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.

3(5),4-Dimethyl- and 3,4,5-trimethylpyrazole at 200 K. X-ray crystallography and quantum-chemical analysis

1999 ◽  
Vol 55 (3) ◽  
pp. 441-447 ◽  
Author(s):  
Lourdes Infantes ◽  
Concepción Foces-Foces ◽  
Jose Elguero
Keyword(s):  
Quantum Chemical ◽  
Molecular Structures ◽  
Asymmetric Unit ◽  
Quantum Chemical Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Unit Form ◽  
Proton Disorder ◽  
Independent Molecules

The crystal and molecular structures of 3(5),4-dimethylpyrazole, C5H8N2, (I), and of 3,4,5-trimethylpyrazole, C6H10N2, (II), have been determined at 200 K. In (I) the 4,5-dimethylpyrazole tautomer is present in the solid state and the six independent molecules in the asymmetric unit form trimers via NH...N hydrogen bonds related by a pseudo centre of symmetry. The asymmetric unit of (II) contains one and a half molecules: these exhibit NH proton disorder and are hydrogen bonded to each other via their respective NH groups to form chains. Ab initio calculations at HF and B3LYP/6-31G** levels indicate that the 3,4-dimethylpyrazole tautomer is more stable than the 4,5-dimethylpyrazole tautomer by only approximately 0.5  kcal  mol−1 (1 kcal mol−1 = 4.184 kJ mol−1).

Syntheses, Crystal Structures and Electrochemical Properties of Acetylacetonato-Ruthenium Complexes Containing Substituted Pyridine Ligands

2013 ◽  
Vol 68 (9) ◽  
pp. 993-999 ◽  
Author(s):  
Xiuli Wu ◽  
Rufei Ye ◽  
Ai-Quan Jia ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Electrochemical Properties ◽  
Crystal Structures ◽  
Zinc Dust ◽  
Ruthenium Complexes ◽  
Reducing Agent ◽  
Molecular Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Pyridine Ligands

Treatment of Ru(acac)3 with 2-cyano-pyridine and 3,5-dimethyl-pyridine in the presence of zinc dust as reducing agent in refluxing THF afforded the ruthenium(II) complexes cis-[RuII(acac)2(2- CN-py)2] (1) and cis-[RuII(acac)2(3,5-Me2-py)2] (2), respectively. Interaction of Ru(acac)3 with 3- Me-pyridine and 3,5-Me2-pyridine in the presence of Br2 in refluxing THF gave the ruthenium(III) complexes [RuIII(acac)Br2(3-Me-py)2] (3) and [RuIII(acac)Br2(3,5-Me2-py)2] (4), respectively. The four complexes have been spectroscopically and electrochemically characterized, and their crystal and molecular structures have been established by X-ray crystallography

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.

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

scholarly journals Catalytic Efficacy of 2,2′-Bipyridine Cobalt(II) Complex: Hydrothermal Synthesis, X-Ray Structure and Aerobic Epoxidation of Alkenes

2020 ◽  
Vol 33 (1) ◽  
pp. 10-14
Author(s):  
RAJESH BERA
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Atmospheric Pressure ◽  
Active Catalyst ◽  
High Yield ◽  
X Ray ◽  
X Ray Crystallography ◽  
Mononuclear Cobalt ◽  
Epoxidation Of Alkenes ◽  
Acetonitrile Medium

A mononuclear cobalt(II) complex, [Co(bpy)2(NO3)](NO3)·3H2O (1) (bpy = 2,2′-bipyridine) has been synthesized hydrothermally and the crystal structure was characterized by X-ray crystallography. Complex 1 is capable of activating aerobic oxygen at atmospheric pressure. [Co(bpy)2(NO3)](NO3)·3H2O (1) was used as an active catalyst for the aerobic epoxidaion of various alkenes with isobutyraldehyde as co-reductant in acetonitrile medium. Complex 1 catalyzes the epoxidaion reaction efficiently, which reflected in high yield of products with desired selectivity.

Synthesis, Characterization, Crystal Structure and Magnetic Properties of [(en)CuII(ImH)2](ClO4)2 (en = Ethylenediamine, ImH = Imidazole): A Metalloligand as a Building Block for Heterometal Chains

2003 ◽  
Vol 58 (6) ◽  
pp. 505-510 ◽  
Author(s):  
Thorsten Glaser ◽  
Maik Heidemeier ◽  
F. Ekkehardt Hahn ◽  
Tania Pape ◽  
Thomas Lügger
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Building Block ◽  
Exchange Interactions ◽  
High Yield ◽  
Magnetic Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Structural And Electronic Properties ◽  
Dark Blue

The reaction of Cu(ClO4)2·6H2O, imidazole (ImH), and ethylenediamine (en) in a 1 : 2 : 1 ratio afforded in high yield dark-blue single-crystals of [(en)CuII(ImH)2](ClO4)2, 1, which can be used after deprotonation as a building block for heterometallic ferrimagnetic chains. The structural and electronic properties of 1 were examined by X-ray crystallography, FTIR, ESI-MS, electrochemistry, UV/vis/NIR, EPR, and magnetic susceptibility measurements. The structure of 1 exhibits intermolecular π-π interactions and hydrogen bonds but the magnetic data exclude the presence of intermolecular exchange interactions.

Kristall- und Molekülstrukturen von zwei trans-1.2.4.5-Tetraza-3.6-diphospha-cyclohexan-3.6-disulfiden / Crystal and Molecular Structures of Two trans- 1,2,4,5-Tetraza-3,6-diphospha-cyclohexane-3,6-disulfides

1984 ◽  
Vol 39 (3) ◽  
pp. 269-274 ◽  
Author(s):  
Franz Dirschl ◽  
Heinrich Nöth
Keyword(s):  
Chair Conformation ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Torsion Angles ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Twist Conformation

The crystal and molecular structures of two trans-1,2,4,5-tetraza-diphospha-3,6-cyclohexane- 3,6-disulfides, 2 and 3, have been determined by X-ray diffraction methods. The 3,6-diphenyl- 1,2,4,5-tetramethyl-derivative 2 crystallizes in the monoclinic system, space group C He. Its P2N 4 heterocycle adopts a twist conformation. In contrast, the hexamethyl derivative 3 is triclinic, space group P1̅, and its ring shows chair conformation. Torsion angles in these two compounds and similar ones reveal less interaction between lone pairs of electrons on adjacent N-atoms in the chair conformation but stronger interaction of those bound to phosphorus. It is suggested that the latter interaction is responsible for the larger N -P -N bond angle (107°) as compared to the smaller one (101°) in the P2N4 rings present in twist conformation.

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.

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