Crystal structure and electrochemical property of one‐dimensional complex: [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]2[Cu(mnt)2]

One metalorganic complex [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]₂[Cu(mnt)₂] (mnt = maleonitriledithiolate) has been obtained by the reaction of dicyclohexyl‐18‐crown‐6 with K₂mnt and CuCl₂·2H₂O. The title complex has been characterized by elementary analysis, FT‐IR, UV‐Vis spectroscopy and x‐ray single crystal diffraction. The title complex crystallizes in the triclinic space group P1 with crystallographic data: a = 10.870(6) Å, b = 11.536(6) Å, c = 12.904(7) Å, α = 101.541(10)°, β = 110.573(9)°, γ = 99.441(9)°, V = 1435.2(13) ų, Z = 1, D_calcd = 1.350 g/cm³, F(000) = 615, R₁ = 0.0641, wR₂ = 0.1475. It displays one‐dimensional chain‐like structure formed by [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]⁺ complex cations and [Cu(mnt)₂]^2‐ complex anions through N‐K‐N interactions. Its electrochemical behavior has also been studied by the cyclic voltammetry. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural studies of crystalline oligosaccharides VI: Crystal structure and conformation of benzyl‐4,6‐O‐benzylidene‐3‐O‐benzoyl‐β‐D‐galactoside

Monsaccharides are the building blocks of polysaccharides and hence are the simplest sugar molecules to study the conformation and molecular structures of sugars. Benzyl‐4,6‐O‐benzylidene‐3‐O‐benzoyl‐β‐D‐galactoside is a key intermediate in the synthesis of polysaccharides. Crystal structural investigation of the title compound was undertaken to establish their chemical structure as well as to study their solid state conformation. Crystals of the title compound, obtained from water/methanol, are orthorhombic, space group P2₁2₁2₁, with cell dimensions a=11.290 (4), b=9.941 (1), c= 21.442(2)Å, V= 2406ų, Z=4, D_obs= 1.42 gm/cm³, D_calc=1.423 g/cm³, 2886 reflections were collected on a CAD‐4 diffractometer. The structure was solved by direct methods and refined to a final reliability index of 4.7%. The galactoside sugar has the chair conformation with C2' and C5' deviating from the mean plane of the other atoms of the sugar. The 4,6‐O‐benzylidene ring also has a chair conformation with the benzoyl group proximal to O6'. The crystal structure is stabilized by O‐H…O hydrogen bonds involving O2' as donor and three C‐H…O hydrogen bond interactions. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallographic Investigations of 3β‐acetoxy‐5α‐cholestan‐6‐one‐semicarbazone ‐ A Steroid

The crystal structure of 3b‐acetoxy‐5a‐cholestan‐6‐one‐semicarbazone (C₃₀H₅₁O₃N₃) has been determined by X‐ray diffraction methods. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters a = 11.641(1), b = 16.552(1) c = 31.181(4) Å and Z = 8. The structure has been refined to an R‐value of 0.050 for 4407 observed reflections. Two molecules in the asymmetric unit have been observed. In both the crystallographically independent molecules, all the three six‐membered rings (A, B and C ) of steroid nucleus exist in chair conformation, while the five‐ membered ring D exists in 13β distorted‐envelope in molecule‐I and 13β, 14α half‐chair conformation in molecule‐II. Three intermolecular N‐H … O hydrogen bonds have been observed.     

Crystal Structure of Diethyl 2‐[2,2,2‐ trifluoro‐1‐(indole‐3‐yl)‐ethyl]‐2‐acetamidomalonate

The title compound (C₁₉H₂₁F₃N₂O₅) has been determined from three dimensional X‐ray diffraction data. The crystals are monoclinic, a = 7.626(4)Å, b = 17.515(4)Å, c = 15.066(3)Å, β = 101.02(3)°, V = 1975(1)ų, Z = 4, D_calc = 1.393g cm^‐3, space group P2₁/c. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.039).     

The Crystal and Molecular Structure of (μ‐terephthlato) bis [(N‐Salicylidene ‐N'‐(2‐hydroxyethyl) ethylenediamine) Copper(II)]

The title compound [[Cu(shen)]₂(tp)], {[Cu(C₁₅H₁₇O₄N₂)]2}, where tp = dianion of terephthalic acid and shen = (N‐salicylidene‐N'‐(2‐hydroxyethyl ethylene‐diamine)) has been prepared and its crystal structure determined by single crystal X‐ray diffraction at room temperature. The complex crystallizes in the orthorhombic space group Pbca with four formula units in a unit cell of dimensions a = 12.298(2), b = 14.214(2) and c = 16.436(2)Å. The structure consists of binuclear units with Cu(II) ion bridged by the tp ligand in a bis‐unidentate fashion. The five coordinate Cu(II) complex adopts a distorted square‐based pyramid. A crystallographic inversion center has been located at the center of the benzene ring of the tp bridging ligand. The Cu … Cu distance inside a same binuclear entity is 11.069Å. Intermolecular aromatic ring stacking interactions were observed with the shortest atom to atom contact being 3.423Å.     

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.     

3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one: A Steroid

The crystal and molecular structure of 3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one has been determined by X‐ray crystallographic techniques. The compound crystallizes in the space group P2₁ with cell parameters : a = 13.060(3), b=6.299(2), c=17.152(6)Å; β =96.47(3)o, V = 1402.02ų, Z = 2, R = 0.072 for 1921 observed reflections. The six‐membered rings (A, B and C) exist in the chair conformations while the five‐membered ring‐d assumes half‐chair. All rings of the steroid skeleton are trans connected.     

Crystal structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea

The crystal structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea (C₁₈H₂₆N₄S₂) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the orthorhombic space group Pbca, with unit cell parameters: a = 15.692(3), b = 20.803(8), c = 11.979(6)Å, Z = 8, V = 3911(7)ų. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.084 for 1447 observed reflections [I > 2σ ( I ) ]. In the thiosemicarbazide moiety, the S = C bond length is 1.656(6), N‐C‐N angle is 115.6(5)°. The crystal structure is stabilized by the intermolecular N‐H...S hydrogen bonds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole

The crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole (C₁₇H₂₂N₂S₁) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the triclinic space group P‐1 with Z = 6. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.052 for 2298 observed reflections [I > 2σ ( I ) ]. There are three crystallographically independent molecules, I, II and III. These molecules are held together by intermolecular N‐H...N hydrogen bonds. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Synthesis and crystallographic characterization of a chiral complex of (R)‐2‐(pyridin‐2‐ylmethylene)amino‐2′‐hydroxy‐1,1′‐binaphthyl(L) with hydrated nickel(II) acetate

A chiral complex of (R)‐2‐((pyridin‐2‐ylmethylene)amino)‐2′‐hydroxy‐1,1′‐binaphthyl ( L ) with hydrated nickel (II) acetate has been synthesized and spectroscopically characterized. The crystal structure of [NiL₂(CH₃OH)(CH₃COO)]CH₃COO·CH₃OH has been determined by single‐crystal X‐ray diffraction. The complex crystallizes in the orthorhombic space group P 2(1) 2(1) 2(1) with cell constants a = 15.1035 (19), b = 17.836 (2), c = 18.730 (2)Å, α = β = γ = 90.00°, Z = 4. The structure was solved by direct methods and refined to R = 0.0346 (wR₂ = 0.0863). The analytical result of the crystal structure indicates that a pair of L ligands chelate to a Ni (II) atom in an asymmetric fashion with one Ni‐N bond being longer than the other, the Ni (II) atom is further coordinated by one methanol molecule and one acetate anion to form a distorted octahedral geometry. In the crystal of the complex, the coordination cation [NiL₂(CH₃OH)(CH₃COO)]⁺, the uncoordinated methanol molecule and uncoordinated acetate anion are further assembled into one‐dimensional chain structure via intermolecular hydrogen bonds along the a‐axis. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of N‐(3,4‐dichlorophenyl)‐N′‐hydroxy‐2‐oxo‐2‐phenylacetamidine

The title compound (C₁₄H₁₀N₂O₂Cl₂) crystallizes in the monoclinic space group P2₁/a with a=10.042(1) Å, b=10.317(1) Å, c=13.877(2) Å, β=97.36(2)°, V=1425.8(3) ų, Z=4, D_x=1.44 g.cm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.0457). The title molecule consists of 3,4‐dichlorophenylamino and 2‐phenyl‐1,2‐ethanedione‐1‐oxime groups. The intermolecular O‐H…N and N‐H…O hydrogen bonds [O…N 2.760(6) and 3.087(5) Å] are highly effective in forming the polymeric chains. The oxime group has an E configuration. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Structure Analysis of 3'5' (dichloro phenyl)‐3‐ethyl‐5‐phenyl thio indalo [1,2‐e] imidazolidine

The title compound crystallizes in monoclinic system with space group P2₁ /n. The cell parameters are a = 12.3824(3) Å, b = 8.9255(1) Å, c = 19.9188(4) Å, V = 2181.75(7) ų , α = γ = 90.0° and β = 97.663(1)°. The structure has an indole moiety and an imidazolidine ring connected together. The phenyl sulfonyl group is attached to the indole moiety and the dichlorophenyl ring to the imidazolidine ring. The structure has a C‐H … Cl intra molecular hydrogen bond and C‐H … π type intermolecular interactions.     

Crystal and Molecular Structure of bis[diaaqua(1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine ‐2,5‐dione))N ickel(II)]dihydrate

The title compound [Ni(CPDD)(H₂O)₂]₂(H ₂O )₂, {]Ni₂(C₄₄H₂₈N₈O₁₂)] (H₂O)₂ }, where CPDD = 1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine‐2,5‐dione) has been prepared and its crystal structure determined by single crystal X‐ray diffraction at room temperature. The complex crystallizes in the triclinic space group P1 w ith two molecules in the asymmetric unit. The cell dimensions are a=10.452(1),b=14.098(1) & c=16.023 Å; D=110.13(1), E=100.63(1) & J=100.85(1)°. The two independent molecules in the asymmertic unit are related by pseudo two fold symmetry. In both the molecules the coordination environment around the Ni(II) may be best described as a distorted octahedral. Due to some delocalization of charge towards one of the oxygens(O1a) from the O2a atom some degree of bond localization has been observed. The individual diones of both the molecules are almost right angles at the metal atom. A long the y‐axis inversion related molecules are forming pseudo‐dimers through hydrogen bonding.     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallographic Analysis of Acetyl β ‐boswellic acid

The crystal structure of the title compound (3 α ‐acetoxy‐urs‐12‐en‐24‐oic acid, C₃₂H₅₀O₄) has been determined by X‐ray crystallographic techniques. The compound crystallizes into orthorhombic space group P2₁2₁2₁ with unit cell parameters : a = 12.773(2), b=16.381(4), c=27.929(7)Å. The structure has been solved by direct methods and refined to R = 0.054 for 4930 observed reflections. The structure contains two crystallographically independent molecules in the asymmetric unit which are almost identical in geometry. Rings A, B, D and E have chair conformations while ring C assumes a sofa conformation in both the molecules. The molecules in the structure are linked together by intra‐ and intermolecular O‐H…= and C‐H…O hydrogen bonds.     

Crystal and molecular structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione

The crystal structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione (C₂₂H₂₀N₂OS) has been determined from three dimensional single crystal X‐ray diffraction data. The title compound crystallizes in the monoclinic space group P 2₁/c, with a = 10.6674(13), b = 10.1077(7), c = 17.9467(19) Å, β = 98.460(9)°, V = 1914.0(3) ų, D_calc = 1.251 g cm^–3, Z = 4. In the title compound, the allyl group shows positional disorder. Molecules are linked by C‐H···O, C‐H···N and C‐H···S intermolecular interactions forming two‐dimensional network. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,thermal and compositional deformations of β‐CsB5O8

The crystal structure of β‐CsB₅O₈ has been determined from X‐ray powder diffraction data using synchrotron radiation: Pbca, a = 7.8131(3) Å, b = 12.0652(4) Å, c = 14.9582(4) Å, Z = 8, ρ_calc = 2.967 g/cm³, R‐p = 0.076, R‐wp = 0.094. β‐CsB₅O₈ was found to be isostructural with β‐KB₅O₈ and β‐RbB₅O₈. The crystal structure consists of a double interlocking framework built up from B‐O pentaborate groups. The crystal structure exhibits a highly anisotropic thermal expansion: α_a = 53, α_b = 16, α_c = 14 · 10^‐6/K; the anisotropy may be caused by partial straightening of the screw chains of the pentaborate groups. The similarity of the thermal and compositional (Cs‐Rb‐K substitution) deformations of CsB₅O₈ is revealed: increasing the radius of the metal by 0.01 Å leads to the same deformations of the crystal structure as increasing the temperature by 35°C. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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 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).     

Crystal structure of 3‐hydroxy methyl 4,6‐dimethoxy‐9‐phenylsulfonyl‐carbazole

The crystal structure of 3‐Hydroxy methyl 4,6‐dimethoxy‐9‐phenylsulfonyl‐carbazole. (C₂₁H₁₉NO₅S) has been determined [CCDC 194425]. The compound crystallizes from methanol in the monoclinic system, space group I2/c, with unit cell parameters: a = 20.498(2), b = 9.258(2), c = 21.866(3)Å, β = 116.450(10)°, Z = 8, V = 3715.2(10)ų. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.050 with 3508 unique reflections. The planar carbazole ring fragment is inclined at an angle of 79.9(1)° to the phenylsulfonyl group. The sum of the angle about N is 351.6(2)°. The atoms linked to the central hexavalent S atom are arranged in a tetrahedral configuration with the larger deviations in the O‐SO angles [O1‐S‐O2 = 119.7(2)°] and the O1‐S‐N and O2‐S‐N angles [106.1(2) and 106.9(1)°, respectively].