Crystal and molecular structure of 1,1′-ferrocene-dicarbaldehyde

The crystal and molecular structure of 1,1-ferrocene-dicarbaldehyde 1 is reported. Crystal data for 1: monoclinic, space group P2₁/n, a = 5.876(1), b = 11.349(1), c = 29.460(3) Å, = 95.067(2)°, V = 1956.9(3) ų, and D _c = 1.64 g/cm³, for Z = 8. The complex crystallizes such that two molecules are located in the asymmetric unit in which the complexes display different degrees of twisting of the cyclopentadienyl (Cp) rings and formyl substituents about the Cp—Fe—Cp and Cp—COH axes, respectively. The molecule self-assembles in the solid state to form a 2D layered structure held together by - interactions and C—H···O hydrogen bonds.     

Crystal and molecular structure of 2′,4′-dimethoxyflavone

C₁₇H₁₄O₄,M _r =282.3, triclinic,P-1,a=8.469(3),b=8.516(2),c=20.425(8)Å,=84.95(3),=81.98(3), =70.47(2)°,V=1373(13)ų,Z=4,D _x =1.365 g cm^–3, (MoK )=0.71069 Å,=0.91 cm^–1,F(000)=592,T=294K,R=0.038 for 3577 observed reflections (F>3 (F)). The asymmetric unit is composed of two molecules. These two molecules, which are in planar conformations, differ in 4-methoxyl group orientation. Short intramolecular contacts are found between the -benzopyran portion and the dimethoxyphenyl ring.     

Crystal structure of bis-N,N′-p-chlorosalicylideneamine-1,2-diaminobenzene

The crystal structure of the title compound, C₂₀H₁₄N₂O₂Cl₂, has been determined by single crystal X-ray diffraction techniques. It crystallizes in the orthorhombic system witha=7.532(3)Å,b=18.563(2)Å,c=25.089(3)Å, space groupPbca,V=3507.9(3)ų,Z=8,F(000)=1584.D _x =1.459 g cm^–3,M=385.3 a. m. u., (MoK)=0.7107 Å, =3.35 cm^–1,T=297°K,R=0.086,R _w =0.049 for 2119 unique diffractometer data. The molecules are linked by van der Waals forces.     

Crystal and molecular structure of 4′-hexyloxyphenyl 4-pentylbenzoate

The molecular and crystal structure of 4??-hexyloxyphenyl 4-pentylbenzoate, C₆H₁₃O-C₆H₄-COO-C₆H₄-C₅H₁₁, which is a liquid-crystal compound, was determined by X-ray diffraction. This compound forms a nematic phase upon melting. The crystal contains three crystallographically independent molecules. In one of them, the alkyl chain is disordered. This is indicative of the looseness of the crystal packing in the aliphatic region. The crystal structure is stabilized by the following two types of weak directional interactions: hydrogen bonds with the participation of the terminal O atom of the ester group and the C-H group of one of the benzene rings and C-H????-system interactions. Only one of the three independent molecules is involved in the latter type of interactions. Hence, the structurization of the mesophase is most likely determined by hydrogen bonding.     

Crystal structure ofcatena-O,O′-diethylphosphonoacetatotriphenyltin

Triphenyltin diethylphosphonoacetate, which crystallizes in the monoclinc space groupP2₁/c (a=15.154(4),b=9.159(3),c=17.685(4) Å, =91.410(8)°), adopts a polymeric structure in which planar triphenyltin cations (_C—Sn—C=357.3(6)°) are axially linked by the diethylphosphonoacetato anions (Sn–O_esteryl=2.129(3), SnO_phosphoryl=2.420(3) Å; O–SnO=171.9(1)° into chains that propagate by translations along theb-axis. The structure has been erfined toR=0.037 for 3384I3(I) reflections.     

Crystal structure of 3,3′-dimethoxybenzydine (2-hydroxybenzal)diimine

Molecular and crystal structure of 3,3'-dimethoxybenzydine(2-hydroxybenzal)diimine, C₂₈H₂₄N₂O₄, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a= 18.045(2) Å, b= 11.725(4) Å, c= 12.436(6) Å, = 120.03(3)°, Z=4, D _x =1.32 g/cm³, (MoK) =0.089 mm^–1, and space group is C2/c. The structure was solved by direct methods and refined to a final R=0.056 for 2325 reflections with I > 2(I). There is half independent molecule in the asymmetric unit. The molecule has a twofold symmetry on the mid point of the C4 C4 ⁱ bond. The N1-C8 imine bond length of 1.284(3) Å is typical of a double bond. The molecule of the title compound is not planar. There is a strong intramolecular hydrogen bond between hydroxy oxygen atom and imine nitrogen atom. The crystal structure is stabilized by a weak intermolecular hydrogen bond of the C H O type forming three-dimensional cage.     

Crystal and molecular structure of 1,4-S,S′-bis-isothiosemicarbazidebutane dihydrobromide

The synthesis and crystal structure of 1,4-S,S-isothiosemicarbazidebutane dihydrobromide have been presented. The crystals are monoclinic:P2₁/n, a=7.9910(10),b=10.979(2),c=8.9240(10)Å, =111.450(10)°,Z=2, room temp. The structure was solved by direct methods. and refined to R=0.0297 for 846 reflections. The title compound consists of the centrosymmetric [C₆H₁₈N₆S₂]²⁺ dication and two Br^– anions. Intramolecular N–H...N and intermolecular N–H...Br hydrogen bonds stabilizetrans conformation of the thiosemicarbazide moiety.     

Crystal and molecular structure of 2-(2′-chloro-5′-nitrostyryl)benzoselenazole

The title compound C₁₅H₉ClN₂O₂Se (nsbse) is orthorhombic, witha=6.823(2),b=7.860(2),c=26.349(5) Å,Z=4,D _x =1.709,(MoK)=28.3 cm^–1,F(000)=720,T=298K in space groupP2₁2₁2₁. The structure was solved by heavy atom and Fourier methods and refined toR=0.045 for 1095 unique observed reflections. The molecule is almost planar, with a dihedral angle of 4.8(2)° between the benzoselenazole and phenyl rings. The C-Se-C angle in the selenazole ring is very small, 84.6(4)°, while the C-N-C angle in that ring is 113.7(7)°.     

Crystal structure of chlorotriphenyltin·diphenylcyclopropenone

Triphenyltin chloride forms with diphenylcyclopropenone a 1/1 molecular complex belonging to the triclinicP¯1 space group (a=10.267(4),b=12.095(2),c=12.319(3)Å,=90.67(2),=101.59(2), =112.58(2)°). The tin atom exists in a distortedtrans-trigonal bipyramidal (Sn-C=2.112(3), 2.123(3), 2.137(4), Sn-C1=2.440(1), Sn-O=2.510(2)Å) geometry, being displaced out of the equatorial plane (EC-Sn-C=354.3(3)°) towards the apical chlorine atom by 0.269(1)Å.     

Crystal structure of a nucleoside analogue, 2′,3′-dideoxy-3′-fluoro-5-chlorocytidine

The title compound, 1-(2,3-dideoxy-3-fluoro--d-erythro pentofuranos-1-yl)-5-chlorocytosine, crystallises in the orthorhombic space groupP2₁2₁2₁ witha=5.142(1),b=14.177(2),c=15.721(2) Å,Z=4. The crystal structure was solved by the heavy atom method and refined by full-matrix least-squares method to a finalR value of 0.031 for 1629 unique observed reflections. The N-glycosidic torsion angle is –156.1(2)° and the sugar moiety is anti to the cytosine base. The sugar pucker is ₂ ³ T withP=178.2(1)° and=31(1)°. The atom 05 is in a +sc conformation with respect to the furanose ring. The molecular packing in the crystal is stabilized by N-HN, N-HO, O-HO hydrogen bonds and C-HO close contacts.     

Crystal structure of a nucleoside analog, 2′,3′-dideoxy-3′-azido-5-chlorocytidine

The title compound, l-(2,3-dideoxy-3-azido--D-erythro pentofuranos-1-yl)-5-chlorocytosine, crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=5.840(1),b=13.780(1),c=15.396(2)Å,Z=4. The structure was solved by direct methods and refined by full-matrix least-squares calculations to a finalR value of 0.033 for 1688 unique observed reflections. The N-glycosidic torsion angle has a value of –160.8(1)°, in the and range. The sugar pucker is ₂ ³ T withP=180(1)° and=34(1)°. The C4–C5 conformation is +sc with =50.8(2)°. The azido group is nonlinear and oriented trans to the C3–C4 bond. The molecular packing in the crystalline space is stabilized by N-HN, N-HO, O-HO hydrogen bonds and C-HO close contacts.     

Crystal structure of a nucleoside analog: 2′,3′-dideoxy-3′-fluoro-5-bromocytidine

The title compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=5.084(1),b=14.322(3),c=16.065(2)Å,Z=4. The structure was solved by the heavy atom method and refined by full-matrix least-squares calculations to a finalR value of 0.033 for 1106 unique observed reflections. The N-glycosidic torsion anglex has a value of –153.7(4)°, in the anti-range. The sugar pucker is²T₃ withP=175(1)° and=30(1)°. The C4-C5 conformation is + sc with =46.7(7)°. The structure is stabilized by N-HN, N-HO and O-HO hydrogen bonds and C-HO close contacts.     

Crystal structure of 2,5-cyclohexadien-4-one-spiro-3′-(2′-methylthio-5′,5′-dimethyl-1′-pyrroline)

The crystal structure of the pyrrole derivative 2,5-cyclohexadien-4-one-spiro-3′-(2′-methylthio-5′,5′-dimethyl-1′-pyrroline) is determined by X-ray diffraction. Two independent molecules have similar structures and close geometric parameters but differ in configuration of the pyrrole ring and orientation of the thiomethyl group with respect to the pyrrole ring.     

Crystal structure of 5-(2′-aminophenyl)-2-dimethylamino-1,3,4-thiadiazole

The crystal structure of 5-(2′-Aminophenyl)-2-dimethylamino-1,3,4-thiazole is determined by X-ray diffraction. The compound is prepared by an unusual recyclization of 3-N, N-dimethylthioureidoquinazolin-4(3H)-one. The crystal is monoclinic, space group P2₁/c, a = 7.420(2) Å, b = 10.466(5) Å, c = 14.752(9) Å, β = 109.2(4)°, ρ_calcd = 1.359 g/cm³, and Z = 4 for the C₁₀H₁₂N₄S composition. The molecule consists of the thiadiazole and phenyl rings and the dimethylamine N(CH₃)₂ and amine NH₂ groups attached to the rings. The molecule as a whole is planar. The dihedral angle between the rings is 8.9°. The N(1) and N(4) atoms in the molecule are bound through the intramolecular interaction (2.76 Å). Molecules, which are linked in pairs by antiparallel hydrogen bonds, form a framework structure.     

Crystal structure of 2,2′-diformyl 4,4′-dimethyl 6,6′-[piperazine-1,4-diyl bis-(methylene)]bis phenol

The title compund C₂₂H₂₆N₂O₄,Mr=382.46 crystallizes in the orthorhombic space group P2₁2₁2₁ with =8.867(1)Å,b=13.228(2)Å,c=17.029(3)Å,V=1956.7(2)ų,Z=4, D_cal=1.30 Mgm^–3,F(000)=816, =6.89 cm^–1, (CuK)=1.5418 Å andT=298 K. The structure was solved by direct methods and refined by full-matrix least-squares. The finalR=0.046 for 1995 unique reflections. The phenyl rings are coplanar (oriented at an angle of 6.4(1)^o) and orients at an angle of 112.2(1)^o and 115.7(1)^o, respectively with the piperazine ring. The piperazine ring adopts achair conformation and the substituents at the N-atoms are in an equatiorial position.DCB Contribution No. 823.     

Crystal structure of 5α-cholest-6-one

The crystal and molecular structure of the steroid 5α-cholest-6-one has been determined by X-ray diffraction analysis. The compound crystallizes in space group P2₁ with the unit cell parameters a = 10.575(1) Å, b = 7.698(1) Å, c = 15.284(2) Å, β= 99.34(1)°, V = 1227.72 ų, Z = 2, and R = 0.054 for 1634 observed reflections. The six-membered rings (A, B, and C) have the chair conformations, whereas the five-membered ring Dis intermediate between 13β-envelope and 13β-14α half-chair. All the rings of the steroid skeleton are trans connected. The molecules are linked together by the intermolecular C-H?O hydrogen bonds.     

Crystal and molecular structure ofN,N′-diphenylpiperazine N,N′-dioxide octahydrate

The title compound isN,N-DiphenylpiperazineN,N-dioxide octahydrate, C₁₆H₃₄N₂O₁₀:M _r=414.46, orthorhombic, space groupPnma (No. 62),a=12.327(2),b=9.804(1),c=17.443(4) Å,V _c=2108.1(5) ų,Z=4. The structure was solved by the direct method and refined toR=0.056 for 3032 observed MoK reflections. In theN,N-dioxide molecule, all atoms except those of the methylene groups lie on a crystallographic mirror plane. The piperazine ring takes the chair form, with two N-O bonds oriented axially in atrans configuration. The crystal structure is characterized by strong hydrogen bonding between the water molecules, as well as between theN-oxide groups and water molecules, giving rise to a three-dimensional network structure composed of edge-sharing four-membered, five-membered, six-membered, and fourteen-membered rings.     

Crystal structure of 1,4-dihydro-1-methyl-3′-methylsulfinyl-4-oxo-6-nitro-3,4′-diquinolinyl sulfide complex with DMF

The title compound crystallized as a complex with N,N-dimethylformamide (DMF) in a monoclinic space group P2 ₁ /c with a = 9.469(2), b = 25.168(5), c = 9.860(3) Å, and = 97.48(3)°. The two quinoline moieties are nearly perpendicular. The sulfoxide oxygen is pointed toward the H-2 proton. The S-methyl group is perpendicular to the parent pyridine ring plane.     

Crystal structure of tetrachlorobisd[μ-imidocarbonylchloridato]diboron

Boron trichloride and mercuric cyanide react slowly to form the title compound, B₂N₂C₂Cl₈, which contains a four-membered B₂N₂ ring with alternating BCl₂ and N—CCl₂. Crystals are triclinic, space group P , a = 6.1198(1), b = 7.4457(3), c = 7.9186(3) Å, = 117.064(2), = 106.923, = 93.712(2)°, Z = 1, and V = 299.07(2) ų. The compound has a crystallographic center of symmetry but the metric symmetry is close to the expected mmm.     

Crystal and molecular structure of aquabis(2,2′-bipyridine)nitratomanganese(II) nitrate monohydrate

A new monomeric manganese(II) nitrate complex with 2,2-bipyridine (bpy), [Mn(bpy)₂(NO₃)(H₂O)](NO₃)·H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group witha=9.721(3),b=14.691(5),c=8.578(3) Å, =106.79(3), =96.05(3), =82.55(3)°,V=1159.9 ų andZ=2. The structure comprises discrete cation [Mn(bpy)₂(NO₃)(H₂O)]⁺ in which the metal atom is coordinated by a pair of bidentate bpy ligands [Mn–N=2.261(4)–2.299(4) Å], a unidentate nitrato [Mn–O=2.284(4) Å] and aqua [Mn–O=2.160(3) Å] ligands in a highly distorted octahedral arrangement.