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 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).     

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 structure and properties of [Cu(sac)2(py)3], a new example of a mononuclear complex with both N‐ and O‐bonded saccharinate ligands

The crystal structure of the title complex has been determined by single X‐ray diffraction methods and refined to an R‐value of 0.0543. It crystallizes in the monoclinic P2₁/a space group with a = 21.1231(9), b = 9.4523(4), c = 16.1874(7) Å, β = 107.3706(3)° and Z = 4. The compound represents only the second known example of a simple mononuclear metal complex containing simultaneously N‐ and O‐bonded saccharinato ligands. Its infrared spectrum and thermal behavior are also briefly discussed.     

Crystal and molecular structure of 2,6‐bis(4‐chlorophenyl)‐3‐phenylpiperidin‐4‐one

The crystal structure of the title compound is described. The chemical formula of the compound is C₂₃H₁₉Cl₂NO. The compound is found to crystallize in monoclinic system with space group P2₁/c, Z = 4. The unit cell dimensions are a = 15.137(3) Å, b = 8.9171(18) Å, c = 14.779(3) Å, β = 91.461(4)° and V = 1994.2(7) ų, D_calc = 1.320 gcm^‐3. The final R factor is 4.4%. The central piperidone ring of the molecule adopts a slightly distorted chair conformation, the mean torsion angle being 52.3°; the phenyl rings are planar. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Structure Analysis of a New Coumarin Derivative

The title compound (6,6‐dimethyl‐cis‐6H,6aH,7H,12bH,13H‐bis[1]benzopyrano[4,3‐b:4',3'‐d]pyran‐13‐one) crystallizes in monoclinic space group P2₁ /c with Z = 4. The unit cell dimensions are a = 8.6231(2) Å, b =10.0260(2) Å, c = 19.8376(2) Å, and β = 102.1(1)°, V = 1674.51(5) ų , D_cal = 1.326 Mg/m³. The coumarin moiety is in the planar conformation, the dioxadecalin moiety is cis fused and within the dioxadecalin moiety both the rings are in half cahir/sofa conformations. The structure has many C‐H … O type interactions.     

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].     

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 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)     

Structure determination of two asymmetrically substituted oxadiazoles from powder diffraction data

The crystal structures of the 1,3,4 oxadiazole compounds N,N‐dimethyl‐N‐[4‐(1,3,4‐oxadiazol‐2‐yl)phenyl]amine ( 1 ) and 2‐methyl‐5‐phenyl‐1,3,4‐oxadiazole ( 2 ) have been determined. In case of 1 no adequate crystals were available; therefore the structure was solved at room temperature from X‐ray powder diffraction data using the method of simulated annealing. This solution is compared to a second one obtained by applying the molecular replacement method. Subsequent Rietveld refinements combined with the so called two stage method based on the data collected to 1.6 Å resolution yielded an R_wp value of 7.27% for 1 . Compound 1 crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice parameters of a = 7.599(4) Å, b = 6.004(2) Å, c = 21.736(3) Å. The crystal structure of 2 was solved by means of single crystal structure analysis (monoclinic space group P2₁/c, a = 8.010(3) Å, b = 10.783(4) Å, c = 19.234(7) Å, β = 90.794(9)°). (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 3‐phenyl‐4‐(p‐chlorobenzylamino)‐4,5‐dihydro‐1‐H‐1,2,4‐triazol‐5‐on

The structure of the title compound, C₁₅H₁₃N₄OCl was determined by single crystal X‐ray diffraction technique. The structure consists of a p‐chlorobenzylamino moiety and triazol and phenyl rings. The title compound crystallizes in the monoclinic space group P2₁/c with a = 14.368(3), b = 6.255(3), c = 17.631(3) Å, β = 113.24(3)°, Z = 4, V = 1455.8(8) ų and D_x = 1.372 gcm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.0477). The dihedral angle between the triazole moiety and the phenyl ring is 28.8(3)°. The molecular packing is stabilized by N‐H…N and N‐H…O types of inter molecular hydrogen bonds. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Structure of N,N'‐Bis(3‐(o‐dimethylaminoimino‐ethyl) ‐2‐hydroxy‐5‐methyl)‐benzylpiperazine

The structure of the synthesized title compound, C₃₀H₄₆N₆O₂ , was solved by using X‐ray diffraction techniques. The compound crystallized in monoclinic space group P2₁/n with cell dimensions a = 14.0629(7), b = 6.5696(3), c = 17.7948(8)Å, β = 111.35(2)°, V = 1531.2(1)ų, Z = 2, D_cal = 1.134 Mgm^‐3 and T = 293(2)K. The molecule possesses a center of symmetry, and hence, there is half a molecule in the asymmetric unit. The piperazine ring adopts chair conformation with the substituents at the equatorial position, subtending a dihedral angle of 88.87(1)° with the phenyl ring. The phenyloxy hydrogen is involved in an intramolecular O‐H...N type of hydrogen bond.     

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.     

The Crystal and Molecular Structure of 11,12‐dibromo‐ 7,8—benzo‐1,5‐di(p—tolylsulphonyl)‐1,5‐diazacyclononan

The crystal structure of the title compound, C₂₅H₂₆Br₂N₂O₄S₂ was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/c, with a=20.7142(2) Å b=11.7910(2) Å, c= 10.6735(3) Å, β=98.549(2)°, V=2577.94(9) ų, Z=4. The structure was solved by direct methods and refined by least‐squares methods to a final R=0.046 for 1866 observed reflections with I>2sigma(I). The title compound, displays disordered geometry around the C1 atom located almost on twofold axis. The nine‐membered heterocylic ring is close to the half‐chair conformation. The dihedral angle between phenyl rings is 34.2(1)°.     

Crystal and molecular structure of trans‐(±)‐3‐acetoxy‐2‐(4‐methoxyphenyl)‐4‐oxo‐2,3,4,5‐tetrahydro‐1,5‐benzothiazepine‐1‐oxide

The title compound is a structurally related isomer of diltiazem, a well known drug. This compound (C₁₈H₁₇NO₅S) crystallizes in the space group P2₁/n with a = 13.803(4), b = 7.704(3), c = 16.093(3) Å, β = 105.37(2)º, Z = 4, V = 1650.1(9) ų. The least‐squares refinement gave residual index R = 0.067 for 2831 observed reflections. The distorted seven‐membered ring in the molecule shows twist‐boat conformation. Hydrogen bonds in which the amide group at one molecule and a carbonyl group in the adjacent molecule are involved to form centrosymmetric dimers in the crystal. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure investigation of pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide

Pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide (I), is a higher homologue of 1‐oxopyridinium‐2‐thioacetic acid (II) [1]. It crystallizes in monoclinic space group P2₁ with a = 9.2168(2) Å, b = 4.1423(2) Å, c = 11.3904(4) Å, β = 98.65(2)°, V = 429.93(3) ų and Z = 2. The least‐squares refinement gave residual index R = 0.024 for 1070 observed reflections. The introduction of an additional methylene group in (II) causes a flip in the carboxylic acid group of (I) that facilitates the molecules to align infinite antiparallel chains through strong C–H···O interactions. The molecules are interlinked by O–H···O hydrogen bonding across the chains and forming an infinite screw chain along y‐direction. The molecular packing is stabilized by O–H···O and C–H···O hydrogen bonding and π‐π electron interactions. This is an important facet of the crystal packing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a 3‐D supramolecular Cu/Mn complex with pydc

A supramolecular compound, {[CuMn(pydc)₂(H₂O)₅]·2H₂O} ( 1 ) (pydc = pyridine‐2,6‐dicarboxylate dianion), has been synthesized and characterized by single‐crystal X‐ray diffraction. Single‐crystal X‐ray analysis reveals that it crystallizes in the triclinic space group P‐1, a = 8.4763(17) Å, b = 9.7715(19) Å, c = 13.909(3) Å, α =101.234(3)°, β =102.520(3)°, γ= 97.375(4)°. Two mixed‐metal ions exhibit similar coordinated geometries with octahedron. 1 possesses a 3‐D unusual supramolecular network featuring 1D water tape. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Structure of Spiro[2‐benzoyl‐cyclohexyl‐4,5‐diphenylpyrrolidine‐3,3'‐chroman‐4‐one]

3‐Phenyl‐chroman‐4‐one is the basic unit of isoflavonoids which are found in the plants of the sub‐family papilionoidae of Leguminosae. They are known to possess antifungal and antibacterial properties. Crystal data of the title compound : Monoclinic, space group P2₁/c, a = 14.021(3), b = 18.682(4), c = 11.362(2) Å, β = 95.75(3)°, R = 0.066. The two phenyl rings directly attached to the pyrrolidine ring are nearly perpendicular to it. The dihydropyrone moiety adopts a half‐chair conformation while the cyclohexane ring attached to the pyrrolidine ring adopts a chair conformation. The best plane passing through the chroman‐4‐one moiety makes a dihedral angle of 82.2(3)° with the pyrrolidine ring. The molecule is stabilized by one intra‐ and two intermolecular C‐H...O hydrogen bonds.     

Crystal Structure of the Amine‐Carbonato‐Cobalt(III) Complex [Co(CO3)(L1)]ClO4 with Aminoalkyl Pendant‐Arm [12]eneN4, L1 = 9‐(3‐aminopropyl)‐1,5,9‐Triazacyclododecene

The crystal and molecular structure of the title complex [Co(CO3)(L1)]ClO4 was determined from X‐ray diffraction data using direct methods. The crystals are monoclinic, a = 13.588(4) Å, b = 9.049(3) Å, c = 15.569(6) Å, β = 114.75(2)°, Z = 4, V = 1738.5(10) ų, space group P21/n. The structure consists of isolated [Co(CO3)(C12H26N4)]+ complex cations, with distorted octahedral geometry and ClO4‐ counter anions. The results are discussed in relation to similar macrocycle and carbonato analogues.