Arsenic(III), Antimony (III) and Bismuth(III) Thiobenzoates: Crystal and Molecular Structures of M(SOCR)3 and PhSb(SOCPh)2

1998 ◽  
Vol 53 (12) ◽  
pp. 1475-1482 ◽  
Author(s):  
Prit Singh ◽  
Sudha Singh ◽  
Vishnu D. Gupta ◽  
Heinrich Nöth
Keyword(s):  
Crystal Structure ◽  
Molecular Structures ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Covalently Bonded ◽  
Bismuth Complex ◽  
Group 15 ◽  
Structure Determinations ◽  
Trigonal Pyramid ◽  
Trigonal Prisms

Abstract Tris-thiobenzoates, Arsenic, Antimony, Bismuth Tris-thiobenzoates of arsenic, antimony and bismuth, M(SOCR)3 have been obtained from their oxides and characterized. In the X-ray crystal structure determinations of these, the group 15 atom and the three covalently bonded sulfur atoms are found to constitute a trigonal pyramid, the central atoms lie at a C3 axis. In the bismuth complex the thiobenzoate ligand tends to chelate. However, three comparatively short intermolecular M···S interactions are significant features for these molecules resulting in stacking of trigonal prisms providing an essentially six coordinate environment around arsenic and antimony and a nine-coordinate one for bismuth. The structure of PhSb(SOCPh)2 can be considered

Single-crystal X-ray structure determinations of vardenafil, vardenafil dihydrate, vardenafil monohydrochloride trihydrate and vardenafil dihydrochloride hexahydrate

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Dedong Wu ◽  
Faraj Atassi
Keyword(s):  
Crystal Structure ◽  
Synchrotron Radiation ◽  
Single Crystal ◽  
Molecular Structures ◽  
Free Base ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Structure Determinations ◽  
Good Agreement

AbstractThe crystal and molecular structures of vardenafil (free, unprotonated base), vardenafil dihydrate and the hydrochloride salts, vardenafil monohydrochloride trihydrate and vardenafil dihydrochloride hexahydrate, were determined by single-crystal X-ray diffraction. The crystal structure of vardenafil monohydrochloride trihydrate is in good agreement with the published crystal structure obtained by powder diffraction using synchrotron radiation. This work shows that the crystal structure of anhydrous vardenafil free base is very similar to the crystal structure of sildenafil free base.

Untersuchungen an Stickstoff-Brom-Verbindungen, IV / Studies on Nitrogen-Bromine Compounds, IV

1977 ◽  
Vol 32 (12) ◽  
pp. 1416-1420 ◽  
Author(s):  
Omar Jabay ◽  
Hans Pritzkow ◽  
Jochen Jander
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Analysis ◽  
Electron Acceptors ◽  
Molecular Structures ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Solid Nitrogen ◽  
Intermolecular Contacts

The crystal and molecular structures of N-bromobenzamide (NBB), N-bromosuccinimide (NBS), and N,N-dibromobenzenesulfonamide (NBBS) were determined by X-ray structure analysis. The nitrogen atoms in NBB and NBS have a trigonal planar coordination (sp2) and the N—Br distances lie in the same range (1.82 A, 1.84 A). The N—Br distance in NBBS, where the nitrogen atom is sp3-hybridized, is somewhat longer (1.88 A). In these structures the molecules are connected by O···H—N (NBB), O···Br—N (NBS) or N···Br—N (NBBS) intermolecular bonds forming endless chains; positivated hydrogen atoms or, in case that they are absent, positivated bromine atoms act as electron acceptors with oxygen or sp3- hybridized nitrogen atoms. These results suggest, that in solid nitrogen tribromide, the crystal structure of which cannot be determined, the nitrogen atoms will be sp3-hybridized and intermolecular contacts via N—Br···N will occur.

scholarly journals Crystal and molecular structures of some phosphane-substituted cymantrenes [(C5H4 X)Mn(CO)LL′] (X = H or Cl, L = CO, L′ = PPh3 or PCy3, and LL' = Ph2PCH2CH2PPh2)

2021 ◽  
Vol 77 (10) ◽  
Author(s):  
Karlheinz Sünkel ◽  
Christian Klein-Hessling
Keyword(s):  
Crystal Structure ◽  
Uv Irradiation ◽  
Molecular Structures ◽  
Bond Lengths ◽  
Crystal And Molecular Structures ◽  
Chlorine Substitution ◽  
Small Influence ◽  
Intermolecular Association ◽  
Structure Determinations

UV irradiation of tetrahydrofuran solutions of [CpMn(CO)3] (Cp = π-C5H5 or π-C5H4Cl) in the presence of the phosphanes PPh3 or PCy3 (Cy = cyclohexyl) and Ph2PCH2CH2PPh2 yields the substitution products [CpMn(CO)2PR 3] (R = Ph or Cy) and [CpMn(CO)(Ph2PCH2CH2PPh2)], namely, dicarbonyl(η5-cyclopentadienyl)(triphenylphosphane-κP)manganese(I), [Mn(C5H5)(C18H15P)(CO)2], 1a, dicarbonyl(η5-1-chlorocyclopentadienyl)(triphenylphosphane-κP)manganese(I), [Mn(C5H4Cl)(C18H15P)(CO)2], 1b, dicarbonyl(η5-cyclopentadienyl)(tricyclohexylphosphane-κP)manganese(I), [Mn(C5H5)(C18H33P)(CO)2], 2a, dicarbonyl(η5-1-chlorocyclopentadienyl)(tricyclohexylphosphane-κP)manganese(I), [Mn(C5H4Cl)(C18H33P)(CO)2], 2b, carbonyl(η5-cyclopentadienyl)[1,2-bis(diphenylphosphanyl)ethane-κ2 P,P′]manganese(I), [Mn(C5H5)(C26H24P2)(CO)], 3a, and carbonyl(η5-1-chlorocyclopentadienyl)[1,2-bis(diphenylphosphanyl)ethane-κ2 P,P′]manganese(I), [Mn(C5H4Cl)(C26H24P2)(CO)], 3b, The crystal structure determinations show a very small influence of the chlorine substitution and a moderate influence of the phosphane substitution on the bond lengths. The PR 3 groups avoid being eclipsed with the C—Cl bonds. All the compounds employ weak C—H...O interactions for intermolecular association, which are enhanced by C—H...Cl contacts in the chlorinated products.

Synthese und Kristallstruktur von Iodmethyltriphenylphosphonium-iodid (C6H5)3PCH2I+I- / Synthesis and Crystal Structure of Iodomethyltriphenylphosphonium Iodide (C6H5)3PCH2I+I-

1993 ◽  
Vol 48 (12) ◽  
pp. 1760-1766 ◽  
Author(s):  
H. Vogt ◽  
K. Lauritsen ◽  
L. Riesel ◽  
M. von Löwis ◽  
G. Reck
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Colourless Needle ◽  
Molecular Structures ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Mndo Calculations ◽  
Good Agreement

Iodomethyltriphenylphosphonium iodide, (C6H5)3PCH2I+I-, has been prepared by the reaction of (C6H5)3P with CH2I2 in dichloromethane forming colourless needle like crystals. The crystal and molecular structures have been determined by an X-ray structure analysis. The crystals are orthorhombic, space group Pca21, Z = 8; a = 1478,8(3) pm, b = 1249,3(3) pm, c = 2053,2(3) pm. R = 0.050 for 3219 observed reflections with I ≥ 2 σ(Ι). In the solid state the title compound exists as two discrete monomeric units, (C6H5)3PCH2I+I-. In both symmetry independent units the I-I distances are surprisingly short with 346,5(1) pm and 356,3(1) pm. For the title compound the results of AM 1, PM 3, and MNDO calculations are in good agreement with corresponding values determined by the X-ray analysis.

Crystal and Molecular Structures of the Sulfurization and Selenation Products of Bis[bis(trimethylsilyl)amino]germanium(II). Crystal Structure of (Triphenylphosphine)gold(I) Bis(trimethylsilyl)amide

2000 ◽  
Vol 55 (5) ◽  
pp. 347-351 ◽  
Author(s):  
Gerald L. Wegner ◽  
Alexander Jockisch ◽  
Annette Schier ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Elemental Sulfur ◽  
Crystal Structure Analysis ◽  
Molecular Structures ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Planar Configuration ◽  
High Yields ◽  
Single Crystal Structure Analysis

Treatment of bis[bis(trimethylsilyl)amino]germanium(II) with elemental sulfur or selenium affords high yields of the corresponding monosulfide [(Me3Si)2N]2GeS and selenide [(Me3Si)2N]2GeSe, respectively. The crystalline products have now been shown to be cyclic dimers with (GeS/Se)2 four-membered rings by X-ray single crystal structure analysis. The crystal structure of (triphenylphosphine)gold(I) bis(trimethylsilyl)amide (Ph3P)Au-N(SiMe3)2 has also been determined. The molecule is a monomer with a tricoordinate nitrogen atom in a planar configuration [Si2NAu]. The compound does not undergo insertion of the bis[bis(trimethylsilyl)amino]germylene.

The synthesis, crystal and molecular structures of triphenyl(phenylthio)silane, Ph3SiSPh, and of bis(μ-thiophenolato)bis[tetracarbonyltungsten(I)], [W(CO)4(SPh)]2

1987 ◽  
Vol 65 (4) ◽  
pp. 898-902 ◽  
Author(s):  
C. Robert Lucas ◽  
Michael J. Newlands ◽  
Eric J. Gabe ◽  
Florence L. Lee
Keyword(s):  
Bond Length ◽  
Phenyl Ring ◽  
Close Approach ◽  
Molecular Structures ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Structure Determinations

Preparations and X-ray structure determinations are described for Ph3SiSPh and [W(CO)4(μ-SPh)]2. The compound Ph3SiSPh crystallizes in space group Pcab with a = 15.260 Å, b = 15.968 Å, c = 16.757 Å, Z = 8, dcalc = 1.20 g cm−3 (MoKα1, λ = 0.70930 Å). The structure was solved with MULTAN and refined to the final R = 0.050 for 1933 significant reflections. The molecule has an unusual C—S—Si angle of 99.5° and a short Si—S bond length of 2.156 Å. The compound [W(CO)4(μ-SPh)]2 crystallizes in the space group P21/c with a = 9.164 Å, b = 12.054 Å, c = 11.163 Å, β = 111.63°, Z = 2, dcalc = 2.35 g cm−3 (MoKα1, λ = 0.70930 Å). The structure was solved with MULTAN and refined to the final R = 0.062 for 2748 significant reflections. The molecule is a dimer with a crystallographic center of symmetry. There is a short W—W distance (2.972 Å), a wide S—W—S′ angle (106.3°), a compressed W—S—W′ angle (73.67°) and there is distortion of a CO on each W due to the close approach of an ortho-H in a phenyl ring.

Convenient synthesis, X-ray crystal structure, and Raman spectrum of the heptasulphide dianion, S72−, in [PPN]2S7•2EtOH

1986 ◽  
Vol 64 (8) ◽  
pp. 1509-1513 ◽  
Author(s):  
Tristram Chivers ◽  
Frank Edelmann ◽  
John F. Richardson ◽  
Kenneth J. Schmidt
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Molecular Structures ◽  
High Yield ◽  
Torsion Angles ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Convenient Synthesis ◽  
Stretching Vibrations

The S72− ion is readily prepared in high yield by the reaction of [PPN]SH with cyclo-S8 in ethanol. The crystal and molecular structures of [PPN]2S7•2EtOH have been determined by X-ray crystallography. The crystals are monoclinic and belong to the space group P21, a = 13.199(2), b = 19.414(2), c = 14.046(2) Å, β = 94.027(6)°, V = 3590.3(7) Å3, Z = 2. The final R and Rw values were 0.064 and 0.060, respectively. The S72− ion is an unbranched chain of sulphur atoms in the cis,trans,cis-configuration with torsion angles of 89.99(18), 71.84(16), 76.54(16), and 94.19(18)°. The S—S distances (in Å) become progressively smaller in the sequence d(S—S central) [2.072(3) and 2.070(3)] > d(S—S internal) [2.050(2) and 2.037(3)] > d(S—S) terminal [2.044(3) and 2.026(4)]. The Raman spectrum of the S72− ion in [PPN]2S7•2EtOH exhibits characteristic S—S stretching vibrations at 503, 453, 419, and 395 cm−1.

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