Crystal structure of tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate

The tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate salt is triclinic with the following cell parameters: a = 9.4283(3), b = 11.4482(3), c = 13.1748(3)Å, = 113.493(2), = 90.381(2), = 97.331(1)°, V = 1290.86(6)ų, with Z = 2 formula units. The structure consists of [C₆H₅NH₃]⁺ cations, water molecules, Cl^– anions, and SbCl₅ square pyramids. Hydrogen bonds, established through water molecule, link the anions [SbCl₅]^2– and Cl^– and make an infinite chain in the [011] direction. Chains are linked together via another hydrogen bond network originating from the ammonium groups. A distortion of the SbCl₅ square pyramid can be attributed to the stereo activity of the Sb(III) lone electron pair.     

Crystal and molecular structure of 6-0-acetylgrayanotoxin III

The crystal and molecular structure of a grayanotoxin III derivative, 6-0-acetylgrayanotoxin III is presented. The crystal is orthorhombic, space group P2₁2₁2₁, witha=15.582(3),b=21.304(3),c=6.339(3)Å,V=2104(1) ų Z=4. The structure was solved by direct methods and refined by full matrix least-squares methods to a finalR=0.047 for 1763 independent reflections withF ₀>3 (F ₀) The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered ring with various conformations.     

Crystal and molecular structure of tris(2-aminocyclopentene-1-dithiocarboxylato)-cobalt (III) monoacetone

The title compound crystallizes in the monoclinic space groupP2₁/c withZ=4 and cell dimensionsa=7.724(1),b=19.274(5),c=18.638(4) Å, and =105.68(2) °. Refinement with 1126 terms, measured with MoK radiation on a diffractometer, has yielded a conventionalR factor of 0.059. The non-hydrogen atoms in the complex molecule were refined with anisotropic temperature factors whereas those in the acetone molecule were refined isotropically. The nitrogen atoms in the complex are not coordinated; the coordination sphere involves Co—S₆ bonding of approximateD ₃ symmetry, the average Co—S bond length being 2.275 Å. The geometry of the coordination sphere with respect to a definedC ₃ reference axis is similar to that found in several tris(N,N-disubstituted-dithiocarbamato)cobalt(III) complexes. The acetone molecule is hydrogen bonded to one of the amino groups, the O N distance being 2.99 Å.     

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.     

Crystal and molecular structure of iso-grayanotoxin II

The crystal and molecular structure of a grayanotoxin derivative, iso-grayanotoxin II, is presented. The crystal is orthorhombic, space group . The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered rings with various conformations.     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

Crystal and molecular structure of augustamine

The crystal and molecular structure of augustamine (1), C₁₇H₁₉NO₄ an amaryllidaceae alkaloid of the tazettine group has been determined by direct methods from single crystal x-ray diffractometer data and refined by full-matrix least squares. The alkaloid (1) crystallizes in the space group P2₁2₁2₁, with cell parameters: a = 7.833(8) b = 11.08(2) å, c = 16.69(6) Å, Z = 4, D_c = 1.381 g/cm^–3, R = 7.6% for 1115 observed reflections. The molecule, having a hexacyclic ring system, is very rigid with the ring B in a chair conformation. Molecular mechanics calculations have been made using MM3(2000) force field.     

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.     

Crystal structure of tetrakisdiphenylammonium hexadecachlorotetrabismuthate(III)

[(C₆H₅)₂NH₂]₄ ⁺[Bi₄Cl₁₆]^4– crystallizes in the triclinic space group witha=11.835(2),b=12.393(2),c=12.625(3)Å, =108.37(3), =108.69(3), =96.00(3)° andD _c=2.135 g cm^–3 forZ=1. The [Bi₄Cl₁₆]^4– anion is a centrosymmetric cluster of four distorted edge-sharing BiCl₆ octahedra. The ranges of the Bi–Cl bonds are 2.484(4)–2.606(3)Å for Bi–Cl(terminal), 2.691(3)–2.956(4)Å for Bi-Cl(µ₂), and 2.960(3)–3.120(4)Å for Bi-Cl(µ₃). The cations and anions are held in place by weak hydrogen bonds.     

Crystal structure of the molecular adduct of 5-mono[(4-nitrophenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene with chloroform (1:1)

The crystal structure of the molecular adduct of 5-mono[(4-nitrophenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene (2) with chloroform (C₃₄H₂₇N₃O₆ CHCl₃) was determined by X-ray crystallographic analysis. It was found to possess a monoclinic space group P2(1)/n, with a = 15.9306(13) Å, b = 10.6293(9) Å, c = 20.3194(17) Å, = 110.480(2)° and D_calc = 1.428 Mg/m³ for _Z = 4. Crystal data indicated that the calix[4]arene moiety of 2 exists in a distorted-cone conformation with intramolecular hydrogen bonds.     

Crystal structure of penthylenediammonium pentachlorothallate(III)

The penthylenediammonium pentachlorothallate(III) salt is orthorhombic with the following unit cell dimensions: a = 7.696(3) Å, b = 13.2890(17) Å, and c = 13.503(18) Å, space group P2₁2₁2₁ with Z = 4. The structure was solved by Patterson methods and refined to a final R value of 0.0387 for 1991 observed reflections. The structure consists of penthylenediammonium cations and polynuclear anions in which slightly distorted [TlCl₆]^3– octahedral sharing two vertices are interconnected into chains. These chains are themselves interconnected by means of the N–HCl bonds originating from the [NH₃(CH₂)₅NH₃]²⁺ entities forming a three-dimensional network.     

Crystal and molecular structure of tris-(O-isopropylxanthato)-chromium(III)

The title compound has been synthesized by the reaction of CrCl₃6H₂O with K{S₂COCH(CH₃)₂} in a 13 molar ratio in an aqueous medium. It has been characterized by elemental analysis and IR spectral studies. Crystals of Cr{S₂COCH(CH₃)₂}₃ are monoclinic, space group P2₁/n witha=10.002(2),b=10.973(1),c=18.961(6) Å,=91.78(2)°,V=2079.9 ų,Z=4,D _calc=1.46 g cm^–3, monochromatic radiation (Mo-K), =0.71069 Å,=11.2 cm^–1,F(0 0 0)=948,T=295K, finalR=0.0320 for 2641 reflections. The environment of the chromium atom is based on an octahedral geometry having six sulfur donor atoms from three symmetrically chelated ligands with average distances: Cr-S=2.396(9) Å, C-S=1.690(3) Å and C-O=1.315(3) Å. The bond distance between oxygen atom and the carbon atom of the isopropyl group (O-C_av=1.478(4) Å) suggests that the form –S ₂ ^(–) C=O⁽⁺⁾CH(CH₃)₂ contributes significantly to the structure of the isopropyl group.     

Crystal and molecular structure of hydridodinitratobis(triphenylphosphine)iridium(III)

Crystals of hydridodinitratobis(triphenylphosphine) iridium(III), IrH(NO₃)2(PPh₃)₂, belong to the trigonal system, space groupP¯3e1, with hexagonal unit-cell dimensionsa = 16.33(1),c = 22.85(2) Å, andZ = 6. The six Ir atoms lie in special positions. Two (of molecule 1) have site symmetry 32 and four (of molecule 2) have site symmetry 3. Both types of molecule have trigonal bipyramidal coordination with phosphorus atoms axial but do not have sufficient nitrate groups (two instead of three) to satisfy the site symmetry. Thus both types of molecule have disordered nitrate groups and the mode of coordination appears to be somewhat different at the two sites.     

Crystal and molecular structure of tetra-n-butylammoniumbis(stilbenedithiolato)-nickelate(III)

The crystal and molecular structure of the title compound, C₄₄H₅₆NS₄Ni, are reported. Crystals are triclinic, space groupP¯1 (No. 2) withZ=2 in a unit cell of dimensionsa=8.874(2) Å,b=9.549(5) Å,c=26.025(7) Å,=97.22(3)°,=95.06(2)°, and=98.75(3)°. The structure was solved by Patterson and Fourier methods and refined by full-matrix least squares toR=0.062 for 2910 unique diffractometer data. The metal atom of the anion has an approximate square-planar configuration and the nitrogen atom of the cation an approximate tetrahedral configuration. The anions as well as the cations are well separated, the closest NiNi and NN approaches being the lattice repeat of 8.874(2) Å.     

Crystal structure of tris(methylcyclopentadienyl) tetrahydrofuranatosamarium

The first crystal structure of tris(methylcyclopentadienyl) tetrahydrofuranato (THF) lanthanide complexes, (CH₃Cp)₃Sm · THF, is determined. The complex crystallizes from mixed solvents of tetrahydrofuran and hexane as a monomer in the orthorhombic space group Pc2₁n with the unit cell parameters a = 9.135(2) Å, b = 13.263(2) Å, c = 16.176(3) Å, and Z = 4.     

Crystal and molecular structure of tris (2,2,6,6-tetramethyl-3,5-heptanedionato) aquodysprosium(III), Dy(thd)3H2O

The crystal structure of Dy(thd)₃H₂O has been solved by three-dimensional X-ray methods at room temperature. The space group isP¯1 and the cell dimensions area = 14·21(1),b = 14·88(2),c = 11·60(2) Å, = 99·76(3), = 109·91(1), = 114·08(1) °.Z = 2,D _m = l·24 andD _x = 1·238 gcm^–3, respectively. Full-matrix least-squares refinement of atomic and individual isotropic thermal parameters, using 3015 intensities obtained by counter methods, terminated with a conventionalR of 0·058. The oxygen polyhedron around dysprosium has pure seven-coordination geometry, the seventh ligand being the water molecule. The water is hydrogen bonded to two oxygen atoms of a centre of symmetry related formula unit so that two formula units are in fact held together by hydrogen bonds in a dimer.Supported by National Institute for Metallurgy, Johannesburg.     

Crystal and molecular structure studies of tris(2-hydroxy-3-t-butyl-5-methylbenzene)-methane trihydrate and N-benzyl-N-phenyl benzamide

The structures of the title compounds, tris(2-hydroxy-3-t-butyl-5-methylbenzene)-methane)C₃₄H₄₆O₃.3H₂O, 3) and N-benzyl-N-phenylbenzamide (C₂₀H₁₇NO, 6), have been investigated by X-ray crystallography. Compound 3 crystallizes in the trigonal space group with cell parameters a = 14.090(5) Å, b = 14.090(5)Å, c = 10.485(5)Å, Z = 2. Compound 6 crystallizes in the monoclinic space group C2/c with cell parameters a = 24.533(4)Å, b = 9.176(4)Å, c = 16.711(5)Å, = 125.88(2)°, Z = 8. Compound 3 has both intra-and intermolecular hydrogen bonds. It also exhibits a helical columnar arrangement of the molecules and goes into mesophase before melting into an isotropic liquid.     

Crystal and molecular structure of bis(tropolonato)-dioxo-(ethanol)uranium(vi)

Crystals of bis(tropolonato)-dioxo(ethanol)uranium(VI) are orthorhombic:a = 12·495(8),b = 8·817(7),c = 15·459(9) Å,Z = 4, space groupPnam. The structure was determined with MoK diffractometer data by standard Patterson and Fourier methods, and was refined by full-matrix least-squares methods toR = 0·049 for 1289 observed reflexions.The coordination plane consists of the four tropolonato oxygen atoms and the oxygen from the ethanol ligand; the uranyl group is perpendicular to it. The molecule lies across the mirror plane, consistent with a boat conformation for the tropolone rings; the dihedral angle between the plane of tropolone ring and the coordination plane is 22·5 °. The deviations of the tropolonato oxygen atoms from the tropolonato plane are 0·08 Å (above) and 0·16 Å (below). It is almost certain that the ethyl group of the ethanol ligand does not lie in the symmetry plane; C(8) is about 0·3 Å on one side of this plane and C(9) is about the same distance on the other, within a satisfactory bonding scheme.     

Synthesis, spectroscopic studies, and crystal structure of tris(tetra-n-butylammonium) hexakisisothiocyanatoindate(III)

The reaction of a 1:10 molar ratio between indium chloride and tetra-n-butylammonium thiocyanate in ethanol affords the complex [(n-C₄H₉)₄N]₃[In(NCS)₆] (1), the structure of which has been established by X-ray diffraction. This compound crystallizes in the cubic space group Pa3¯ with eight formula units in the unit cell. The formula unit consists of three separate cationic tetra-n-butylammonium groups and an independent hexakisisothiocyanatoindium anionic group. The six near linear thiocyanate ligands coordinate octahedrally through the nitrogen atom to the indium metal center. The coordination of the n-butyl groups to the ammonium-nitrogen atom is tetrahedral. The complex has also been characterized by IR, ¹H and ¹³C NMR, physical properties, and X-ray powder analysis.