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 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 structure of chloritopentamminecobalt(III) tetracyanopalladate(II)

The X-ray crystal structure of [(NH₃)₅Co(ClO₂)][Pd(CN)₄]·H₂O consists of two discrete complex ions and a water of hydration. The red crystals are triclinic, P , with lattice parameters a = 7.1992(5), b = 9.4873(7), c = 11.7752(8) Å. = 66.680(1), = 75.784(1), = 82.203(1)°, and Z = 2 giving a cell volume of 715.27(9) ų and a calculated density of 2.043 g/cm³ at 293°. The chlorite ion is O-bonded to the cobalt atom with amine N—Co distances all equal. The chlorite ion is bent with a O—Cl—O angle of 110.8(2)° and the Cl—O distances being 1.601(3) and 1.558(3) Å, the longer value for the O atom also coordinated to Co. The Pd(CN)^–2 ₄ ions are planar, C-coordinated and stack along the x-axis, separated by 3.599(1) Å and alternatively rotated by 29.9(5)°.     

Crystal structure of 1,2,4,6-tetraphenylpyridinium tetrabromoferrate(III)

The title structure, which belongs to the triclinicP¯1 space group witha=13.901(4),b=10.732(1),c=10.570(8)Å=109.14(4),=96.17(4), =90.34(2)°, is refined toR=0.052 for 2985I3(I) reflections. The structure consists of a non-interacting 1,2,4,6-tetraphenylpyridinium and tetrahedral tetrabromoferrate (III) ions.     

Crystal structure of lanthanum(III) oxalate decahydrate

La₂(C₂O₄)₃·10H₂O crystallizes in space groupP2¹/c (No. 14) witha=11.382(6),b=9.624(5),c=10.502(8) Å,=114.52(4)°, andZ=2. The structure (R=0.029 for 3190 MoK data) is composed of two-dimensional networks of edge-sharing 153 coordination polyhedra matching the (020) set of planes, each La(III) atom being surrounded by three ⁴ chelating oxalate groups and three aqua ligands with La-O distances in the range 2.518(4)–2.622(4) Å. The remaining water molecules are disordered over seven principal sites in the intervening space.     

Crystal structure determination of (triethyleneglycol)bis(3,5-dinitrobenzoate) strontium(II) monohydrate

The complex {[Sr(C₇H₃N₂O₆)₂(C₆H₁₄O₄)]·H₂O}₂ is a centrosymmetric dimer. Each Sr^{2 +} in the cluster is nine coordinated by four oxygens of triethyleneglycol and the carboxylate oxygens of 3,5-dinitrobenzoate (DNB) anions. One of the DNBs behaves as a symmetrical bidentate chelating ligand whereas the other acts as a highly unsymmetrical, tridentate, chelating-cum-bridging ligand. The crystal is triclinic with a space group P1. The unit cell dimensions are a = 14.955(2), b = 12.730(2), c = 7.389(2) Å, = 73.06(1)°, = 99.56(1)°, = 80.02(2)° , V = 1289.84 ų, = 0.71070 Å, Z = 2. The centrosymmetrically related Sr^{2 +} is separated by a short distance of 4.565(1) Å, which results in a closely packed cluster of monomers. Both the alcoholic oxygens are H-bond donors toward the carboxylate oxygens of one of the DNB anion. The water molecule occupies intermolecular spaces.     

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 structure of dicalcium potassium trihydrogen bis(pyrophosphate) trihydrate

The crystal structure of Ca₂KH₃(P₂O₇)₂·3H₂O has been determined by single crystal X-ray diffraction. Crystals are monoclinic, space groupP2₁/n witha=10.518(3),b=19.253(9),c=7.340(3)Å,=90.07(2)°, andZ=4. The structure was refined toR=0.048 andR _w=0.044 for 1839 reflections withI3(I). The structure consists of a compact assembly of Ca, K, HP₂O₇, and H₂P₂O₇ ions and three water molecules arranged in layers perpendicular to theb-axis. The two independent Ca ions and the HP₂O₇ ion comprise one layer; K and H₂P₂O₇ ions and the three water molecules form an interstitial layer. Coordinations of the two independent Ca ions are quite similar, but the environments of HP₂O₇ and H₂P₂O₇ ions are quite different, probably due to their locations in different layers. The general structural features are quite similar to those of Ca(NH₄)HP₂O₇.Certain commercial materials and equipments are identified in this paper to specify the experimental procedure. In no instance does such identification imply recommendation or endorsement by the National Institute of Standards and Technology or the ADA Health Foundation or that the material or equipment identified is necessarily the best available for the purpose.     

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 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 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 di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate

The salt di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate crystallizes in the orthorhombic system with space group Cmc2₁, the unit cell dimensions are: a = 29.383(1), b = 10.509(2), c = 9.941(1) Å, with Z = 8. The structure shows a layer arrangement perpendicular to the a axis: planes of SbCl₆ octahedra alternate with planes of [C₁₂H₁₇N]⁺ cations. The SbCl₆ octahedra are connected through a O(W)–HCl hydrogen bonds and a chlorine bridge, so that infinite unidimensional chains of composition [SbCl₅(H₂O)₂]^2n– _n are formed in the structure along the c direction. These chains are connected to [C₁₂H₁₇N]⁺ entities by N–HCl and N–HO(W) hydrogen bonds, forming a three-dimensional network. It was found that lengths of Sb–Cl bonds may differ from each other. The differences shown as a distortion of the SbCl₆ octahedra were attributed to the Sb(III) lone electron pair stereoactivity.     

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.     

Fluoro-containing complexes of chromium (III). II. Crystal structure oftrans-difluorodiaquo-ethylenediaminechromium(III) chloride

The results of an X-ray structure determination of one of the three possible chloride salts of [Cr(en) F₂(OH₂)₂]⁺ show the two fluoro ligands to betrans to each other. The purple crystals are monoclinic in the space groupC2/c-C _2h ⁶ , witha=11.409(3),b=9.319(2),c=10.260(3) Å,β=128.73(2)° andD _c =1.73 g cm^?3 forZ=4. Least-squares refinement based on 1341 independent observed reflections resulted in a finalR of 0.026. The molecule lies on a crystallographic two-fold axis, and the Cr-F, Cr-N, and Cr-O bond lengths are 1.885(1), 2.044(2), and 1.997(2) Å respectively. It is suggested that the ill-defined shoulder in the visible electronic spectrum of this complex is indicative of atrans dihalo geometry.     

Crystal structure of bis[dihydrobis(3,5-dimethy-1-pyrazolyl)borato]cadmium(II)

The structure of [H₂B(3,5-Me₂pz)₂]₂Cd shows the four nitrogen donor atoms form a pseudotetrahedral arrangement about the cadmium(II). The intraligand N—Cd—N angles are restricted to an average of 91.4° by the chelate rings forcing the interligand N—Cd—N bond angles to average 119.4°. The Cd—N bond distances average 2.21 Å with a range of 0.04 Å. The crystal is in the triclinic space group, P with a = 7.6793(2) Å, b = 8.5992(2) Å, c = 25.0874(4) Å, = 91.0791(2)°, = 97.9769(4)°, = 110.2344(6)°, and Z = 2.     

Crystal and molecular structure of 2,6-di (o-chloro)phenyl-3,5-dimethyl-N-nitrosopiperidin-4-one(NOCDMPO)

The title compound (C₁₉H₁₈O₂N₂Cl₂) crystallized in the monoclinic space groupP2₁/n witha=13.062(2),b=10.931(2),c=13.120(2)Å, and=104.57(1)°. The structure was solved by direct methods and refined toR=0.047 for 2776 reflections. The piperidine ring assumes a distorted boat conformation. The angle between phenyl rings is 78.98(7)°. The nitroso group is oriented by 138.22(7)° to the best plane of the piperidine ring. The interaction between the molecules are van der Waals in nature.DCB Contribution No. 814.     

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 bis(N,N-di-n-butyldithiocarbamato)copper(III) triiodide

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)-copper (III) triiodide, Cu(S₂CN(C₄H₉)₂)₂ ⁺I₃ ^–, has been determined from a single-crystal X-ray diffraction study. The monoclinic unit cell, space groupP2₁/c,a = 14·026(6),b = 8·62(1),c = 25·015(9) Å, = 95·35(5) °, contains four formulaentities. Three-dimensional intensity data were obtained from Weissenberg photographs. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·083 for 950 independent non-zero reflexions. The structure contains two symmetry-independent cations. In both cations, the copper atom is in planar coordination with four sulphur atoms, the mean Cu(III)-S bond length being 2·22(2) Å. Cu(III)-S distances are about 0·08 Å less than Cu(II)-S distances in comparable complexes.