Crystal structure of Zn[Cl2Ti(C5H5)2]2·2C6H6

The structure of crystals of the composition Zn[Cl₂Ti(C₅H₅)₂]₂·2C₆H₆ has been determined from Patterson and Fourier syntheses of two projections, and refined toR = 0·117 by full-matrix three-dimensional least-squares methods. The crystals are orthorhombic:Pbcn,a = 18·45(5),b = 15·40(6),c = 11·35(3) Å,Z= 4. The complex consists of a central distorted ZnCl ₄ ^2– tetrahedron linked along the Cl—Cl edges to two distorted TiCl₂(C₅H₅)₂ ⁺ tetrahedra in such a way that their centres are nearly collinear The two C₆H₆ molecules in the formulae unit may be regarded as benzene of crystallization.     

Crystal structure of dinitratotris(pyridine)nickel(II), Ni(NC5H5)3(NO3)2

Ni(NC₅H₅)₃(NO₃)₂ crystallizes in the triclinic space group P¯1 witha=8.432(2),b=9.993(2),c=12.181(3)Å, =69.78(2),=83.16(2), =67.73(1), andD _c =1.57 g cm^–3 forZ=2. The Ni²⁺ ion is six-coordinate with one bidentate and one monodentate nitrato ligand.     

Crystal and molecular structure of di(μ 3-oxo-tri-μ-oxotrichlorohexakis(pyridine)-triangulotritungsten(IV))hexatungstate(VI)-6-pyridine, [W3(O)O3Cl3(C5H5N)6]2W6O19·6C5H5N

[W₃(O)O₃Cl₃(C₅H₅N)₆]₂W₆O₁₉·6C₅H₅N, the side product of the reaction between WCl₄(C₅H₅N)₂ and pyridine, crystallizes in the rhombohedral space groupR¯3 (No. 148), witha=14.044(1) Å,=87.70(1)°, andZ=1. The structure was solved by the heavy-atom method, and refined to the unweighted and weighted residuals of 0.068 and 0.055, respectively. The tungsten atoms define an equilateral triangle with a capping and three bridging oxygen atoms. Two pyridines in thecis position and a chlorine atom form, together with the oxygens, a distorted octahedron around the tungsten atoms; three octahedra are connected through common edges. Important bond lengths are: W-W (single bond) 2.532(1), W-O (tricapped) 2.09(1), W-O (bridging) 1.92(1) and 1.94(1), W-C1 2.424(5), and W-N (pyridine) 2.23(1) and 2.26(1) Å. In W₆O ₁₉ ^2– , six WO₆ octahedra have one common central oxygen, twelve bridging and six terminal oxygen atoms. Corresponding W-O bond lengths are: 2.323(1) (central oxygen), from 1.90 to 1.94(1) (bridging oxygens), and 1.70(2) Å (terminal oxygens). Lattice pyridine molecules have no important contacts with either anion or cation.     

Crystal and molecular structure of (2–3-η-2-Butyne-1,4-diol)-bis-(triphenylphosphan)-nickel(O) Ni{[(C6H5)3P]2 (C4H6O2)}

The crystal and molecular structure of (2–3-η-2-Butyne-1,4-diol)-bis-(triphenylphosphan)-nickel(O) has been determined by X-ray structure analysis. It crystallizes in the tetragonal space group 14 with the cell parameters a = b = 22.277(3), and c = 15.118 (4) Å. The structure was solved by the heavy atom method and refined to R = 0.0716. The coordination geometry about the nickel atom is trigonal-planar. Each molecule is hydrogen bonded to two neighbours. The result is an eight-membered oxygen ring.     

X-ray and neutron diffraction studies of the hydridotriruthenium cluster complex (μ-H)Ru3(CO)7(μ-As(C6H5)CH2As(C6H5)2) ((C6H5 2AsCH2As(C6H5)·CH2Cl2: an example of dibridged metal-metal bond M(μ-H)(μ-X)M,involving a heavy bridgehead atom

The title compound is (μ-H)Ru₃(CO)₇(μ-As(C₆H₅)CH₂As(C₆H₅)₂)((C₆H₅)₂ AsCH₂As(C₆H₅)₂)·CH₂C1₂. Crystal data: monoclinic,P2₁/n, cell parameters (X-ray)a=12.82(2) Å,b=22.91(2) Å,c=17.83(2) Å, β=99.1(3)°; (neutron)a=12.94(1) Å, β=22.95(2)Å,c=17.93(3)Å,β=99.55(5)°. The structure was solved from X-ray data. FinalR indices areR(F)=0.051,R _w (F)=0.049 (X-ray);R(F)=0.064,R _w (F)=0.048,R(F ²)=0.072,R _w (F²)=0.088 (neutron). The complex is derived from Ru₃(CO)₈(dpam)₂ through reaction with hydrogen. The structure consists of a triangular array of metal atoms involving three metal-metal bonds[Ru(1)?Ru(2)=2.912(7)Å;Ru(1)?Ru(3)=2.829(3) A; Ru(2)?Ru(3)=2.845(6) Å]. The metal-metal edge Ru(1)?Ru(2) is supported by a bridging bis(diphenylarsino)methane ligand which lies in the equatorial plane. Activation of the second dpam ligand has generated the new face-bridging ligand unit μ-As(C₆H₅)CH₂As(C₆H₅)₂. In this unit, the bridgehead As atom spans over the Ru(1)?Ru(2) bond, while the second As atom is only bonded to Ru(3). The metal environment is achieved by CO ligands. The hydride ligand is bridging the Ru(1)?Ru(2) vector [Ru(1)?H=1.791(10) Å; Ru(2)?H=1.818(8) Å]. Geometric features of the dibridged Ru(μ-H)(μ-As)Ru bond are discussed.     

Syntheses,Characterizations and Crystal Structures of Two New Racemic Amidophosphoesters: rac-(C6H5O)(cyclo-C6H11NH)P(O)N(C4H8)NP(O)(NH-cyclo-C6H11)(OC6H5) and rac-(p-CH3-C6H4NH)P(O)(OC6H4-p-CH3)(OC6H5)

Crystallography Reports - The new racemic compounds, rac-diphenyl bis(cyclo-hexylamido)(piperazine)-1,4-diyldiphosphinate, C28H42N4O4P2 (I), and...     

Crystal structure of mixed-ligand copper(II) complexes. Bis(2,2′-bipyridyl)monophenylphos-phatocopper(II)monophenylphosphate monohydrate, [Cu(C10H8N2)2(C6H5OPO3)]-(C6H5OPO3H2)(H2O)

The title mixed-ligand copper(II) complex has been synthesized and its crystal structure at room temperature solved. The crystals are monoclinic:P2₁/c,a=12.004(3),b=19.402(5),c=14.192(4) Å,=108.80(3)°,Z=4. The structure was solved by direct methods, and refined to anR value of 0.041 for 4457 nonzero independent reflections. The crystal structure consists of discrete [Cu(bipy) (MPhP)] units, noncoordinated MPhPH₂, and H₂O molecules. Each [Cu(bipy)₂(MPhP)] unit involves a five coordinate CuN₄O chromophore with a distorted trigonal-bipyramidal stereochemistry. The phosphate groups are linked together by short hydrogen bonds of (P)-O-H--O-P type.     

Crystal structure of the orange isomer of [(C6H5)3P]2[C2S2(CF3)2]RuCO

The structure of the title compound has been determined by X-ray analysis. It is monoclinic:a = 10.147,b = 10.081,c = 38.627 Å, β = 102.27 °,Z = 4,P2₁/c. The structure was solved by standard methods and refined by least squares to a (conventional)R-factor of 4.7%. The Ru atom is in square-pyramidal configuration: the Ru-S distances (2.286, 2.336Å) are significantly different, but the Ru-P distances average to 2.389 Å. Comparisons are made with the violet isomer.     

Partial X-ray analysis of triiodo-heptakis (triphenylphosphine)undecagold,Au11C126H105I3P7

Journal of Chemical Crystallography -     

Crystal and molecular structure of diaqua-bis-(3,5-dimethyl-1-guanyl pyrazole) nickel (II) nitrate, [Ni(C6N4H10)2(H2O)2](N03)2

The title compound crystallizes in space groupP2₁/n witha=10.651(3),b=11.082(2),c=8.993(3) Å,=106.79(3)°;R=0.064 andR _w=0.074 for 3399 observed reflections (I3(I)) from 3674 measured. The structure was solved by direct methods and refined by least squares. The Ni atom of the complex is located at a center of inversion, and is surrounded by four nitrogen atoms of the two ligands in square-planar geometry. The oxygen atoms of the two centrosymmetrically related water molecules complete the coordination around the metal ion to form an elongated octahedron.     

On the organoaluminum chemistry of multidentate phosphine ligands. Reaction of trimethylaluminum with bis(diphenylphosphino)methane: Synthesis and molecular structure of [Al(CH3)3]2[(C6H5)2PCH2P(C6H5)2]

Reaction of an excess of trimethylaluminum with bis(diphenylphosphino)-methane in heptane affords the crystalline complex [A1(CH₃)₃]₂[(C₆H₅)₂PCH₂P(C₆H₅)₂]. The title compound crystallizes in the triclinic space group P¯1 with unit cell parametersa=10.053(6),b=11.017(6),c=15.908(8) Å,=85.58(4),=71.80(4), =77.49(4)°,V=1634(1) ų, andD _c=1.07 g cm^–3 forZ=2. Least-squares refinement based on 2924 observed reflection with intensitiesI3I) in the range 2.00245.0° converged atR=0.050 (R _w=0.067). The Al-P distances are 2.585(2) and 2.521(2) Å, and the P-C-P angle is 121.4(2)°.     

Crystal and molecular structure of 2,2′-bipyridyl-(μ3-1-keto-2,3,4-triphenylcyclobutenyl) dicarbonylbromomolybdenum(1)benzene [(C6H5)3C3CO](C10H8N2)(CO)2MoBr·C6H6

The crystal structure of [(C₆H₅)₃C₃CO](C₁₀H₈N₂)(CO)₂MoBr·C₆H₆ has been determined. The complex crystallizes in the triclinic space groupP ¯1 witha=8.52(1),b=19.42(3),c=10.54(1) Å, =97.4(1), =74.6(1), and =87.5(1)°. There are two formula units per cell. A total of 2924 unique observed reflections was collected photographically using CuK radiation. The structure was refined toR=0.072. The molybdenum atom in this compound can be considered as situated at the center of a very distorted octahedron. The six coordination sites about the metal atom are occupied by two carbonyl groups which share with the bipyridyl the four equatorial positions. The bromine and a -bonded keto-triphenylcyclobutenyl ring take up the two axial positions. There is an ³ interaction between the cyclobutenyl ring and the molybdenum atom. The detailed geometry of the 1-keto-2,3,4-triphenylcyclobutenyl ligand is similar to that found by Coffey (1962) in a cobalt complex. In the present compound the cyclobutenyl ring is slightly puckered with a dihedral angle of 11.05° between the plane which contains the allylic carbon atoms and that containing the ketonic group. Two solvating benzene molecules are centered at the inversion sites in the unit cell.     

X-ray analysis of octakis(tri-p-tolylphosphine) enneagoldtris(hexafluorophosphate), [Au9{P(p-MeC6H4)3}8](PF6)3: A redetermination

Journal of Chemical Crystallography - A redetermination of the crystal structure of the gold cluster [Au9{P(p-MeC6H4)3}8](PF6)3 has been performed. The compound crystallizes in the tetragonal space...