Crystal and molecular structure of 2-(1,3-benzothiazol-2-yl)-2-(4-tert-butylcyclohexylidene)ethanonitrile

The crystal and molecular structure of the title compound (C₁₉H₂₂N₂S) has been investigated by single crystal X-ray methods. The crystals are orthorhombic, space groupPbca, with cell dimensions:a=12.082(2)Å,b=11.460(2)Å,c=25.128(4)Å. The structure was solved by direct methods, and refined with 1225 independent reflections by a full-matrix, least-squares procedure, which converged toR=0.042. The benzene and thiazole planes are coplanar and the cyclohexane ring adopts a chair conformation.     

Crystal and molecular structure of grayanotoxin VII

The crystal and molecular structure of a grayanotoxin VII is presented. The crystal is monoclinic, space group P2₁, with a = 7.647(1) Å, b = 11.7591(7) Å, c = 10.0873(6) Å, = 91.143(8)°, V = 906.9(1) ų, Z = 2. The structure was solved by direct methods and refined by full-matrix least-squares methods to a final R = 0.057 for 1494 independent reflections. The molecule has a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered rings.     

An X-ray diffraction study of mesoionic 1-thia-2,3,4-triazolo-5-aminidine and some of its derivatives

X-ray diffraction data are presented for the title mesoionic compound (I), its hydrochloride salt (II) and methylated derivative (III). The crystal of (I) is orthorombic, space group P2₁2₁2₁, with cell dimensions: a = 5.857(1) Å, b = 12.494(2) Å, c = 16.328(3) Å, with four molecules per unit cell. The crystal of (II) is monoclinic, space group P2₁/n, with cell dimensions: a = 5.5720(10) Å, b = 21.5770(4) Å, c = 11.2330(2) Å, beta = 95.15(3)°, with four molecules per unit cell. The crystal of (III) is monoclinic, space group P2₁/n, with cell dimensions: a = 12.0886(5) Å, b = 7.9103(4), c = 104.29(1) Å, beta = 104.29(1)°, with four molecules per unit cell. Of particular interest is the fact that the C5–N6 bond appears to have a high double bond character in all three of the compounds studied. In addition, it is found that the exocyclic N-phenyl group changes from being in the cis conformation with respect to sulfur in compounds (I) and (III) to the trans conformation in the hydrochloric salt (II).     

The crystal and molecular structure of chandonium dibromide: A synthetic bisquaternary aza steroidal neuromuscular blocking agent

The crystal and molecular structure of 17a-methyl-3-pyrrolidino-17a-aza-D-homo-5-androstene dimethyl bromide (HS818, chandonium dibromide). C₂₆H₄₆N₂Br₂, has been determined crystallographically by the heavy atom method and refined by full-matrix least-squares calculations toR =0.074 for 5045 reflections. The compound crystallizes in space groupP2₁2₁2₁ witha=6.468(2),b=14.055(5),c=28.216(11) Å. The N⁺...N⁺ inter-onium distance in chandonium bromide is 10.32 Å, close to the distance of 10.29 Å observed in chandonium iodide. Rings A, C, and D have a chair conformation and ring B is in a half-chair conformation. Ring E has a distorted envelope conformation. All rings in the steroid skeleton aretrans-connected.     

X-ray crystal structure of cytochalasin D produced by Tubercularia sp., a novel endophytic fungus of Taxus mairei

The crystal structure of cytochalasin D, which was isolated from Tubercularia sp., a novel endophytic fungus of Taxus mairei, and cocrystallized with dimethyl sulfoxide, is reported. The title compound crystallizes in the monoclinic space group P2₁, with a = 7.583(6) Å, b = 11.053(10) Å, c = 18.632(10) Å, = 95.79(6)°, V = 1553.6(3) ų, Z = 2. The structure was solved by direct methods and refined by least-squares methods to a final R factor of 0.103 for 2937 independent reflections.     

X-ray structure of sesterterpene, 16β-acetoxy-24-methyl-12,24-dioxoscalaran-25-al

The molecular geometry of a tetracyclic sesterterpene has been determined by X-ray diffraction. The conformation of the aldehyde group as observed in the crystal structure supports the rationalization for the absence of aldehyde proton coupling in the nmr spectra of the compound. Crystal data: C₂₈H₄₂O₅, M.W.=458.6; orthorhombic, P2₁2₁2₁;a=10.797(2),b=29.270(9),c=8.033(1)Å,V=2538.7ų,Dx=1.199 g cm^–3;R=0.045 for 2287 observed reflections.     

Separation of 4-aminobenzoic acid by cocrystallization: Crystal structure of the complex of 4-aminobenzoic acid with (2R,3R)-tartaric acid

4-Aminobenzoic acid (PABA) has been successfully separated from a mixture containing 2-aminobenzoic acid and (2R,3R)-tartaric acid. X-ray structure analysis confirms the separating result. The molecular complex formed by PABA and tartaric acid in 1:1 molar ratio crystallizes in the orthorhombic space group P2₁2₁2₁ with cell dimensions of a = 7.329(1) Å, b = 12.095(2) Å, c = 15.231(3) Å, V = 1350.1(4) ų, Z = 4. The crystal structure comprises protonated PABA, monoanion of tartaric acid, and crystalline water. The extensive H-bonding network exists in the crystal structure. H bonding between tartaric acid and both terminal groups on para position of PABA is considered as a possible reason for the successful separation.     

Studies in molecular structure,symmetry and conformation. IX. Crystal and molecular structure of the mixed crystal of L-threonine and L-allothreonine

The mixed crystal ofL-threonine andL-allothreonine is orthorhombic, space groupP2₁2₁2₁, witha = 13.60(1),b = 7.87(1),c = 5.16(1) Å andZ = 4. The structure, which is closely isomorphous with that ofL-threonine, was solved from photographic data and refined to anR of 11.6%. The structure is spatially disordered, containing the molecules in bothL- andL-allo forms.Contribution No. 394 from the Centre of Advanced Study in Physics, University of Madras, Guindy Campus, Madras-600025, India.     

α-substituted Phosphoryl Compounds (II). The Crystal and Molecular Structure of Diphenyl-[5,6-dichloro-1, 3-benzodioxol-(2)]-phosphine-oxide,C19H13O3PCl2

The compound crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell, and with the lattice parameters a = 11.807 Å, b = 13.070 Å, c = 11.312 Å, β = 96.74°. With X-ray diffraction data collected on a four circle diffractometer, the crystal structure has been determined by direct methods and refined to an R-value of 0.061 for 2735 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

Structure of 9-oxa-2,3-(4′-methoxy)-benzo bicyclo[4,3,0]non-1(6)-ene-7,8-dione: C13H10O4

The crystal and molecular structure of the title compound: C₁₃H₁₀O₄,M _r=230.22, determined by single crystal X-ray diffraction is reported. Crystals are monoclinic, space groupP2_l/c,a=3.991(3),b=21.381(4),c=12.289(4)Å,b=91.15(1)°,V=1048(1)Å₃,z=4,D _x=1.46Mg m^–3, (MoK)=0.7107 Å,m=0.87 mm^–1,F(000)=480,T=298 K. The structure was solved by direct methods and the finalR value is 0.071 (wR=0.055) for 795 independent observed reflections. The cyclohexadienic moiety of the molecule adopt a twist conformation.     

Crystal and molecular structure of 10,20-epoxy-grayanotoxin-II

The photooxidation with HgO in benzene and the hydrolysis with 2%-KOH in methanol of the grayanotoxin (GTX) derivative (4) gave a 10,20-epoxy-grayanotoxin-II(5). The crystal structure of (5) has been determined by X-ray diffraction at room temperature. The crystal is monoclinic, space group P2₁, with a = 14.248(10) Å, b = 6.670(10) Å, c = 9.990(10) Å, = 105.507(8)°, V = 914.9(2) ų, Z = 2. The structure was solved by direct methods and refined by full-matrix least squares methods to a final R1 = 0.046 (wR2 = 0.0833) for 1161 independent reflections. The molecule has a pentacyclic structure consisting of two five-membered, one six-membered, one seven-membered, and one three-membered rings. The three-membered ring is connected with the seven-membered ring by spiro-type bond.     

Synthesis and crystal structure of a 2D (6,3) coordination network, {[Ag(L)1.5]NO3} n [L = 1,3-bis(benzylthio)propane]

A new dithioether silver(I) complex, {[Ag(L)_1.5]NO₃} _n (1) has been prepared by the reaction of AgNO₃ with 1,3-bis(benzylthio)propane (L) in methanol/chloroform. The structure was characterized by single-crystal X-ray diffraction analysis: rhombohedral system, space group R –3c, with a =b = 15.651(7), c = 39.26(4) Å, V = 8328(1) ų, and Z = 6. The crystal structure consists of [Ag(L)_1.5]⁺ cations and NO₃ ^– anions. In 1, each silver(I) center is coordinated equivalently to three sulfur donors from three different ligands to give a trigonal-planar coordination geometry. Each L links two adjacent silver(I) centers in bis-monodentate bridging mode to form a 2D (6,3) network sheet. Furthermore, these 2D sheets are linked by the weak coordination interactions between nitrate ions and silver(I) atoms to form a 3D brick-wall framework.     

Crystal and molecular structure of 1-vinyl-3-methyl-imidazolium iodide,C6H9N2I

The title compound crystallizes with two independent molecules in the unit cell. The two molecules arecis-trans isomers. Crystal data: orthorhombic, P2₁2₁2₁,a=7.0417(6),b=9.5341(9),c=25.411(2) Å,Z=8. The crystal structure has been solved by automated Patterson methods and refined toR=0.024 for 1843 observed reflections.     

Crystal structure of benzyltriphenylphosphonium chloride

The crystal structure of the title compound has been determined from single-crystal X-ray diffractometer data. The crystals are orthorhombic with unit-cell dimensionsa =17.147(3),b = 18.147(3),c = 13.860(3) Å, space groupPbca andZ = 8. Full-matrix least-squares refinement, using 2215 independent reflections, has reachedR = 0.040.The structure contains tetrahedral benzy IPPh₃ cations and free chloride ions. The three P-C(phenyl) distances are in the range 1.785(3)-1.796(3) Å, with a mean of 1.790 Å, while the P-C(benzyl) distance is fractionally larger at 1.811(3) Å. The tetrahedral angles at the phosphorus atom range from 108.0 to 111.6 °. There are indications that one of the phenyl rings may be slightly disordered.     

Structure of 21-fluoro-4,9(11)-pregnadiene-3,20-dion-17α-yl acetate,C23H29O4F

The crystal and molecular structure of 21-fluoro-4,9(ll)-pregnadiene-3,20-dion-17a-yl acetate has been determined by X-ray diffraction methods;P2₁2₁2₁,a=15.827(4),b=16.912(4),c=7.513(2) Å,Z=4;R=0.062, (R _w =0.065) for 2028 unique observed reflections. The progesterone side chain has an unusual conformation; the C16-C17-C20-O20 torsion angle is 173.1(4)°. Molecular mechanics calculations suggest that this conformation may be cuased by 17-acetoxy substituent and the additional double bond between C9 and C11.Research supported in part by RP.II. 10 grant from the Polish Ministry of National Education (to Z. G., P. G., and Z. W.) and by PHS Grant DK26546 (to WLD).     

Preparation and crystal structure of spiro(5,7-dimethoxy-1(1H)oxo-2-benzopyran-3(4H),1′-cyclohexane)

Spiro(5,7-dimethoxy-1(1H)oxo-2-benzopyran-3(4H),1-cyclohexane) (C₁₆H₂₀O₄) was prepared by alkylation of o-lithio 3,5-dimethoxy-N-methyl benzamide with methylene cyclohexane oxide followed by alkaline hydrolysis and its crystal structure was determined by X-ray crystallographic techniques. The compound crystallizes into monoclinic space group P2₁/c with unit cell parameters: a = 11.914(3) Å, b = 9.861(3) Å, c = 12.508(7) Å, = 91.34(3), Z = 4. The structure has been solved by direct methods and refined to R = 0.039 for 1870 observed reflections. The heterocyclic ring adopts distorted sofa conformation while cyclohexane ring assumes a highly symmetric chair conformation. The dihedral angle between the mean planes of isocoumarin nucleus and cyclohexane ring is 105.51(5). Molecules are held together in the crystal by C=H ... O hydrogen bonds.     

Crystal structures of a pair of diastereomeric 3-(N,N-dimethylammonium)-1,1-diphenyl-1-butanol O,O′-di-p-toloyl hydrogen tartrates

The crystal structures of a pair of diastereomeric salts of (–)-(2R, 3R)-O, O-di-p-toloyl tartaric acid and (–)- and ( + )-3-N,N-dimethylamino-1,1-diphenyl-1-butanol have been determined. Crystal data: 3: (-)-(R)-C₁₈HC₂₄NO⁺(-)-(2R,3R)-C₂₀H₁₇O^- ₈ orthorhombic, P2₁2₁2₁, a = 7.873(2), b = 15.343(3), c = 28.76(1) Å, V = 3474(2) ų, Z = 4, and D _calc = 1.254 g cm^–3. 4: (+)- (S)-C₁₈H₂₄NO⁺, (-)-(2R,3R)-C₂₀H₁₇O^- ₈orthorhombic, P2₁2₁2₁, a = 7.504(1), b = 17.215(2), c = 26.490(4) Å, V = 3422.0(8) ų,Z = 4, and D _calc = 1.273 g cm^–3. The geometries and the conformational energies of the solid state conformations of the cations have been compared with global and local energy minimum conformations determined by molecular mechanics calculations. In the solid state, one conformation with and one without an intramolecular hydrogen bond are observed. The calculated global energy minimum conformation in aqueous solution contains the intramolecular hydrogen bond.     

X-ray crystallographic structure of the 9,10-dihydro-11,12bis[(1,3,3-trimethylureido)methyl]-9,10ethanoanthracene dihydrate

As a part of studies on MDR reversal agents, structure of the 9,10-dihydro-11,12-bis[(1,3,3-trimethylureido)methyl]-9,10-ethanoanthracene dihydrate is reported. Crystal data: C₂₆H₃₄N₄O₂ × 2 H₂O; mol. mass 470.60; monoclinic; space group: C2/c, a = 15.7492(6) Å; b = 7.2245(3) Å; c = 24.3442(10) Å; β = 106.795(2)^∘; V = 2651.73(22) ų; z = 4; dx = 1.179 mg/m³; μ = 0.64 mm⁻¹; F(000) = 1016; final R = 0.061 for 2501 reflections [I > 4 σ (I)]. Only half of the molecule is unique. The two nonplanar rings from the independent part of 9,10-dihydro-9,10-ethanoanthracene adopt a boat conformation. Crystallographic data demonstrate the “syn-syn” conformation of urea substituents in the molecule. In the crystal, water molecules are linked to the main species by H-bonds: O3′⋅sH12w—O1—H11w⋅sO3′(1.5 − x, 0.5 − y, 1 − z).     

α-substituted phosphoryl compounds (III). The crystal and molecular structure of diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide,C19H15OPS2

Diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell. The lattice parameters are a = 9.600 Å, b = 11.270 Å, c = 16.484 Å; β = 99.72°. With X-ray diffraction data collected at an automatic four circle diffractometer, the crystal structure has been solved by direct methods and refined to an R-value of 0.08 for 2690 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

Synthesis and crystal structures of complexes of Ni (II) to chiral Schiff bases of (R)- and (S)-serine with (S)- and (R)-2-N-(N′-benzylprolyl)-aminobenzophenone

The three-dimensional molecular and crystal structures of a pair of enantiopure mirror complexes of Ni (II) to chiral Schiff bases of (R)- and (S)-serine with (S)- and (R)-2-N-(N′-benzylprolyl)-aminobenzophenone (BPB), denoted as (S,R)-BPB-Ser-Ni and (R,S)-BPB-Ser-Ni, respectively, have been determined by X-ray diffraction. The complexes crystallize in the orthorhombic space group P2 ₁ 2 ₁ 2 ₁ with unit cell parameters: a = 10.050(2) Å, b = 10.100(2) Å, c = 26.514(5) Å, V = 2691.3(9) ų, and Z = 4 for (S,R)-BPB-Ser-Ni; and a = 9.878(2) Å, b = 10.130(2) Å, c = 26.304(5) Å, V = 2632.1(9) ų, and Z = 4 for (R,S)-BPB-Ser-Ni. The Ni atom is square-planar-coordinated to N(1), N(2), O(4), and N(3) of the Schiff base with minor distortion. The hydroxymethyl group on the serine moiety is axial to the coordination plane and parallel to the neighboring phenyl group.