Synthesis and conformational analysis of 2-arylseleno-1,3-dithianes. Crystal and molecular structure of 2-(4-methoxyphenylseleno)- and 2-(4-trifluoromethylphenylseleno)-1,3-dithiane

1986 ◽  
Vol 64 (4) ◽  
pp. 732-738 ◽  
Author(s):  
B. Mario Pinto ◽  
Jesus Sandoval-Ramirez ◽  
R. Dev Sharma ◽  
Anthony C. Willis ◽  
Frederick W. B. Einstein
Keyword(s):  
Molecular Structure ◽  
Nuclear Magnetic Resonance ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Axial Orientation ◽  
Monoclinic Space Group ◽  
Crystallographic Investigation ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The synthesis of 2-(4-methoxyphenylseleno)-1,3-dithiane 3 and 2-(4-trifluoromethylphenylseleno)-1,3-dithiane 5 from 2-chloro-1,3-dithiane 1 and the corresponding sodium arylselenolates is described. Nuclear magnetic resonance spectroscopic investigation of the products indicates that the compounds exist predominantly in a conformation in which the arylseleno moiety adopts an axial orientation. X-ray crystallographic investigation indicates that the 1,3-dithiane ring exists in the chair conformation with the arylseleno moiety in the axial orientation. Compound 3 is orthorhombic, space group P212121 with a = 5.449(2) Å, b = 9.217(2) Å, c = 24.860(3) Å, V = 1248.5 Å3, Z = 4. The structure was refined to R = 0.038 for 689 reflections with I > 2.3σ(I). Compound 5 is monoclinic, space group C2/c, with a = 28.628(7) Å, b = 5.246(2) Å, c = 21.342(5) Å, β = 121.12(1)°, V = 2743.8 Å3, Z = 8. Its structure refined to R = 0.064 for 966 reflections with I > 2.3σ(I).

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.

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.

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°).

The Crystal and Molecular Structure of Chloro-mer-Tris(dimethylphenylphosphine)-cis-dihydridoiridium(III) by X-Ray and Neutron Diffraction

1988 ◽  
Vol 41 (5) ◽  
pp. 641 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Molecular Structure ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Neutron Data ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The structure of mer-(Pme2Ph)3Cl-cis-H2IrIII (1) has been determined by single-crystal X-ray and neutron diffraction analyses. Crystals are monoclinic, space group P21, with a 11.476(4), b 14.069(5), c 8.286(3)Ǻ, β 92.45(1)° and Z 2. Full-matrix least-squares analyses converged 0.022 for 7773 X-ray data and R(F2) = 0.062 for 1538 neutron data. Ir -H [1.557(11)Ǻ trans to Cl, 1.603(10) Ǻ trans to P] and Ir -P distances [2.292(1)Ǻ trans to P, 2.328(1)Ǻ trans to H] both exhibit trans lengthening effects. Consistent with the increased hydride content the Ir -P distances in (1) are c. 0.04 Ǻ shorter than for the corresponding bonds in its dichloro monohydrido analogues and c. 0.08 Ǻ shorter than those in the trichloride . In contrast Ir-Cl [2.505(1)Ǻ] is not significantly different to the corresponding distance (2.504 Ǻ av.) in mer -(PMe2Ph)3-cis-Cl2HIrIII.

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.

Adiponitrile at 100 K

2017 ◽  
Vol 73 (11) ◽  
pp. 937-940 ◽  
Author(s):  
Rüdiger W. Seidel ◽  
Richard Goddard ◽  
Nils Nöthling ◽  
Christian W. Lehmann
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Low Temperature ◽  
Single Crystal ◽  
Large Scale ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Intermolecular Contacts

Adiponitrile, C6H8N2, is a key intermediate in the synthesis of the polyamide Nylon 66 and is produced industrially on a large scale. We have determined the crystal and molecular structure of adiponitrile by single-crystal X-ray analysis at 100 K, a suitable crystal (m.p. 275 K) having been grown from the melt at low temperature. The compound crystallizes in the monoclinic space group P21/c with Z = 2. In the crystal structure, the molecule adopts an exact C i-symmetric gauche–anti–gauche conformation of the C—C—C—C skeleton about an inversion centre. The molecules are densely packed, with short intermolecular contacts between the α-H and nitrile N atoms.

Synthesen, Kristall- und Molekülstruktur ionischer Nickel-Komplexe mit Phosphanen im kationischen und anionischen Komplex-Teil / Syntheses, Crystal and Molecular Structure of Ionic Nickel Complexes with Phosphanes in the Cationic and Anionic Part

1985 ◽  
Vol 40 (3) ◽  
pp. 357-362 ◽  
Author(s):  
Maria Brenndörfer ◽  
Hans Albert Brune ◽  
Tony Debaerdemaeker ◽  
Reinhard Hemmer
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Nickel Complexes ◽  
Lattice Parameters ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Anionic Part

The syntheses of five new nickel-II-complexes of the type [HPR′3][R3PNiCl3] (R,R′ = C6H5, n-C4H9, C6H11 , C5H9 and R = C6H5, R′ = C6H11) are described.The structure of the compound [HP(C6H11)3][(C6H5)3PNiCl3] was determined by X-ray analysis. The crystals are monoclinic; space group P21/n with the lattice parameters a = 18.180(5), b = 18.842(4), c = 11.173(3) Å and β = 107.12(6)°; Z = 4.

The reaction of tetrasulphur dinitride with norbornadiene; the crystal and molecular structure of S4N2•C7H8, an eight-membered C2S4N2 heterocycle

1983 ◽  
Vol 61 (6) ◽  
pp. 1185-1188 ◽  
Author(s):  
Hans Koenig ◽  
Richard T. Oakley ◽  
A. Wallace Cordes ◽  
Mark C. Noble
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reaction of tetrasulphur dinitride with norbornadiene produces the 1:1 adduct S4N2•C7H8; X-ray crystallographic analysis of this compound reveals that olefin addition cleaves one of the sulphur–sulphur bonds of S4N2, yielding a novel eight-membered C2S4N2 ring. Crystals of S4N2•C7H8 are monoclinic, space group P21/c, a = 6.127(1), b = 17.369(1), c = 9.580(1) Å, β = 106.74(1)°, V = 1003.8(5) Å3Z = 4. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.039. The S—S—N—S—N—S fragment of the C2S4N2 ring is planar to within 0.15 Å. The S—C—C—S unit is folded out of this plane to produce a dihedral angle of 74.5°.

scholarly journals cis-Dichloro-(1 ,5-bisdiphenylphosphanopentane)platinum(II). Synthese, Krystall– und Molekülstruktur / cis-Dichloro-(1 ,5-bisdiphenylphosphanopentane)platinum(II). Synthesis, Crystal and Molecular Structure

1981 ◽  
Vol 36 (9) ◽  
pp. 1125-1129 ◽  
Author(s):  
Heinz-Peter Klein ◽  
Ulf Thewalt ◽  
Heinz Zettlmeißl ◽  
Hans Albert Brune
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Lattice Parameters ◽  
High Yield ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

Abstract The title compound has been prepared in high yield from K2[PtCl4] and 1,5-bis(diphenylphosphano) pentane in dry CH2Cl2. The crystals are monoclinic, space group P21/c with lattice parameters a = 11.733(3), b = 17.229(5), c = 13.743(4) Å, and β= 92.37(3)°; Z = 4. An X-ray analysis shows that the complex is monomeric and that it has a planar cis-configuration.

Die Kristall- und Molekülstruktur von Lithiumtrifluormethansulfonat Li[SO3CF3] · (THF) / The Crystal and Molecular Structure of Lithiumtrifluoromethanesulphonate Li[SO3CF3] · (THF)

1990 ◽  
Vol 45 (9) ◽  
pp. 1304-1308 ◽  
Author(s):  
H. Schumann ◽  
J. A. Meese-Marktscheffel ◽  
J. Loebel
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Oxygen Atoms

The title compound 1 crystallizes in the monoclinic space group P21/c with a = 1023.4(1), b = 985.4(1), c = 1915.3(4) pm, β = 97.73(1)°, V = 1914.9·10-30 m3 and Z = 8. The X-ray structure was solved from 1977 observed reflections with I > 6σ(I) and refined to a final R value of 0.044. The structure shows Li tetracoordinated by one THF-oxygen and by three oxygen atoms each belonging to a different SO3CF3 group.

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