The Crystal and Molecular Structure of Pentane-2,4-dionato-(2,3,5,6-tetrahepto-2,3-dicarbomethoxo[2.2.1]bicycloheptadiene)rhodium(I), Rh(C5H7O2) (C7H6(CO2CH3)2)

1975 ◽  
Vol 53 (18) ◽  
pp. 2707-2713 ◽  
Author(s):  
Debbie Allen ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
John Powell
Keyword(s):  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Rhodium Atom

The crystal and molecular structures of pentane-2,4-dionato-(2,3,5,6-tetrahapto-2,3-dicarbomethoxo[2.2.1]bicycloheptadienerhodium(I), Rh(C5H7O2)(C7H6(CO2CH3)2), have been measured by single crystal X-ray diffraction. The orange crystals are monoclinic, space group P21/c, Z = 4, a = 9.245(4), b = 9.003(4), c = 21.680(15) Å, β = 113.41(5)°. The calculated and observed densities are 1.645 and 1.642(5) respectively. Intensity data were collected on a Syntex [Formula: see text] diffractometer and a full matrix least squares refinement on 3010 observed reflections leads to a conventional R = 0.0660. The structure can be considered as a roughly square planar arrangement of ligands around the rhodium atom composed of two β-ketoenolate oxygen atoms (Rh—O, 2.037(5) and 2.025(5) Å ) and the centers of the two ethylenic groups. The Rh—C distances for the olefin group attached to the two carbomethoxo groups, 2.117(8), 2.108(8) Å, appear to be slightly larger than those for the other olefinic group, 2.087(7), 2.082(6), and the corresponding C=C distances of 1.375(10) and 1.410(9) Å are different at the 95% confidence level.

Complexes containing unsaturated medium rings: The crystal and molecular structures of two rhodium(I) complexes

1978 ◽  
Vol 31 (4) ◽  
pp. 781 ◽  
Author(s):  
R Mason ◽  
GR Scollary
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Medium Rings

The crystal and molecular structures of two rhodium(I) complexes with long-chain alkyne- or alkene-α,ω-diyldiphosphines have been determined by single-crystal X-ray diffraction techniques. RhCl(CO){But2P(CH2)4C≡C(CH2)4PBut2} crystallizes in the orthorhombic space group Pna21 with a 21.991 (2), b 11.915(1), c 11.890(1) Ǻ and Z 4. The structure was refined by least-squares methods to a conventional R factor of 0.097 for 1768 independent reflections (Mo Kα diffraction data). The rhodium ion is in a square-planar coordination geometry with trans-phosphorus atoms; the unsaturated (alkynyl) group is not bonded to the rhodium. Crystals of RhCl{But2P(CH2)2CH=CH(CH2)2- PBut2} are monoclinic, space group P21/c, a 20.783(12), b 8.580(4), c 14.799(9) Ǻ, β 100.70(2)°, Z 4. The structure analysis has converged to R 0.069 for 1417 reflections (Mo Kα diffractometry); the coordination geometry of the rhodium is again planar with the ethylenic group occupying a single bonding site. The effect of ring size on the rhodium-phosphorus bond lengths is discussed.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

Weak interactions observed in ruthenium and iridium complexes containing hydride, amine, and bulky phospyhine ligands

1997 ◽  
Vol 75 (5) ◽  
pp. 475-482 ◽  
Author(s):  
Wei Xu ◽  
Alan J. Lough ◽  
Robert H. Morris
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Weak Interactions ◽  
Crystal Structure Analysis ◽  
Monoclinic Space Group ◽  
Iridium Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Van Der Waals Contacts

New amineruthenium and amineiridium hydride derivatives have been synthesized and characterized with the objective of observing intramolecular [Formula: see text] or [Formula: see text] interactions. These include RuHCl(CO)(L)(PPri3)2 (1a, L = NH2NH2; 1b, L = NH3) and IrCl2(L)(H)(PCy3)2 (2a, L = SC(NH2)2; 2b, L = NH3; 2c, L = NH2NH2; 2d, L = NH2(CH2)3NH2; 2e, L = NH2OH). Instead, weak [Formula: see text] van der Waals contacts have been detected in the solid state by X-ray analysis and in solution by NMR T1 measurements and nOe techniques. Both X-ray crystal structure analysis and minimum T1 measurements indicate that the [Formula: see text] distances in the [Formula: see text] interactions are ca•2.0–2.2 Å. The weak interactions might influence the course of deuteration of these complexes under D2 gas. The crystal and molecular structure of IrCl2(NH3)(H)(PCy3)22a has been determined by X-ray diffraction at 173 K: monoclinic, space group P21/n, a = 14.859(2) Å, b = 18.579(3) Å, c = 18.548(3) Å, β = 97.29(1)°, V = 5079.1(13) Å3, Z = 4, full-matrix least-squares refinement on F2 for 10 953 independent reflections; R[F2 > 4σ(F2)] = 0.0283, wR(F2) = 0.0704. Keywords: ruthenium, iridium, hydride, dihydrogen, complexes, hydrogen bond, NMR, X-ray.

Crystal structures of 1-(m-nitrophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (C22H22N2O7) (I) and 1-(p-chlorophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (C22H22NO5Cl) (II)

1989 ◽  
Vol 189 (3-4) ◽  
Author(s):  
G. D. Nigam ◽  
G. Mattern ◽  
R. Fröhlich
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of 1-(m-nitrophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (I) and 1-(p-chlorophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (II) have been determined by X-ray diffraction methods. (I) crystallizes in the monoclinic space group

Crystal and molecular structure of 4α-t-Butylcyclohexane-1β,2β-diol

1972 ◽  
Vol 25 (10) ◽  
pp. 2117 ◽  
Author(s):  
MD Brice ◽  
BR Penfold ◽  
WT Robinson
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Least Squares Techniques

The crystal and molecular structure of 4α-t-butylcyclohexane-1β,2,β-diol, C10H20O2, has been determined by X-ray diffraction methods. The compound crystallizes in the triclinic space group Pi with 4 molecules in a unit cell of dimensions a = 12.268, b = 15.921, c = 6.322�, α = 82.53, β = 114.45, γ = 111.13�. The intensity data were measured by counter methods using Cu Kα radiation; the structure was solved by means of the tangent formula, and was refined using full matrix least-squares techniques to a final R-factor of 0.063 for 1199 reflections. The crystal structure consists of two sets of crystallographically non-equivalent molecules hydrogen-bonded to form discrete chains parallel to the c axis. The cyclohexane rings are in the chair conformation.

The crystal and molecular structure of a platinum-silatrane complex

1977 ◽  
Vol 30 (5) ◽  
pp. 1007 ◽  
Author(s):  
GR Scollary
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

A structural analysis of the platinum-silatrane complex, PtCl [Si(OCH2CH2)3N] [PMe2Ph]2, has been carried out by X-ray diffraction. Crystals are monoclinic, space group P21/c, a 6.630(4), b 17.465(6), c 22.297(6) Ǻ, β 97.4(2)�, Z 4. The structure has been refined by a full- matrix least-squares procedure to R 0.048 for 2165 reflections. Basic geometries are square (platinum), tetrahedral (silicon) and trigonal (nitrogen). Within the silatrane ligand, the Si-N non-bonding distance is 2.89(1) Ǻ.

Synthesis of aminoalcohol compounds of platinum and crystal structure of trans-[Pt(2-amino-2-methyl-1-propanol)2Cl2]

1984 ◽  
Vol 62 (12) ◽  
pp. 2657-2660 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson
Keyword(s):  
Crystal Structure ◽  
Organic Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Bonding System ◽  
Square Planar ◽  
Hydrogen Bonding System

Three types of complexes, trans-[Pt(LH)2Cl2], [Pt(L)2], and [Pt(LH)2(SR)2] where LH = NH2—C(CH3)2(CH2OH) and NH2—C(CH2OH)3 and L are the deprotonated ligands, have been synthesized.The crystal structure of trans-[Pt(NH2—C(CH3)2CH2OH)2Cl2] has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with a = 6,282(3), b = 20,901(13), c = 10,769(10) Å, β = 92,64(6)°, and Z = 4. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.049 and Rw = 0.042. The coordination around the platinum atom is square planar. The Pt—Cl distances are 2.306(2) and 2.309(3) Å and the Pt—N bonds are 2.060(8) and 2.071 (7) Å. The hydroxyl oxygen atoms are disordered; the disorder is different for each organic ligand. The structure is stabilized by an extensive hydrogen bonding system.

Structural and spectroscopic characterization of isotypic sodium, rubidium and cesium acesulfamates

2015 ◽  
Vol 70 (7) ◽  
pp. 491-496 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Eduardo E. Castellano ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Aqueous Solutions ◽  
Single Crystal ◽  
Potassium Salt ◽  
Spectroscopic Characterization ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThree new acesulfamate salts, NaC4H4NO4S, RbC4H4NO4S and CsC4H4NO4S, were prepared by reactions in aqueous solutions and thoroughly characterized. Their crystal and molecular structures were determined by single crystal X-ray diffraction methods. They crystallize in the monoclinic space group P21/a with a = 7.2518(2), b = 8.9414(4), c = 10.5929(4) Å, β = 99.951(3)°, V = 676.52(4) Å3 for the Na salt; a = 7.4663(3), b = 9.6962(4), c = 10.4391(4) Å, β = 95.150(3)°, V = 752.68(5) Å3 for the Rb salt and a = 7.5995(4), b = 9.9439(4), c = 10.8814(6) Å, β = 91.298(5)°, V = 822.08(7) Å3 for the Cs salt, and Z = 4 molecules per unit cell. The three compounds are isotypic to each other and to the previously reported potassium salt. The metal ions are in irregular polyhedral coordination with six neighboring acesulfamate anions through their nitrogen and carbonyl and sulfoxide oxygen atoms. The FTIR spectra of the compounds were also recorded and are briefly discussed.

Two crystal structures of 10,10′-(l,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone

1992 ◽  
Vol 200 (3-4) ◽  
Author(s):  
G. Dewald ◽  
M. Hanack ◽  
E.-M. Peters ◽  
L. Walz
Keyword(s):  
Crystal Structures ◽  
Diffraction Data ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of dimorphic 10,10′-(1,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone (1) have been determined using X-ray diffraction data. The compound crystallizes either in the monoclinic space groupSince all non-hydrogen atoms are of pure

Reactions of "cyclen-" and "cyclam-phosphorane" with [Pt2Cl4(PEt3)2]. Monodentate and bidentate complexes and the crystal and molecular structure of [PtCl(PEt3)(cyclamPH)]Cl•CH2Cl2

1989 ◽  
Vol 67 (1) ◽  
pp. 48-53 ◽  
Author(s):  
David Eric Berry ◽  
Jane Browning ◽  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Alan Pidcock
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Simple Formula ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Square Planar ◽  
Coordination Plane

Reaction of "cyclamphosphorane" (cyclamPH) with [Pt2Cl4(PEt3)2] yields [PtCl(PEt3)(cyclamPH)]Cl. The complex crystallizes as a dichloromethane solvate in the monoclinic space group P21/n, with a = 13.877(3), b = 23.231(7), c = 8.295(2)Å, β = 91.86(4)°, and an X-ray diffraction study shows square planar platinum coordination in which the labile proton of cyclamPH has transferred from phosphorus to nitrogen and the ligand is attached via simple [Formula: see text] chelation. The phosphorus is trans to chlorine in the platinum coordination plane.The corresponding product, trans-[PtCl2(PEt3)(cyclenPH2)]Cl, derived from reaction of "cyclenphosphorane" (cyclenPH) with [Pt2Cl4(PEt3)2], is shown by NMR studies to have a quite different structure in which the ligand is protonated at two nitrogen sites but not at phosphorus. The phosphorus is pentacoordinate with four attachments to nitrogen atoms and one to platinum. The two chlorine atoms are mutually trans in the platinum coordination plane. Keywords: crystal structure, cyclenphosphorane reaction, cyclamphosphorane reaction, X-ray diffraction.

Sign in / Sign up

Export Citation Format

Share Document