Crystal structure of R(–)–1–Tosyl–2–methylpyrrolidine

The crystal structure of R(–)-1-tosyl-2-methylpyrrolidine has been determined by X-ray structure analysis. The compound crystallizes in the monoclinic space group P2₁ with cell parameters a = 7.858(1), b = 14.929(6), c = 11.128(1) Å, β = 105.42(1)°. The structure has been solved by direct methods and refined to R = 0.046. There are two crystallographically independent molecules A and B in the asymmetric unit. The pyrrolidine ring of molecule A is disordered with atom C4 occupying two possible sites. The S atom has a distorted tetrahedral coordination in both the molecules. Two bifurcated hydrogen bonds are observed. Molecules are held together by hydrogen bonds.     

2′-Methyl-3′-nitroflavone

The crystal and molecular structure of the title compound has been determined by direct methods and refined to a final R of 0.044. The compound crystallizes in space group P2₁/n with cell dimensions a = 16.681(2), b = 3.838(1), c = 20.550(4) Å, and β = 104.21(2)°. The phenyl and benzene rings of the title molecule are quite planar. The γ-pyrone ring exhibits maximum deviation 0.032(4) Å from planarity and makes a dihedral angle of 139.8(2)° with the 2-phenyl substituent.     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Double Salt Formation in the Cu(HCOO)2–Sr(HCOO)2–H2O System

The solubility in the Cu(HCOO)₂–Sr(HCOO)₂–H₂O system has been studied by the method of physico-chemical analysis at 25 and 50 °C. It has been established that two double salts are formed in the system: CuSr₂(HCOO)₆ · H₂O at 25 °C and CuSr(HCOO)₄ · 4 H₂O at 50 °C. The latter salt has not yet been described in the literature. It has been characterized by X-ray powder diffraction and DT and TG analysis. CuSr(HCOO)₄ · 4 H₂O crystallizes in the triclinic system with lattice parameters a = 12.376(6) Å, b = 13.394(4) Å, c = 11.508(6) Å, α = 93.38(3)°, β = 94.01(3)°, γ = 75.04(3)°. Dehydration proceeds in two stages.     

Crystal structure of 4-(2-hydroxyethyl)-4-aza-5α-androstan-17β-ol “HS-478”

The crystal structure of HS-478 (aqueous solvate) has been determined by direct method and refined by block diagonal least squares to R₀ = 0.043. The intensity was measured in a four-circle diffractometer in the ω/2θ scanning mode, CuKα radiation. The crystals are triclinic P1, a = 6.721(3), b = 66.532(3), c = 12.188(5) Å, α = 96.86(2)°, β = 82.82(2)°, and γ = 114.68(2)°. Rings A, B, C are chair whereas ring D is envelope. Rings A/B and B/C are trans fused, whereas rings C/D are quasi trans. The hydroxyethyl side chain connected to N(4) has conformation of (−t, t).     

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)     

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 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].     

Synthesis and crystal structure determination of 6,7‐dihydro‐2‐methoxy‐4‐(substituted)‐5H ‐benzo[6,7]cyclohepta[1,2‐b ]pyridine‐3‐carbonitrile

The compounds 6,7‐dihydro‐2‐methoxy‐4‐(4‐methylphenyl)‐5H ‐benzo[6.7]cyclohepta[1,2‐b ]pyridine‐3‐carbonitrile (compound IIIa) and 4‐(4‐chlorophenyl)‐6,7‐dihydro‐2‐methoxy‐5H ‐benzo[6,7]cyclohepta[1,2‐b ]pyridine‐3‐carbonitrile (compound IIIb) were synthesized and their structures have been determined from three dimensional X‐ray data using direct method and refined by full matrix least squares with anisotropic thermal parameters for non‐hydrogen atoms to conventional R(gt) of 0.036 and 0.038 for the two compounds respectively. For compound (IIIa) the crystals are monoclinic, space group C_c, with a=11.2909 (5) Å, b=17.7755(8) Å, c=9.1437(4) Å and β=95.428(3)°, while the crystals of the second compound (IIIb) are triclinic, space group P1, with a=8.7465(3)Å, b=10.3958(3)Å, c=10.9011(4)Å, α= 108.3870(10)°, β=101.3741(12)°, γ=97.9594(12)°. The molecular structure of the two compounds have nearly the same configuration, where the cyclohepta ring takes the boat shape and the methoxy and the carbonitrile groups are attached at the same position C₂ and C₈. The difference occurs only at the position C₄, where the substituent is methylphenyl for compound (IIIa) and chlorophenyl for the other. The bond lengths, valency angles and the hydrogen bonding were calculated and fully discussed. (© 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 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 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 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)     

Crystal and Molecular Structure of 1-Cyano, 4(Trans-1′, N-Pentyl-Cyclohexyl-4′-Carboxy)-Benzene,ECH-5

The crystals of ECH-5 belong to the triclinic system, the space group is P1 with two molecules in the unit cell. The lattice dimensions are a = 9.153(2), b = 16.848(3), c = 5.770(4) Å, α = 97.26(5), β = 93.68(4), γ = 93.07(2)°. The structure was solved by direct methods and was refined using block diagonal least squares method to a final value of R₀ = 0.083 for 1787 observed reflections. The cyclohexane ring is chair. Torsion angles calculations showed that the middle part of the molecule is bent. The molecules are packed in head to tail manner, and they are arranged nearly parallel to each other.     

Refined Crystal and Molecular Structure of Andrographolide — Diterpene

A refined crystal structure of andrographolide has been obtained by X-ray anaysis using CuKα radiation. It crystallizes in the monoclinic crystal system with unique b-axis in space group P2₁. The unit cell parameters are a = 6.552(2) Å, b = 8.009(1) Å, c = 17.989(1) Å and interaxial angle β = 97.32(1)°. The structure has been solved by direct methods and was refined up to R = 0.041, ωR = 0.0464. Both the cyclohexane rings are in chair conformation with the furan ring in twist conformation. The crystal structure is stabilized by hydrogen bonding.     

Structural analysis of bis{(N,N′–dimethylformamide) (μ‐formato)[μ‐bis(salicylidene)–1,3‐propanediaminato] nickel(II)} copper(II) and zinc(II) monohydrate hetero‐trinuclear complexes

The two linear hetero‐trinuclear metallic complexes with Cu²⁺, Ni²⁺ and Zn²⁺ ions, [CuNi₂ {(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(I) and [ZnNi₂{(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(II), form crystals which belong to the monoclinic system, space group P2₁/c, with unit cell dimensions a=10.537(4), b=16.612(5), c=13.837(3) Å, β=111.09(5)°, V=2259.8(12) ų in (I) and a=10.525(4), b=16.658(5), c=13.826(3) Å, β=111.11(5) °, V=2261.4(8) ų in (II), respectively. The coordinations around the M (Ni²⁺, Cu²⁺, Zn²⁺) ions in the title complexes are distorted octahedrals. The stereochemistries of the bridge ligands, linking to the metal ions each other, are changed between Ni…M (Cu²⁺, Zn²⁺) distances. The Ni…M (Cu²⁺, Zn²⁺) distances are 3.0469(13) and 3.0645(14), respectively. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular structure of 3,3-Diethyl–2,4,6–[1 H,3 H,5 H] Pyrimidine Trione

C₈H₁₂O₃N₂, M_r = 184.19, Trigonal, R3 (hexagonal axes) a = b = 26.800(1) Å, c = 6.828(3) Å, α = β = 90°, γ = 120°, V = 4247.11 ų, Z = 18, D_m = 1.297 Mg m⁻³, D_c = 1.296 Mg m⁻³, mu = 0.79 mm⁻¹, F(000) = 1764, T = 293 K, final R = 0.080 for 1205 observed reflections. There are two crystallographically independent molecules in the unit cell of the title compound.     

Crystal and molecular structure of the chiral compound 4–(2–methylbutyloxy)phenyl–4–(2-propenyloxy)-benzoate,C21H24O4

The enantiomeric [(S)-(–)-MBP3B] and the racemic form [(±)-MBP3B] of the title compound with the formula C₃H₅O–C₆H₄–CO₂–C₆H₄–OC₅H₁₁ were studied by single crystal analysis at room temperature. (S)-(–)-MBP3B crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 7.835(3) Å, b = 11.093(6) Å, c = 44.820(3) Å and 8 molecules per unit cell. The structure was determined from 966 reflections with intensities > 3σ. The refinement with isotropic temperature factors leads to R = 0.094. The crystals of the racemic form are monoclinic, space group P2₁/a with a = 7.899(5) Å, b = 11.046(6) Å, c = 22.845(12) Å, β = 99.28(3)°, Z = 4.1236 diffractometer data (I > 3σ) were refined by least-squares methods with anisotropic temperature factors for the non-H atoms to R = 0.070. The packing arrangement for both forms shows a layer-like structure with very similar packing coefficients, k = 0.7085 for the pure enantiomer and k = 0.7014 for the racemic form.     

Structural features of a new [Fe(nicotinamide)2(H2O)4]·[Fe(H2O)6]·(SO4)2·2H2O complex

A new nicotinamide complex of Fe(II) cation was prepared by reaction between ferrous sulfate and nicotinamide in aqueous solution. The complex was characterized on the basis of elemental analysis, FT IR and UV–VIS spectroscopy, electrochemistry (cyclic voltammetry) and X–ray crystallography. The complex consists of the molecular composition of [Fe(nicotinamide)₂(H₂O)₄]· [Fe(H₂O)₆]·(SO₄)₂·2H₂O. The complex crystallizes in the monoclinic space group P 2₁/c [a = 12.862(3), b = 7.110(3), c = 16.382(3) Å; β = 95.79(2)°]. It has been proven that nicotinamide is coordinated to Fe(II) through the nitrogen atom of its heterocyclic ring. © 2006 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)