Synthesis and Spectroscopic Studies of Triorganotin(IV) Complexes Involving Diorganophosphino and Diorganophosphino-N-Phenyl(Thioformamido) Ligands - the Crystal and Molecular-Structure of Dicyclohexylphosphino-N-Phenyl(Thioformamido)-Triphenyltin, Ph3Sn[(c-C6H11)2PC(S)NPh]

1986 ◽  
Vol 39 (8) ◽  
pp. 1221 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls
Keyword(s):  
Molecular Structure ◽  
Sulfur Atom ◽  
Crystal And Molecular Structure ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Tetrahedral Environment ◽  
Tin Complexes

Phosphorus-31 and tin-119 n.m.r . data imply that the tin complexes R3Sn[R1,PC(S) NPh ] (where R = Ph, Me, Bu; R′ = Ph) exist in solution as both sulfur-bonded and nitrogen-bonded isomers. When R′ = c-C6H11, only one isomer is observed. n.m.r . data are also reported for the series R3SnPR′2. Both series of complexes contain four-coordinate tin in dichloromethane solution. The crystal and molecular structure of the tin(IV) complex Ph3Sn[(c-C6H11)2PC(S) NPh ] has been determined by single-crystal X-ray diffraction techniques. The crystals are triclinic, space group Pī , a 10.689(2), b 11.066(1), c 16.315(3) Ǻ, α 101.94(1), β 104.85(1) and γ 105.72(1)° with Z 2; R and Rw were 0.032 and 0.030 respectively for 5169 unique reflections with I ≥ 2σ(I). The structure has two independent centrosymmetrically related mononuclear molecules within the unit cell. The tin atom is in a tetrahedral environment formed by three phenylic carbon atoms and a sulfur atom from the [(c- C6H11)2PC(S) NPh ]- ligand.

Investigation of Isomer Formation of Triorganotin(IV) Complexes Involving Diorganophosphino-N-Phenyl(Thioformamide) Ligands: The Crystal and Molecular-Structure of [Diphenylphosphino-N-Phenyl(Thioformamido)]Triphenyltin, Ph3Sn[Ph2PC(S) NPh ]

1988 ◽  
Vol 41 (2) ◽  
pp. 195 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Sulfur Atom ◽  
Crystal And Molecular Structure ◽  
Steric Effects ◽  
X Ray Diffraction ◽  
Similar Compound ◽  
Space Group ◽  
X Ray ◽  
Tetrahedral Environment

The isomer of Ph3Sn[Ph2PC(S) NPh] formed depends on the method of preparation. The crystal and molecular structure of the tin(IV) complex Ph3Sn[Ph2PC(S) NPh ] has been established by single-crystal X-ray diffraction techniques. The crystals are monolinic, space group P21/n, a 12.620(2), b 10.541(2), c 24.292(4)Ǻ, β 96.90(1) with Z 4; R and Rw were 0.031 and 0.034 respectively for 5632 unique reflections with I > 3σ(I). The crystals consist of discrete Ph3Sn[Ph2PC(S) NPh ] molecules. There is a tetrahedral environment about the tin atom formed by the three phenylic carbons and a sulfur atom of the [Ph2PC(S) NPh ]- ligand . Comparisons are made with the structurally similar compound Ph3Sn[(c-C6H11)2PC(S) NPh ]. On the basis of these comparisons and on earlier n.m.r . data, a favoured four-centered mechanism for insertion of dipolar PhNCS into the tin-phosphorus bond of Ph3SnPPh2 is inferred. Differences in reactivity of Ph2PC(S)N(H)Ph and (c-C6H11)2PC(S)N(H)Ph appear to result from electronic rather than steric effects.

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.

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.

Crystal and molecular structure of Octacarbonylbis(diphenylarsino)-methanedimanganese(0)

1983 ◽  
Vol 36 (4) ◽  
pp. 683 ◽  
Author(s):  
BF Hoskins ◽  
RJ Steen
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Parent Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
X Ray

The crystal structure of the complex Mn2(CO)8(dam) (dam = Ph2AsCH2AsPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are triclinic, space group P1, with a 11.191(1), b 16.498(5), c 9.455(1) �, a 93.64(2), β 109.08(2), γ 89.36(2)� and contain two discrete, binuclear molecules of Mn2(CO)8(dam) per unit cell. The structure, solved by direct and Fourier methods, was refined by a least-squares procedure to R and Rw of 0.065 and 0.082 respectively for 1907 independent, statistically significant reflections collected by counter methods. The feature of particular interest in this compound is the accommodation of the bridging bidentate dam ligand [As.. .As separation 3.242(2) �] across a shorter Mn�-Mn� bond [2.962(3) �] which constrains the molecule so that a much less staggered configuration of the two manganese coordination octahedra is observed relative to the parent compound Mn2(CO)10, the rotation of the two equatorial planes in the former being 30�.

The preparation and the crystal and molecular structure of S3N2NH2+BF4−; a molecular orbital study of the protonation of the trisulphur trinitride anion

1984 ◽  
Vol 62 (9) ◽  
pp. 1822-1827 ◽  
Author(s):  
Clifford G. Marcellus ◽  
Richard T. Oakley ◽  
A. Wallace Cordes ◽  
William T. Pennington
Keyword(s):  
Molecular Structure ◽  
Molecular Orbital ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Membered Ring ◽  
Molecular Orbital Calculations ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Molecular Orbital Study

Protonation of the trisulphur trinitride ion, S3N3−, with tetrafluoroboric acid yields the ring-contracted S-amino thiodithiazyl salt, S3N2NH2+BF4−. The crystal and molecular structure of this salt has been determined by X-ray diffraction. The crystals are triclinic, space group P1, with a = 5.445(2), b = 7.346(3), c = 9.473(5) Å, α = 85.89(4), β = 83.92(3), γ = 82.13(3)°, V = 372.6(4) Å3, Dc = 2.02 g cm−3, and Z = 2. The structure was solved by direct methods and refined by full-matrix least-squares procedures to give a final R = 0.060. The structure of the five-membered ring with a single exocyclic NH2 group bonded to sulphur is discussed in relation to other S3N2NR derivatives. The reasons for the instability of six-membered rings of the type S3N3R are discussed in the light of MNDO molecular orbital calculations on an S3N3H model.

Synthesis, Infrared and X-Ray Studies of Diphenyltellurium(IV) Nitrosocarbamylcyanmethanides. X-Ray Evidence for Stability of a Tritelluroxane Fragment -Ph2Te-O-Ph2Te-O-Ph2Te-

1996 ◽  
Vol 51 (6) ◽  
pp. 832-837 ◽  
Author(s):  
Konstantin V. Domasevitch ◽  
Victor V. Skopenko ◽  
Eduard B. Rusanov
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Spectroscopic Data ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Nitroso Group ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic ◽  
Derivatives Of

Abstract Diphenyltellurium(IV) derivatives of the types Ph2Te{ACO}2 (1), Ph4Te2O{ACO}2 (2) and Ph6Te3O2{ACO} (3) (ACO = nitrosocarbamylcyanmethanide -ONC(CN)C(O)NH2) have been prepared. The IR spectroscopic data reveal that the ambidentate ligands are coordinated to the tellurium(IV) atom in a monodentate manner via the nitroso oxygen atom. The crystal and molecular structure of 3 has been determined from X-ray diffraction data (triclinic, space group P1̅ with a = 12.382(2), 6=13.100(2), c = 14.944(3) Å, a = 87.74( 1), β = 85.04(2), 7 = 66.29( 1)°, V = 2211.0 A , Z = 2, R = 0.040). The structure is made up of unsymmetric molecules, in which the tellurium atoms are linked by oxo bridges to form chains Te-O-Te-O-Te (d(Te-O) ca. 1.94-2.09 A). The Te-0 (nitroso group) bond lengths are in the range 2.33 - 2.36 Å

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

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