scholarly journals The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

1996 ◽  
Vol 74 (9) ◽  
pp. 1671-1681 ◽  
Author(s):  
Jack Passmore ◽  
Paul D. Boyle ◽  
Gabriele Schatte ◽  
Todd Way ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Ft Raman Spectroscopy ◽  
New Phase ◽  
Ft Raman

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

The preparation, X-ray crystal structure, and spectroscopic characterization of pentafluorophenyl-bis(pentafluorophenylthio)sulfonium hexafluoroarsenate, [(C6F5S)2SC6F5][AsF6]

1998 ◽  
Vol 76 (7) ◽  
pp. 1050-1059 ◽  
Author(s):  
Scott Brownridge ◽  
T Stanley Cameron ◽  
Jack Passmore ◽  
Gabriele Schatte ◽  
George W Sutherland
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Room Temperature ◽  
Spectroscopic Characterization ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Ft Raman Spectroscopy ◽  
Ft Raman

Pentafluorophenyl-bis(pentafluorophenylthio)sulfonium hexafluoroarsenate, [(C6F5S)2SC6F5][AsF6], was prepared by the reaction of (C6F5)2S2 and AsF5 in liquid SO2 at room temperature. The compound has been characterized by single-crystal X-ray and powder diffraction, and IR and FT-Raman spectroscopy. Crystals of [(C6F5S)2SC6F5][AsF6] are orthorhombic, space group P212121 (cell dimensions measured at room temperature in brackets): a = 13.132(3) [13.157(2)] Å, b = 21.477(4) [21.575(3)] Å, c = 8.770(2) [8.775(1)] Å, α = ß = γ = 90.00°; V = 2473.3(9) Å3, Z = 4, temperature = 181 ± 1 K. The structure consists of [AsF6]- anions and [(C6F5S)2SC6F5]+ cations that have a different structure than the related [X2MMMX]+ cations (M = S, Se; X = Cl, Br), which contain a trichalcogen chain with a pronounced chalcogen-chalcogen bond alternation. Ab initio calculations suggest the observed [(C6F5S)2SC6F5]+ geometry is due to steric and solid state effects. Comparison of the Raman spectra of [(C6F5)S2SC6F5][AsF6], [Cl2SSSCl][AsF6], and [(CH3)2ClS3]+ implies that [(CH3)2ClS3]+ has a structure with equal sulfur-sulfur distances, and therefore the structure is likely [(CH3S)2SCl]+ and probably not the previously reported [(CH3)2SSSCl]+.Key words: [R3X3]+ cations, X-ray crystal structure, FT-Raman spectroscopy, [(C6F5S)2SC6F5]+, pentafluorophenyl-bis(pentafluorophenylthio)sulfonium cation, hexafluoroarsenate.

FT Raman Spectroscopy as a Tool for Characterization of Derivatized Silica Gel Sorbents

2005 ◽  
Vol 70 (2) ◽  
pp. 168-177
Author(s):  
Zuzana Tománková ◽  
Pavel Matějka ◽  
Karel Volka ◽  
Vladimír Král
Keyword(s):  
Raman Spectroscopy ◽  
Silica Gel ◽  
Stationary Phases ◽  
Amide Bonds ◽  
Raman Spectroscopic ◽  
Ft Raman Spectroscopy ◽  
Trimethylsilyl Groups ◽  
Ft Raman

The potential of Fourier-transform (FT) Raman spectroscopy for verification of individual steps of synthesis of new chromatographic stationary phases was studied. 3-Aminopropylated silica gel was modified with two different optically active compounds ((+)-cloprostenol, (+)-(R)-2,2'-dihydroxy-1,1'-binaphthalene-3-carboxylic acid) via amide bonds. In the next step, free silanol groups were protected with trimethylsilyl groups. The FT Raman spectroscopic results compared with the data obtained by elemental analysis enable not only qualitative verification of synthetic steps, but also a semiquantitative determination of covering of the silica gel surface by derivatization agent.

The use of NIR-FT-Raman spectroscopy for the characterization of polymer-supported reagents and catalysts

Tetrahedron ◽  
2001 ◽  
Vol 57 (41) ◽  
pp. 8675-8683 ◽  
Author(s):  
B Altava ◽  
M.I Burguete ◽  
E Garcı́a-Verdugo ◽  
S.V Luis ◽  
M.J Vicent
Keyword(s):  
Raman Spectroscopy ◽  
Ft Raman Spectroscopy ◽  
Polymer Supported ◽  
Ft Raman

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

A synergic approach of X-ray powder diffraction and Raman spectroscopy for crystal structure determination of 2,3-thienoimide capped oligothiophenes

2018 ◽  
Vol 20 (5) ◽  
pp. 3630-3636 ◽  
Author(s):  
C. Cappuccino ◽  
P. P. Mazzeo ◽  
T. Salzillo ◽  
E. Venuti ◽  
A. Giunchi ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Powder Diffraction ◽  
Structure Determination ◽  
Molecular Conformation ◽  
Rapid Identification ◽  
Crystal Structure Determination ◽  
X Ray

This work presents a Raman based approach for the rapid identification of the molecular conformation in a series of new 2,3-thienoimide capped quaterthiophenes.

scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse polymerer 1:1-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen / Crystal Growth in Gels and X-Ray Characterization of Polymeric 1:1-Complexes of CuBr2 and CuCl2 with Pyrazine

1989 ◽  
Vol 44 (5) ◽  
pp. 553-556 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Growth ◽  
Chloro Complex ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Linear Chains

Single crystals of Cu(pz)Br2 and Cu(pz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a = 1239.2(3) pm, b = 685.9(2) pm, c = 390.7(3) pm, β = 96,23(5)°. Crystal data for the chloro-complex: monoclinic, space group C2/m with a = 1197.1(3) pm, b = 684.9(3) pm, c = 370.1(3) pm, β = 95.96(5)°. Crystal structure analyses reveal that CuHal2 molecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atoms.

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