The crystal and molecular stucture of μ-Bis(diphenylarsino)methanehexacarbonyldi-μ-chloro-dirhenium(I)-n-hexane (4/1)

1975 ◽  
Vol 28 (6) ◽  
pp. 1201 ◽  
Author(s):  
CJ Commons ◽  
BF Hoskins
Keyword(s):  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Rhenium Complex ◽  
Metal Atoms ◽  
A Site

The crystal and molecular structure of the n-hexane solvate of μ- bis(diphenylarsino)methane-hexacarbonyldi-μ-chloro-dirhenium(I), Re2(CO)6(Ph2AsCH2AsPh2)Cl2, has been determined by three-dimensional X-ray diffraction methods. The complex crystallizes in the space group Pī with a 15.763(1), b 19.077(1), c 12.233(1) Ǻ and α 88.745(10), β 110.506(5), γ 92.900(6)�. The structure was solved by conventional Patterson and Fourier methods and refined by a block-diagonal least- squares method to R and Rw of 0.045 and 0.054, respectively, for 7061 independent statistically significant reflections collected by counter methods. The crystal consists of discrete molecules of the complex and n-hexane held together by van der Waals forces. There are two molecules of the dirhenium complex in the crystallographic asymmetric unit with the n-hexane molecule situated about a site of symmetry ī. The binuclear rhenium complex contains bridging halogen atoms and a bridging diarsine ligand. Three carbonyl ligands are also bonded to each rhenium atom, giving the metal atoms approximately octahedral environments. The average Re-As, Re-Cl, and Re-C bond lengths are 2.58, 2.52, and 1.89 Ǻ respectively.

Studies of the rhenium-oxygen bond. III. The crystal and molecular structure of 1-oxo-6-ethoxo-2,4-dichloro-3,5-dipyridinerhenium(V)

1977 ◽  
Vol 55 (2) ◽  
pp. 333-339 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Dominant Factor ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Bond

The crystal and molecular structure of the title compound has been examined by single crystal X-ray diffraction. The crystals are monoclinic with a = 28.045(10), b = 8.766(3), c = 12.376(5) Å, β = 91.14(3)°. The space group is C2/c and there are eight molecules per unit cell. A total of 5053 independent reflections, of which 2860 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares to an R2 value of 0.0449. The ligands form a very rough octahedron around the rhenium atom with Re—Cl(1), 2.441(3); Re—Cl(2), 2.366(3), Re—O(1), 1.684(7); Re—O(2), 1.896(6); Re—N(1), 2.144(7); Re—N(2), 2.132(7) Å. The pyridine rings are a dominant factor in determining the details of the molecular structure.

Crystal and Molecular Structure of 3-Iodo-2-propynyl-N-butylcarbamate

1997 ◽  
Vol 52 (2) ◽  
pp. 256-258 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Rainer Grüning ◽  
Jörg Lorberth
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Carbamate Group ◽  
Oxygen Atoms

Abstract The crystal structure of the title compound has been determined by X-ray diffraction methods. Due to the Lewis acidic character of the iodine substituent a “zig-zag” chain is formed via intermolecular interactions (2.933(4) A) between iodine and oxygen atoms of theocarbamate moiety. A three-dimensional network is formed through hydrogen-bridging (2.04 A) between NH-groups and the oxygen atoms of the neighbouring carbamate group of the next molecule.

The crystal structure of a dithiophosphate-bridged binuclear cobalt(II) complex of a macrocyclic ligand

1981 ◽  
Vol 34 (1) ◽  
pp. 65 ◽  
Author(s):  
GA Williams ◽  
R Robson
Keyword(s):  
Crystal And Molecular Structure ◽  
Macrocyclic Ligand ◽  
Cobalt Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Axial Ligands ◽  
Octahedral Environment ◽  
Metal Atoms ◽  
A Cell

The crystal and molecular structure of LCO2 [S2P(OEt)2]2 (where L is a binucleating ligand derived from the macrocycle LH2 formed by condensation of two molecules each of propane-1,3-diamine and 2-hydroxy-5-methylisophthalaldehyde) has been determined by single-crystal X-ray diffraction techniques at 295 K. The compound crystallizes in the triclinic space group Pī with two molecules in a cell of dimensions a 18.644(6), b 11.694(4), c 9.487(4) �, α 84.99(3), β 82.61(3), γ 73.48(2)�. Automatic diffractometry has provided significant Bragg intensities for 2799 independent reflections and the structure has been refined by least-squares methods to R 0.054. The structure is molecular, consisting of discrete binuclear units LCo2[S2P(OEt)2]2. The two centrosymmetric molecules in the unit cell are crystallographically unique but essentially chemically similar. The two cobalt(11) atoms in each molecule are separated by 3.075(2) and 3.072(2) �. Each cobalt atom is in an octahedral environment, with an N2O2 equatorial plane and two sulfur atoms of bridging dithiophosphate ligands in the axial positions. The Co-S bonds are the longest yet observed [2,680(3), 2.652(3), 2.642(3), 2.623(3) �]. The cobalt(11) centres are high spin, with �eff 4.53 BM per cobalt atom. The macrocyclic ligand deviates slightly from planarity. The forces exerted both by the ligand L on associated metal atoms, and by axial ligands on the macrocycle, are discussed.

The crystal and molecular structure of ovalene: some three-dimensional refinements

1973 ◽  
Vol 137 (2-3) ◽  
Author(s):  
R. G. Hazell ◽  
G. S. Pawley
Keyword(s):  
Molecular Structure ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray

AbstractThree-dimensional x-ray diffraction data have been taken from ovalene, C

Synthesis of Novel Tetracarboxylato Dirhenium(III) Compounds and Crystal Structure of [Re2(1-Adamantylcarboxylate)4Cl2] · 4 CHCl3

2001 ◽  
Vol 56 (4-5) ◽  
pp. 381-385 ◽  
Author(s):  
Alexander V. Shtemenko ◽  
Alexander A. Golichenko ◽  
Konstantin V. Domasevitch
Keyword(s):  
Coordination Compounds ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Quadruple Bond ◽  
Metal Atoms ◽  
Vis Spectroscopy ◽  
Related Compounds ◽  
Van Der Waals Contacts

Abstract The coordination compounds o f the general formula Re2 (L)4X2 (X = Cl, Br; L = 1 -adamantyl-carboxylate and 1 -adamantylacetate) have been prepared and characterized by means of UV-VIS spectroscopy (20000 cm-1 , δ → δ*). The crystal and molecular structure of Re2(AdCOO)4Cl2 · 4 CHCl3 solvate was determined by X-ray diffraction. The units Re2(AdCOO)4Cl2 adopt a centrosymmetric dinuclear array with each metal atom coordinated in a distorted octahedron comprising one rhenium and one chlorine atoms (Re-Cl 2.505(2) Å) and four carboxylate oxygen atoms in the equatorial plane. The rhenium-rhenium separation of 2.2300(5) Å corresponds to quadruple bond between the metal atoms. All R e-0 bonds have an almost uniform length (2.017(4) -2.032(4) Å) and do not differ essentially from the parameters reported for related compounds. The closest environment of the Re2(AdCOO)4Cl2 molecules in the crystal comprises weak Cl---HC hydrogen bonds with the chloroform molecules and significantly shortened van der Waals contacts Cl---Cl, 3.46 Å.

An X-Ray Crystallographic Study of Cd[P(C-C6H11)3]2(NO3)2.CH2Cl2

1986 ◽  
Vol 39 (4) ◽  
pp. 713 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls ◽  
ERT Tiekink
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Cadmium Atom ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Full Matrix ◽  
X Ray ◽  
Crystallographic Study ◽  
Tetrahedral Environment

The crystal and molecular structure of bis ( tricyclohexylphosphine )cadmium(II) nitrate as its dichloromethane solvate, Cd [P(c-C6H11)3]2(NO3)2.CH2Cl2, has been determined by single- crystal, three-dimensional X-ray diffraction methods. The crystals of the cadmium(II) complex are monoclinic with space group C2/c, a 20.880(6), b 12.775(3), c 17.075(5) Ǻ and β 106.38(2)°, Z 4. The structure was solved by normal Fourier methods and refined by a full-matrix least-squares procedure. The refinement used the 2169 statistically independent reflections for which I ≥ 2σ(I) converged with R and Rw of 0.065 and 0.067 respectively. The crystals consist of discrete Cd [P(c-C6H11)3]2(NO3)2 molecules and CH2Cl2 in the ratio 1 : 1. There is a distorted tetrahedral environment around the cadmium atom formed from the coordination of the two phosphines and two nitrates with each nitrate essentially occupying one stereochemical position. The two markedly different Cd -O bond lengths of 2.405(9) and 2.575(8) Ǻ show gross asymmetry in the coordination of the nitrate.

An Intermediate in the Conversion of an Acetylene to a Vinyl Derivative: The Crystal and Molecular Structure of trans-Chloromethylbis(trimethylarsine)-platinum(II) Hexafluorobut-2-yne

1972 ◽  
Vol 50 (14) ◽  
pp. 2276-2284 ◽  
Author(s):  
Brian W. Davies ◽  
Richard J. Puddephatt ◽  
Nicholas C. Payne
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Free Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Monodentate Ligand ◽  
X Ray ◽  
Trigonal Bipyramidal

The crystal and molecular structure of trans-chloromethylbis(trimethylarsine)platinum(II) hexafluorobut-2-yne has been determined from three dimensional X-ray diffraction data recorded by diffractometric methods. The structure has been refined by full-matrix least-squares methods on F using 1156 reflections to an agreement factor R = 0.077. The crystals are monoclinic, space group [Formula: see text] with a = 6.803(8), b = 14.93(2), c = 20.20(2) Å, β = 104.9(1)°, and Z = 4. The coordination of the platinum atom is trigonal bipyramidal, with the acetylene considered a monodentate ligand, and the two trimethylarsine ligands occupying the equatorial plane. The chlorine atom and the methyl ligand occupy the apical positions, with Pt—Cl and Pt—C distances of 2.47(1) Å and 2.10(4) Å, respectively. The long Pt—Cl bond length indicates the strong trans-influence of the methyl ligand. The observed C—C bond length of 1.32(4) Å in the acetylene ligand is lengthened from the value of 1.22(9) Å measured in the free ligand. The geometry of the coordinated ligand is discussed in terms of the bonding scheme proposed by Greaves etal.

CaTMg2 and CaTCd2 (T =Rh, Pd, Pt) with YPd2Si-type Structure

2013 ◽  
Vol 68 (2) ◽  
pp. 111-120 ◽  
Author(s):  
Michael Johnscher ◽  
Marcel Kersting ◽  
Samir F. Matar ◽  
Rainer Pöttgen
Keyword(s):  
Three Dimensional ◽  
Site Occupancy ◽  
Small Range ◽  
X Ray Diffraction ◽  
Interatomic Distances ◽  
Metal Atoms ◽  
Transition Metal Atoms ◽  
Covalently Bonded ◽  
A Site ◽  
Calcium Compounds

The intermetallic calcium compounds CaTMg2 and CaTCd2 (T =Rh, Pd, Pt) were obtained by high-frequency melting of the elements in sealed niobium ampoules or through reactions in muffle furnaces. The polycrystalline samples were characterized by powder X-ray diffraction. They crystallize with a site occupancy variant of YPd2Si, a ternary ordered version of Fe3C. The structures of CaPdMg2 and CaPdCd2 were refined from single-crystal diffractometer data: Pnma, a=792.2(2), b=803.4(2), c=572.0(1) pm, wR2=0.0663, 1621 F2 values, 24 variables for Ca0:94PdMg2:06 and a=794.6(2), b=809.5(3), c=554.7(2) pm, wR2=0.0301, 819 F2 values, 23 variables for CaPdCd2. A small range of homogeneity was observed for Ca1-xPdMg2+x. The magnesium and cadmium atoms build up three-dimensional tetrahedral substructures (306 - 327 pm Mg-Mg and 307 - 317 pm Cd-Cd) that resemble hexagonal diamond, lonsdaleite. Together with the palladium atoms one obtains three-dimensional, covalently bonded [PdMg2] and [PdCd2] networks which leave cages for the calcium atoms. The latter are bonded to these networks via shorter Ca-Pd contacts (298 - 319 pm in Ca0:94PdMg2:06 and 295 - 312 pm in CaPdCd2). The course of the interatomic distances is in line with calculated overlap populations. The CaPdMg2, SrPdMg2 and CaRhIn2 structures are all derived from a CaIn2-related subcell by an ordered filling of transition metal atoms into trigonal prisms. This leads to different herringbone patterns for the networks of puckered and elongated hexagons of magnesium and indium atoms.

The crystal and molecular structure of aqua-bis(ethylenediamine)cupric-tris(cyano)-selenocyanatodicuprate

1982 ◽  
Vol 47 (10) ◽  
pp. 2623-2632 ◽  
Author(s):  
Viktor Vrábel ◽  
Jan Lokaj ◽  
Ján Garaj ◽  
František Pavelčík
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Triclinic System

The crystal structure of [Cu(H2O)(en)2][Cu2(CN)3(SeCN)] was solved by single crystal X-ray structural analysis in the triclinic system with a space group of P1 and in the monoclinic system with a space group of C2. In the triclinic system the unit cell has dimensions of a = 0.8445(3), b = 0.7903(3), c = 0.8444(3) nm, α = 119.58(2), β = 118.59(2) and γ = 93.63(3)° and, in the monoclinic system, a = 1.3331(4), b = 0.8670(2), c = 0.8267(3), β = 122.60(2)°. The structure was refined by the least squares method to final value of R = 5.5% in the triclinic system and R = 7.8% in the monoclinic system. The coordination sphere around the Cu(II) atom is square pyramidal, formed of two ethylenediamine molecules and one water molecule. The Cu(I) atoms are tetrahedrally coordinated by bridging SeCN and CN ligands to form infinite three-dimensional chains. The SeCN group is bonded to the Cu(I) atoms through the Se atom at distances of 0.2731(3) and 0.2745(3) nm.

The crystal structure of diethylene tetraxanthogen, the oxidation product of the diethylene dixanthate ion

1974 ◽  
Vol 27 (1) ◽  
pp. 27
Author(s):  
BF Hoskins ◽  
MR Hunt
Keyword(s):  
Oxidation Product ◽  
Least Squares Method ◽  
Ring Structure ◽  
The Novel ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
X Ray ◽  
Disulphide Bonds ◽  
A Site ◽  
Short Carbon

The structure of the oxidation product of the diethylene dixanthate anion, diethylene tetraxanthogen (Cl12H1606S8), has been determined by single crystal X-ray diffraction methods. The crystals are tetragonal of space group Z41/acd with a 15.798(1), c 17.755(1) �, containing eight molecules per unit cell. The structure was solved using conventional Patterson and Fourier methods and refined by a full-matrix least-squares method to R 0.055 for the 817 independent statistically significant reflections collected by counter methods. The crystals are composed of discrete molecules held together by van der Waals forces. Each molecule, situated about a site of symmetry 222, has the novel 22-membered ring structure involving disulphide bonds of length 2.035(2) �. The planarity of the dithiocarbonate moiety and the relatively short carbon-to-oxygen and carbon-to-sulphur bond lengths correlate with extensive π-electron delocalization over the group.

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