a = 12.5908(9), b = 11.2158(9), c = 10.4255(8) Å, α = 90, β = 110.7360(10), γ = 90°, V = 1376.88(18) ų, Z = 4, F(000) = 528, D_c = 1.160 g/cm³, μ = 0.214 mm^?1, the final R = 0.0381 and wR = 0.1030. A total of 6836 reflections were collected, of which 2423 were independent (R_int = 0.0154). In the crystal packing diagram, intermolecular N?H···S hydrogen bonds stabilize the solid state of the title compound.     

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)     

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.     

Structural analysis of 1,1′-bis(diphenylphosphino)ferrocene dioxide

The title compound 1,1′-bis(diphenylphosphino)ferrocene dioxide has been analyzed by X-ray crystal diffraction analysis. The crystals are monoclinic, space group P2(1)/c with a = 22.461(5), b = 10.515(2), c = 12.024(2) Å, α = 90, β = 96.28(3), γ = 90°, V = 2822.7(10) ų, Z = 4, F(000) = 1256, D_c = 1.422 g/cm³, μ = 0.683 mm^?1, the final R = 0.0514 and wR = 0.1369. A total of 22218 reflections were collected, of which 4957 were independent (R_int = 0.0422). In the crystal packing diagram, intermolecular O?H···O hydrogen bonds between the P=O and H₂O stabilize the solid state of the title compound.     

Synthesis Characterization and Crystal Structure of 2-(3,4,5-trimethoxyphenyl)-1-(4-fluorophenyl)-4,5-diphenyl-1H-imidazole

The title compound, C₃₀H₂₅FN₂O₃, was prepared from the four-component one-pot condensation reaction and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-Visible, and single-crystal X-ray diffraction. The compound crystallizes in the triclinic crystal system with the space group Pī, with unit cell parameters a = 10.286(2) Å, b = 11.795(2) Å, c = 21.331(4) Å, α = 100.270(3)°, β = 90.093(3)°, γ = 90.062(3)°, and Z = 4. The crystal and molecular structure of the title molecule is stabilized by intra-molecular interactions of types C–H···N and C–H···O.     

Crystal Structure of Dimeric Cu(II) Complex {μ,μ'‐acetato O,O bis [N‐salicylidene‐2‐amino‐pyridine‐methanolato N,N,O]} : perchlorate

The crystal structure of the title complex has been solved using X‐ray diffraction data.The compound crystallizes from aqueous ethanol solvent in the triclinic system, space group P‐1, with unit cell parameters: a = 8.9532(1), b = 12.7423(3), c = 14.9012(3) Å, α = 73.767(1), β = 75.322(1), γ = 77.496(1)°, Z = 2, V = 1559.4(5) ų. The trial structure was determined by automated Patterson methods and subsequent difference Fourier techniques using DIRDIF98 and refined to a final R‐factor of 0.064. The copper ion Cu1 adopts a (4+1) square‐pyramidal geometry defined by the tridentate N‐salicylidimine dianions and the neutral monodentate pyridine ligand in the basal plane. The apical position is occupied by a solvent methanol molecule at a distance of 2.341(4) Å. The copper Cu2 adopts a square‐planar geometry.     

α-substitued phosphoryl compounds (IV). The crystal and molecular structure of diethyl[bis-(p-chlorophenoxy)-methan]-phosphonate,C17H19O5PCl2

Diethyl-[bis-(p-chlorophenoxy)-methan]-phosphonate crystallizes in the triclinic space group P 1 with two molecules per unit cell. The lattice parameters are a = 8.757 Å, b = 10.479 Å, c = 12.878 Å, α = 82.21°, β = 116.27°, γ = 113.80°. With X-ray diffraction data, collected on an automatic four circle diffractometer, the crystal structure was solved by direct methods and refined to an R-value of 0.049 for 3116 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl phosphonic acid esters. Correlations between the geometry of the structure and NMR-data are of interest.     

Crystal and Molecular Structure of 6‐Methyl‐2‐(trifluoromethyl)‐(6H)‐imidazo[1,2‐c]pyrimidin‐5‐one

The title compound (C8H6F3N3O) crystallizes as colorless plates, triclinic, a = 10.916(2) Å, b = 11.140(1) Å, c = 8.368(1) Å, α = 95.938(9)o, β = 105.24(1)o, γ = 64.843(9)o, V = 888.6(2) ų, Z = 4, D_calc = 1.623g/cm³, space group P . The structure was solved by direct methods and refined by the full‐matrix least‐squares method (R_w = 0.047).     

Synthesis,Crystal Structure and Characterization of (Z)-2-N′-hydroxyisonicotinamidine

The compound (Z)-2-N′-hydroxyisonicotinamidine, (2) was synthesized and characterized by ¹H NMR, FT-IR, FAB-Mass, UV-Visible Spectra, and elemental Analysis. Its molecular structure was solved by single crystal X-ray diffraction method. The title molecule, C₆H₇N₃O is crystallized in the orthorhombic crystal system with the space group Pna2₁ and with unit cell parameters a = 12.5664(8) Å, b = 8.8622(6) Å, c = 5.7953(4) Å, α = 90°, β = 90°, γ = 90°, and Z = 4. The molecular and crystal structure of the title molecule is stabilized by an intramolecular interaction of the type N—H···O, and the intermolecular interactions of types N—H···N and O—H···N.     

Structure Analysis of Methyl‐3,4‐dihydro‐3‐(p‐methylphenyl)‐4‐oxo‐2‐quinazolinyl thiopropionate

The crystal structure of methyl‐3, 4‐dihydro‐3‐(p‐methylphenyl)‐4‐oxo‐2‐quinazolinyl thiopropionate (C₁₉H₁₈N₂O₃S) has been determined by X‐ray diffraction methods. The compound crystallizes in the triclinic space group P with unit cell parameters: a = 9.094(2), b = 9.428(3), c = 10.612(3) Å, α = 94.55(3), β = 95.44(2), γ = 106.75(3)° and Z = 2. The structure has been refined to an R‐value of 0.054 for 2533 observed reflections [F_o > 4σ(F_o)]. The quinazoline moiety and the methyl substituted phenyl ring is almost planar. The dihedral angle between these two moieties is 84.96(8)° . The crystal structure is stabilized by an intermolecular C‐H … O interaction.     

Synthesis and supramolecular interactions involved in the crystal structure of (2,4,10,12-tetrabromo-6,7,14,15-tetrahydro-6, 14-thiacycloocta[1,2-b:5,6-b’]diquinoline)2·(1,1,2,2-tetrachloroethane) inclusion compound

The tetrahalo aryl inclusion host 2,4,10,12-tetrabromo-6,7,14,15-tetrahydro-6,14-thiacycloocta[1,2-b:5,6-b’]diquinoline 3 was re-synthesized to explore its ability to trap toxic polychlorinated hydrocarbons such as 1,1,2,2-tetrachloroethane (TCE) in the form of host–guest compound. Host 3 crystallizes from a fresh sample of TCE to form an inclusion compound of the formula (3)₂·(TCE) in triclinic system, space group P-1, with a = 7.7732(16) Å, b = 10.739(2) Å, c = 14.816(3) Å, α = 97.329(4)°, β = 98.619(4)°, γ = 103.359(4)°, V = 1172.7(4) ų, and Z = 2. The X-ray crystal structure of the (3)₂·(1,1,2,2-TCE) is described and analyzed in terms of crystal engineering and supramolecular chemistry. The hosts assemble by means of different types of packing motifs. The included TCE molecules are enclosed within host molecular pens. Novel halogen···halogen intermolecular interactions as well as other non-covalent intermolecular interactions involved in the crystal structure are presented and proved to play an important role in linking these host–host, host–guest, and guest–guest building blocks.     

Synthesis and Structure of 1,4-Diazabutadiene Liquid Crystals

Abstract

Nine 1,4-diazabutadiene compounds, Ar-N=C(R)-C(R)=N-Ar, R=H, Me; Ar=H_2n+1C_nO-C₆H₄, 2,4-(H₉C₄O)(Me)-C₆H₃ were synthesized and their liquid crystal properties were studied through thermal polarizing microscopy. The X-ray single crystal structure of compound 9 (Ar-N=C(H)-C(H)=N-Ar, Ar=2,4-(Me)(H₉C₄O)C₆H₃) was tested. It is a monoclinic crystal system, space group P2₁/C with the unit cell parameters: a=7.0703(3)Å, b=8.6741(4)Å, c=18.3115(8)Å, β =95.392(1)?. V=1114.57(9)ų, z=2, Dc=1.134 Mg/m³, R=0.0490, Rw=0.1237.     

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.