Diphosphido bridged early/late heterobimetallic complexes: synthesis and molecular structure of Cp2Zr(μ-PPh2)2ReH(CO)3

1989 ◽  
Vol 67 (10) ◽  
pp. 1584-1589 ◽  
Author(s):  
Pei Yao Zheng ◽  
Douglas W. Stephan
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Metal Centre ◽  
Space Group ◽  
Heterobimetallic Complexes ◽  
Dative Bond ◽  
Crystallographic Study ◽  
Metal Metal ◽  
Early Late

The reaction of the metal–metal bonded complex Re2(CO)10 with Cp2Zr(PPh2)2 results in formation of the diphosphido bridged heterobimetallic species, Cp2Zr(μ-PPh2)2ReH(CO)3, 1. Complex 1 crystallizes in the space group P21/c with a = 17.393(3) Å, b = 14.348(7) Å, c = 13.036(3) Å, β = 92.35(2)°, Z = 4, and V = 3250(2) Å3. The crystallographic study confirmed that complex 1 contains two phosphido bridges between the Zr and Re centres. The Zr—P bond distances are 2.629(3) and 2.615(3) Å, while the Re—P bonds are 2.498(3) and 2.474(3) Å. The Zr—Re separation is 3.274(1) Å. The details of the geometry of the ZrP2Re core are discussed in relation to that of other diphosphido bridged early/late heterobimetallics. The possibility of dative bonding between the electron-rich, late metal and the electron-deficient early metal centre is discussed. The data indicate that if such dative bond is present in the d0–d6 complex 1, it is very weak. Keywords: rhenium, zirconium, heterobimetallic, crystal structure.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

The crystal structure of dibutyl-bis(pentamethylenedithiocarbamato)tin(IV)

1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Distorted Octahedron ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.

Synthesis and X -Ray Crystal Structure of the Heterobimetallic Complex [FeRh (μ-CO)(CO)3((μ-PBut2)((μ-Ph2PCH2PPh2)]

1997 ◽  
Vol 52 (7) ◽  
pp. 810-814 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Kurt Merzweiler ◽  
Clemens Bruhn
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Metal Carbonyl ◽  
Homogeneous Catalyst ◽  
Catalyst Precursor ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Heterobimetallic Complex

Abstract The reaction of the phosphido-bridged metal carbonyl [FeRh(CO)6(μ-PBut2)] (1) with dppm [dppm = bis(diphenylphosphino)methane] leads to the heterobimetallic complex [FeRh(μ-CO)(CO)3(μ-PBut2)(μ-dppm)] (2) in good yields. The molecular structure of 2 was determined at room temperature [triclinic, space group P1̄, a = 9.509(6), b = 13.637(5), c = 14.926(8) Å, α = 81.38(4), β = 82.75(4), γ = 71.25(4)°]. The compound acts as a homogeneous catalyst precursor in the hydroformylation reaction of ethylene, but it decomposes during this process.

Metalltetrahydridoborate und Tetrahydridometallate, 11 [1] Zur Kristall- und Molekülstruktur von Magnesiumtetrahydridoborat Mg(BH4)2 • 3 THF / Metal Tetrahydridoborates and Tetrahydridoborato Metallates, 11 [1] The Crystal and Molecular Structure of Magnesium Tetrahydridoborate Mg(BH4)2 • 3 THF

1982 ◽  
Vol 37 (12) ◽  
pp. 1499-1503 ◽  
Author(s):  
Heinrich Nöth
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Oxygen Atom ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Equatorial Position ◽  
Crystallographic Axis ◽  
Space Group ◽  
Distorted Trigonal Bipyramid ◽  
Double Hydrogen

Mg(BH4)2 • 3 THF was prepared from MgHo and B2H6 in tetrahydrofuran. It crystallizes monoclinically, space group C2/c, Z = 4. The crystal structure reveals that the molecule contains a seven-coordinate Mg center. Its BH4 groups form double hydrogen bridges to magnesium. The geometry at Mg corresponds to a slightly distorted trigonal bipyramid for the O 3 B 2 (Mg)-coordination polyhedron, with two THF molecules in apical and one in equatorial position. A two-fold crystallographic axis passes through Mg and the equatorial oxygen atom thus posing C2 symmetry on the molecule

The direct electrochemical synthesis of thiolato complexes of copper, silver, and gold; the molecular structure of [Cu(SC6H4CH3-o)(1,10-phenanthroline)]2•CH3CN

1987 ◽  
Vol 65 (6) ◽  
pp. 1336-1342 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
High Yield ◽  
Space Group ◽  
Anodic Copper

The electrochemical oxidation of anodic copper or silver (= M) into non-aqueous solutions of RSH (R = alkyl, axyl) gives MISR as insoluble materials in high yield. In the presence of 1,10-phenanthroline (= L), the products are MISR•phen for M = Cu, but not Ag. Gold resists oxidation under such conditions, and AuISR (R = n-C4H9, C6H5) was obtained in only poor yield. The crystal structure of the solvated dimeric adduct [Cu(SC6H4CH3-o)•phen]2•CH3CN is triclinic, with a = 10.682(3) Å, b = 11.729(4) Å, c = 15.608(5) Å, α = 76.87(2)°, β = 76.35(2)°, γ = 68.07(2)°, V = 1742(1) Å3, Z = 2 and space group [Formula: see text]. The structure is based on a folded Cu2S2 ring with an unusually short Cu—Cu distance of 2.613(3) Å Each copper atom has CuS2N2 pseudo-tetrahedral stereochemistry, with Cu—S = 2.337 Å(av) and Cu—N = 2.10 Å(av).

scholarly journals Crystal structure of 8-hydroxyquinoline: a new monoclinic polymorph

2014 ◽  
Vol 70 (9) ◽  
pp. o924-o925 ◽  
Author(s):  
Raúl Castañeda ◽  
Sofia A. Antal ◽  
Sergiu Draguta ◽  
Tatiana V. Timofeeva ◽  
Victor N. Khrustalev
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Three Dimensional ◽  
Solvent Mixture ◽  
Acta Cryst ◽  
Space Group ◽  
Compound C ◽  
Centrosymmetric Dimers

In an attempt to grow 8-hydroxyquinoline–acetaminophen co-crystals from equimolar amounts of conformers in a chloroform–ethanol solvent mixture at room temperature, the title compound, C9H7NO, was obtained. The molecule is planar, with the hydroxy H atom forming an intramolecular O—H...N hydrogen bond. In the crystal, molecules form centrosymmetric dimersviatwo O—H...N hydrogen bonds. Thus, the hydroxy H atoms are involved in bifurcated O—H...N hydrogen bonds, leading to the formation of a central planar four-membered N2H2ring. The dimers are bound by intermolecular π–π stacking [the shortest C...C distance is 3.2997 (17) Å] and C—H...π interactions into a three-dimensional framework. The crystal grown represents a new monoclinic polymorph in the space groupP21/n. The molecular structure of the present monoclinic polymorph is very similar to that of the orthorhombic polymorph (space groupFdd2) studied previously [Roychowdhuryet al.(1978).Acta Cryst.B34, 1047–1048; Banerjee & Saha (1986).Acta Cryst.C42, 1408–1411]. The structures of the two polymorphs are distinguished by the different geometries of the hydrogen-bonded dimers, which in the crystal of the orthorhombic polymorph possess twofold axis symmetry, with the central N2H2ring adopting a butterfly conformation.

Reaction of N,N′-dihydroxy-.N,N′-dimethylmethanediamine with phenylboronic acid and the crystal and molecular structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine

1989 ◽  
Vol 67 (11) ◽  
pp. 1959-1963 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Exact Formula ◽  
Full Matrix ◽  
Space Group ◽  
Hydrogen Bonded

The reaction of N,N′-dihydroxy-N,N′-dimethylmethanediamine with phenylboronic acid leads to the product 1,7-dimethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5-boratabicyclo[3.3.0]octane rather than the expected product 1,5-dimethyl-3-phenyl-1,5-diaza-2,4-dioxa-3-boracyclohexane. The structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine has been determined and is discussed in terms of its reaction with PhB(OH)2. Crystals of N,N′-dihydroxy-N,N′-dimethylmethanediamine are tetragonal, a = 8.5346(3), c = 8.4178(7) Å, Z = 4, space group P421c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.036 and Rw of 0.038 for 333 reflections with I ≥ 3σ(I). The structure consists of hydrogen-bonded dimers having exact [Formula: see text] symmetry. Keywords: N,N′-dihydroxy-N,N′-dimethylmethanediamine, crystal structure.

The Crystal Structure of the Tetrameric Adduct of Antimony Trichloride and Phosphoryl Isothiocyanate, [SbCl3·OP(NCS)3]4

1994 ◽  
Vol 49 (4) ◽  
pp. 441-444 ◽  
Author(s):  
Alexander V. Sienkiewicz ◽  
Anatoliy A. Kapshuk
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Antimony Trichloride ◽  
Cage Structure ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cubic System ◽  
Tetrameric Complex

The crystal and molecular structure of the tetrameric complex of the composition [SbCl3·OP(NCS)3]4 synthesized from SbCl3 and OP(NCS)3 in CCl4 waso determined by X-ray crystallography [143 m space group, cubic system with a = 13.927(4) Å]. The complex exhibits a tetranuclear "cage" structure with a [Sb4O4] core which consists of μ3-bridging oxygen and six coordinate antimony(III) atoms; the Sb-O distance, 3.060 Å, is exceptionally long.

Crystal and molecular structure of L-prolinatodiphenylboron

1977 ◽  
Vol 55 (6) ◽  
pp. 958-965 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Conformational Disorder ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of L-prolinatodiphenylboron are monoclinic, a = 5.9427(5), b = 14.4633(7), c = 8.9654(4) Å, β = 98.423(8)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.037 and Rw of 0.053 for 1477 reflections with I ≥ 3σ(I). The proline ring exhibits conformational disorder. The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.893(3) Å) along the short a axis. Intramolecular N—B coordination occurs to form a system of two fused five-membered rings. Bond lengths (corrected for libration) are: N—B, 1.630(3), O—B, 1.529(3), O—C, 1.219(3) and 1.300(3), N—C, 1.506(3) and 1.507(3), C(sp3)–C(sp3), 1.525(4), C(sp2)—C(sp3), 1.517(3), and mean C—C(phenyl), 1.394 Å.

Polysulfonylamine, CIII [1] Ein Hydroxylamin mit bemerkenswert kurzer O-N-B Bindung: Kristall- und Molekülstruktur von MeO-N(SO2Me)2 / Polysulfonylamines, C III [1] A Hydroxylamine with a Remarkably Short O-N Bond: Crystal and Molecular Structure of MeO-N(SO2Me)2

1998 ◽  
Vol 53 (5-6) ◽  
pp. 634-636 ◽  
Author(s):  
Martina Näveke ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Low Temperature ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles

Abstract The crystal structure of the known title compound was determined by low-temperature X-ray diffraction (orthorhombic, space group Pbcn, Z = 4). The molecule displays an unusually short O-N bond, a relatively long C-O bond and a moderately pyramidal O-NS2 skeleton (O-N 133.1, C-O 148.5 pm, sum of bond angles at N: 347.4°).

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