The crystal and molecular structure of trans-chloro(3-hydroxypropyl-N,N-dimethylaininocarbene)-bis(dimethylphenylphosphine)platinum(II) hexafluorophosphate

1978 ◽  
Vol 56 (12) ◽  
pp. 1602-1609 ◽  
Author(s):  
Robert F. Stepaniak ◽  
Nicholas C. Payne
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
Square Planar ◽  
Cell Dimensions ◽  
Cation Coordination

The crystal and molecular structure of trans-chloro(3-hydroxypropyl-N,N-dimethylaminocarbene)bis(dimethylphenylphosphine)platinum(II) hexafluorophosphate has been determined from three-dimensional X-ray data collected on an automated four circle diffractometer using CuKα radiation. The compound crystallizes in the orthorhombic space group Pna21, with Z = 4, and cell dimensions a = 14.403(2), b = 12.631(2), and c = 16.151(2) Å. Full matrix least-squares refinement on F gave a final conventional R factor of 0.047 for 3442 observations with I > 3σ(I). The cation coordination geometry is square planar, with the carbene ligand lying approximately perpendicular to the plane. The Pt—Cl bond length is 2.356(4) Å and the Pt—C(carbene) distance is 1.978(12) Å. The C(carbene)—N bond length is 1.293(16) Å. These dimensions are discussed in terms of the trans influences of the carbene and chloride ligands and the bonding in the carbene species.

The Crystal and Molecular Structure of 3-Chloro-3-deoxy-1,2;5,6-di-O-isopropylidene-β-D-idose

1972 ◽  
Vol 50 (1) ◽  
pp. 93-98 ◽  
Author(s):  
F. W. B. Einstein ◽  
K. N. Slessor
Keyword(s):  
Molecular Structure ◽  
Furan Ring ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
A Cell ◽  
The Mean ◽  
Least Squares Techniques

The crystal and molecular structure of 3-chloro-3-deoxy-1,2;5,6-di-O-isopropylidene-β-D-idose has been determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.7% for the 817 observed reflections. The compound crystallizes in the orthorhombic space group P212121 with four molecules in a cell of dimensions a = 9.744(6), b = 26.76(2), c = 5.403(3) Å.The structure analysis has served to confirm the site of halogenation and that it occurs stereospecifically. The conformation of the furan ring is an envelope arrangement with C(4) displaced from the mean plane.

Perchlorato, Nitrato, and Acetylacetonato Complexes of Copper(I). The Crystal and Molecular Structure of Perchloratobis(tricyclohexyiphosphine)Copper(I)

1975 ◽  
Vol 53 (13) ◽  
pp. 1949-1957 ◽  
Author(s):  
Roderic J. Restivo ◽  
Abraham Costin ◽  
George Ferguson ◽  
Arthur J. Carty
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Infrared Spectra ◽  
Copper Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Cell Dimensions

Copper(I) perchlorate, nitrate, and acetylacetonate complexes of the types Cu(triphos)ClO4 (triphos = CH3C(CH2PPh2)3), Cu(Cy3P)2ClO4 (Cy3P = P(C6H11)3), Cu(triphos)NO3, Cu(Cy3P)2(HFac)(HFac = hexafluoroacetylacetonate), and Cu (Cy3P)2(TtFac) (TtFac = thienyltrifluoroacetylacetonate) have been synthesized by reduction of the corresponding perchlorate, nitrate, and acetylacetonates with tertiary phosphines. Infrared spectra indicate the presence of monodentate perchlorate groups in Cu(triphos)ClO4 and in Cu(Cy3P)2ClO4 and the crystal structure of the latter has been determined by a three-dimensional X-ray analysis using diffractometer data. The crystals are monoclinic, space group C2/c, with cell dimensions a = 18.159(6), b = 9.493(2), c = 22.182(3) Å, and β = 95.41(2)° and four molecules per unit cell. The structure was refined by block-diagonal least squares methods to a final R of 0.051 for 2617 reflections using anisotropic thermal parameters for the nonhydrogen atoms. The structure consists of discrete Cu(Cy3P)2ClO4 molecules with symmetry C2 separated by normal van der Waals distances. The copper atom is three-coordinate and the perchlorate anion is monodentate but disordered over two sites. Principal dimensions include: Cu—P 2.262(1) Å, Cu—O 2.220(7) Å, [Formula: see text][Formula: see text] and 99.8(2)°, and [Formula: see text]

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.

scholarly journals The Crystal and Molecular Structure of Diazido-2,2′-bipyridinecopper(II)

1974 ◽  
Vol 52 (17) ◽  
pp. 3125-3133 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Masood A. Khan
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar ◽  
Copper Coordination ◽  
Cell Dimensions ◽  
Coordinate Bond

The crystal and molecular structure of diazido-2,2′-bipyridinecopper(II), C10H8N2(N3)2Cu, is determined by single crystal X-ray diffraction, and refined to an R value of 0.067. The cell dimensions are a = 664.9(2), b = 843.3(1), c = 1082.0(2) pm, α = 86.99(2)°, β = 87.77(3)°, γ = 78.59(2)°. The space group is [Formula: see text] (No. 2) with 2 molecules per unit cell and the measured density is 1.71(2) g cm−3. The copper coordination is square planar with two additional longer bonds. The coordinate bond lengths in pm to the bipyridine ligand are: Cu—N(1), 201.6(6); Cu—N(2), 201.9(6). The coordinate bonds to the azido ligands are: Cu—N(3), 194.9(6); Cu—N(6), 196.6(6). The longer bonds are: Cu—N(3)″, 268.0(8), Cu—N(6)′ 268.2(8). The N—N bond lengths within each azido ligand are unequal: N(3)—N(4), 118.2(10); N(4)—N(5), 115.4(11); N(6)—N(7), 119.2(9); N(7)—N(8), 114.8(9). The angles at N(3) and N(6) are both 130° and at N(4) and N(7) the angles are both 175(1)°. Each azide takes part in asymmetric bridging through a single nitrogen atom. The results are compared with other structural studies on azido complexes and to a nitrate complex of Ag(II) which is structurally similar.

Cyclische Diazastannylene, X [1] Die Kristall-und Molekülstruktur eines Moleküls mit verzerrt-würfelförmigem Sn4N3O-Käfig / Cyclic Diazastannylenes, X [1] The Crystal and Molecular Structure of a Molecule with a Distorted Cube-Shaped Sn4N3O-Cage

1981 ◽  
Vol 36 (2) ◽  
pp. 144-149 ◽  
Author(s):  
M. Veith ◽  
. Recktenwald
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Point Symmetry ◽  
Mean Values ◽  
Space Group ◽  
X Ray ◽  
Tert Butyl ◽  
Cell Dimensions

Abstract The crystal and molecular structure of (me3CN)3(me3A1O)Sn4 has been determined from three-dimensional X-ray data (4-circle diffractometer, R - 0.048). The crystals are mono-clinic, space group P2i/c, with cell dimensions a = 1017.4(5), b - 1488.5(7), c = 1748(1) pm, β-91.5(1)° and Z - 4. The molecules approach 3m point-symmetry and include a Sn4N3O-cage, the atoms occupying the corners of a distorted cube formed by two, differently sized, interpenetrating concentric tetrahedra of tin and nitrogen/oxygen atoms. The nitrogen atoms are attached to tert-butyl groups, whereas the oxygen atom of the cage acts as a base towards the aluminiumtrimethyl group. Typical bond distances and angles (mean values) are: Sn-N = 219.9, Sn-0 = 220.3 pm; N-Sn-N = 81.2°; N-Sn-0 = 79.0°; Sn-N-Sn = 98.8° and Sn-O-Sn -100.2°.

Crystal and molecular structure of a platinum(0) complex of cyclooctyne

1980 ◽  
Vol 33 (6) ◽  
pp. 1373 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Space Group ◽  
X Ray ◽  
Coordination Sites ◽  
Square Planar ◽  
R Factors ◽  
Normal Bond ◽  
Least Squares Techniques

The crystal and molecular structure of a platinum(0) complex of cyclooctyne, [(coct)Pt(PPh3)2], has been determined from three- dimensional X-ray data collected by counter methods. The complex crystallizes in the space group P21/n [a non-standard setting of space group P21/c (C2h5, No. 14)], with a 20.660(9), b 12.299(5), c 15.470(7) Ǻ, β 110.26(2)°, Z 4. The structure was solved by conventional Patterson and Fourier methods and was refined by block-diagonal least-squares techniques to weighted and unweighted R-factors of 0.048 and 0.047 respectively, for the 4733 unique reflections with I/σ(I) ≥ 3.0. The molecule is essentially square planar about the 'central' platinum atom, with the triphenylphosphine groups occupying cis coordination sites. The Pt-C distances are equal within experimental error [2.034(9) and 2.037(9) Ǻ] and compare favourably with the corresponding distances in the platinum(0)-cyclohexyne and -cycloheptyne analogues. The acetylenic C=C distance is 1.279(13) Ǻ and shows the normal bond lengthening consequent upon coordination.

Cyclische Diazastannylene, III1 Die Kristall-und Molekülstruktur der monoklinen Phase von 1.3-Di-tert-butyl-2.2-dimethyl-1.3.2.4λ2 -diazasilastannetidin / The Crystal and Molecular Structure of the Monoclinic Phase of 1,3-Di-feri-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine

1978 ◽  
Vol 33 (1) ◽  
pp. 7-13 ◽  
Author(s):  
M. Veith
Keyword(s):  
Molecular Structure ◽  
Monoclinic Phase ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Site Symmetry ◽  
Space Group ◽  
X Ray ◽  
Tert Butyl ◽  
Cell Dimensions

Abstract The crystal and molecular structure of the monoclinic phase of 1,3-di-tert-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine has been determined from three-dimensional X-ray data collected on a two-circle diffractometer at -120 °C (MoKa radiation, 2623 reflexions, R - 0,050). The crystals are monoclinic, space group C2/c, with cell dimensions a = 10.655(5), b = 25.75(1), c = 17.33(1) Å, β = 106.8(1)° and Z = 12. Four monomeric (crystal site symmetry 2 (C2)) and four dimeric units (crystal site symmetry 1̄ (Ci)) are present in the structure interacting over tin-tin (3.68 Å). Remarkable are the very short Sn-N bond (2.09 Å) in the monomer and the donation bond Sn-N (2.39 Å) in the dimer. The coordination of the tin atoms in the different units is discussed in detail.

The Crystal and Molecular Structure of Dichloro(acetylacetonato)-2,2′-bipyridylindium(III)

1974 ◽  
Vol 52 (22) ◽  
pp. 3793-3798 ◽  
Author(s):  
J. G. Contreras ◽  
F. W. B. Einstein ◽  
D. G. Tuck
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
R Factor ◽  
Chloride Ligands ◽  
Least Squares Techniques

The molecular structure of dicholoro(acetylacetonato)-2,2′-bipyridylindium(III) has been determined from three dimensional X-ray data collected by counter methods. The structure has been refined by least-squares techniques to a conventional R factor of 4.3% for the 3524 observed reflections. Crystals of Cl2In(acac)(bipy) are monoclinic, a = 11.340(3), b = 12.198(3), c = 14.330(3) Å, β = 120.25(2)°, z = 4, space group P21/c. The chloride ligands are cis, with In—Cl at distances of 2.443(1) and 2.394(1) Å; the In—O bond lengths are 2.124(3) and 2.164(3) Å, and the In—N bond distances are 2.276(4) and 2.299(4) Å.

The Crystal and Molecular Structure of Tetrameric Phosphonitrilic Isothiocyanate

1972 ◽  
Vol 50 (9) ◽  
pp. 1315-1320 ◽  
Author(s):  
J. Brian Faught
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Phosphorus Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Unit Cell ◽  
Triclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Nitrogen Ring

The crystal structure of tetrameric phosphonitrilic isothiocyanate, N4P4(NCS)8, has been determined by three-dimensional X-ray studies from data collected on a Picker FACS-1 automated diffractometer. The compound crystallizes in the triclinic space group [Formula: see text] with a = 8.098(8), b = 8.018(7), c = 9.937(10) Å, α = 104.08(7), β = 99.42(7), γ = 95.42(7)°, and one molecule per unit cell. The structure was solved from 1766 independent non-zero reflections and refined to a conventional R factor of 0.063. Nitrogen atoms of two isothiocyanate groups are bonded to each phosphorus atom of the eight-membered phosphorus–nitrogen ring. The ring has a chair configuration. The average dimensions of the structure are P—Nring = 1.543 + 0.017, P—Nisothiocyanate = 1.644 ± 0.011, N—C = 1.168 ± 0.008, C—S = 1.535 + 0.009 Å, [Formula: see text] [Formula: see text] [Formula: see text] [Formula: see text] and NĈS = 176.6 ± 1.1°.

The crystal and molecular structure of tris(pentamethylenedithiocarbamate) chromium(III)-chloroform (1 : 2)

1981 ◽  
Vol 46 (1) ◽  
pp. 6-19 ◽  
Author(s):  
Viktor Kettman ◽  
Ján Garaj ◽  
Jaroslav Majer
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Complex Molecules ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cell Dimensions ◽  
Crustal Density ◽  
Unit Cell Dimensions

The crystal and molecular structure of [Cr(S2CN(CH2)5)3].2 CHCl3 was found by the X-ray structural analysis method. The value R 0.090 was found for 1 131 observed independent reflections. The substance crystallizes in a space group of symmetry P212121 with the following unit cell dimensions: a = 0.8675 (6), b = 1.815(2), c = 2.155(3) nm. The experimentally observed crustal density was 1.48 Mgm-3 and the value calculated for Z = 4 was 1.51 Mgm-3. The CrS6 coordination polyhedron has the shape of a trigonally distorted octahedron, where the D3 symmetry is a approximately retained. The degree of trigonal distortion expressed as the projection of the chelate S-Cr-S angle onto the plane perpendicular to the C3 pseudo axis is Φ = 41.7° (Φ = 60° for an octahedron). The skeleton of the structure formed by the complex molecules contains channels filled with chloroform molecules. The specific type of complex-chloroform interaction consists of the formation of hydrogen bonds of the chloroform protons with the fully occupied pπ-orbitals of the sulphur atoms in the coordination polyhedra. The low stability and crystal decomposition can be explained by loss of chloroform from the channels.

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