Syntheses, Structures and Vibrational Spectra of Some Dimethyl Sulfoxide Solvates of Bismuth(III) Bromide and Iodide

1998 ◽  
Vol 51 (4) ◽  
pp. 285 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Jack M. Harrowfield ◽  
Peter C. Junk ◽  
Brian W. Skelton ◽  
Allan H. White

Room-temperature single-crystal X-ray studies are recorded for some dimethyl sulfoxide (dmso) solvates of bismuth(III) bromide and iodide. Colourless BiBr3.3dmso is triclinic, P-1, a 8·467(4), b 9·109(4), c 13·901(4) Å, α 76·34(4), β 76·95(4), γ 64·56(4)°, Z = 2; conventional R on |F| was 0·050 for No 2306 independent ‘observed’ (I > 3σ(I)) reflections. The complex is mononuclear with a quasi-octahedral fac-bismuth environment, [(dmso-O)3BiBr3], isomorphous with the previously determined chloride. Orange BiI3-2dmso is triclinic, P-1, a 12·558(2), b 8·962(2), c 8·342(1) Å, α 61·85(1), β 78·27(1), γ 76·89(2)°, Z = 2 f.u., R 0·048 for No 1953. The complex is binuclear, a pair of iodide atoms bridging the two bismuth atoms, [(dmso-O)2I2Bi(µ-I)2BiI2(O-dmso)2]; the two O-dmso ligands about each six-coordinate bismuth lie trans. Red BiI3.2 ⅔ dmso is triclinic, P-1, a 16·435(6), b 14·926(2), c 12·396(3) Å, α 74·89(2), β 73·24(2), γ 79·18(2)°, Z = 6, R 0·059 for No 5858. The complex is [Bi(O-dmso)8] [Bi2I9], the eight-coordinate metal environment of the cation being, unusually, dodecahedral; in the anion a pair of quasi-octahedral six-coordinate bismuth atoms are bridged by three iodides, [I3Bi(µ-I)3BiI3]3-. Bands in the far-infrared and Raman spectra due to the v(BiX) modes are assigned and discussed in relation to the structures of the complexes. The assignment of the v(BiO) modes is discussed.


1998 ◽  
Vol 51 (4) ◽  
pp. 311 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Jack M. Harrowfield ◽  
Aaron M. Lee ◽  
Brian W. Skelton ◽  
Allan H. White

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for the title compounds, [bpyH]+[(bpy)BiX4]-, X = Cl, Br, the chloride being obtained in a second acetonitrile- sesquisolvated form. [bpyH]+[(bpy)BiX4]-, X = Cl, Br, are isomorphous, monoclinic C2/c, a ≈ 15·3, b ≈ 9·6, c ≈ 16·8 Å, β 109°, Z = 4, conventional R on |F| being 0·056, 0·059 for No 1456, 769 independent ‘observed’ (I > 3σ(I)) reflections respectively. [bpyH] [(bpy)BiCl4].1½MeCN is monoclinic, P21/m, a 9·572(2), b 34·521(8) c 8·218(2) Å, β 102·13(2)°, Z = 4, R 0·043 for No 2635. All anionic species are mononuclear, the bismuth being quasi-octahedral. Bands in the far-infrared and Raman spectra due to the vibrations of the N2BiCl4 core in [(bpy)BiCl4]- are assigned, and their relationship to the vibrations of [BiCl6]3- is discussed.



1973 ◽  
Vol 51 (3) ◽  
pp. 402-404 ◽  
Author(s):  
A. Bree ◽  
R. A. Kydd ◽  
V. V. B. Vilkos ◽  
R. S. Williams

A study of the polarized infrared and Raman spectra of acenaphthylene single crystals has been made. These results, together with Gordon and Yang's preliminary X-ray work, suggest that the molecules pack in some disordered arrangement in the solid at room temperature. Most of the A1 fundamentals were identified in the Raman solution spectrum from their low depolarization ratio, and a few tentative assignments of nontotally symmetric fundamentals were made.



2003 ◽  
Vol 2003 (8) ◽  
pp. 518-521 ◽  
Author(s):  
M.K. Marchewka

Room temperature powder infrared and Raman measurements for the new melaminium salt, bis(2,4,6-triamino-1,3,5-triazin-1-ium) sulfate dihydrate, 2C3H7N6+·SO42-·2H2O, in the crystalline state, were carried out. The vibrational spectra in the region of internal vibrations of the ions corroborate recent X-ray data of Janczak et al. Some spectral features of this new crystal are referred to those of other crystalline melaminium salts.



1984 ◽  
Vol 39 (4) ◽  
pp. 357-361 ◽  
Author(s):  
Robert Becker ◽  
Wolfgang Brockner ◽  
Herbert Schäfer

Pb2P2Se6 crystallizes in the monoclinic system, space group Pn (No. 13) with the lattice constantsa = 974.2 (4) pm. b = 766.2 (3) pm. c = 689.8 (3) pm, β=91.44(5)°.The title compound is isotypic to the homologous Pb2P2S6. In the structure there are discrete P2Se4-6 anions.Far infrared, infrared and Raman spectra of this compound have been recorded. The observed frequencies are assigned on the basis of P2Se4-6 units with C2h symmetry in the crystal. DTA-data have been determined and interpreted.



1983 ◽  
Vol 38 (5) ◽  
pp. 555-558 ◽  
Author(s):  
Robert Becker ◽  
Wolfgang Brockner ◽  
Claus Wibbelmann

Far infrared, infrared and Raman spectra of tin hexathiohypodiphosphate Sn2P2S6 (mono­clinic modification II) have been recorded. The observed frequencies are assigned on the basis of P2S64-units with C2h symmetry in the crystal. The assignment is supported by the correlation D3d (dissolved P2S64- ion) → C2h. DTA-data have been determined and interpreted.



1986 ◽  
Vol 41 (8) ◽  
pp. 958-970 ◽  
Author(s):  
Ralf Steudel ◽  
Jürgen Steidel ◽  
Torsten Sandow

AbstractThe homocyclic S11 and S13 molecules have been synthesized from titanocenepentasulfide and S6Cl2 or S8Cl2, respectively, and obtained as yellow crystals which are metastable for several days at 20 °C. X-Ray structural analyses of single crystals at -105± 5 °C exhibited molecules of approximately C2 symmetry with bond distances (d), bond angles (a) and torsional angles (r) in the following ranges: S11 : d = 203.2 -211.0 pm, α = 103.3-108.6°, τ = 69.3 - 140.5°; S13: d = 197.8 - 211.3 pm, α = 102.8-111.1°, τ = 29.5 - 116.3°. Infrared and Raman spectra of S11 and S13 are reported. In addition, the synthesis of S6Cl2 and S8Cl2 from S6 or S8, respectively, and chlorine is described.



1996 ◽  
Vol 49 (9) ◽  
pp. 997 ◽  
Author(s):  
LI Semenova ◽  
BW Skelton ◽  
AH White

Adducts [( dmso )nLn(O2NO)3], obtained by the crystallizatior , of lanthanoid (III) nitrate ( Ln (NO3)3.-xH2O) with excess dimethyl sulfoxide (' dmso ') in methanol or ethanol, have been the subject of a series of room-temperature single-crystal X-ray studies, defining more clearly the manner in which stoichiometry and structure systematically vary with change in metal ion radius. All complexes studied are mononuclear, the metal ion being complexed by three bidentate nitrate ligands and a number of dmso ligands , four for La-Sm and three beyond. The array La- Sm is monoclinic C2/c, a ≈ 14.9, b ≈ 15.5, c ≈ 15.5 Ǻ, β ≈ 108.4°, Z = 4 f.u .; the metal atom is disposed on a crystallographic 2 axis, which also passes through one of the nitrate groups. The series Eu -Tm (inclusive also of Y) is monoclinic, P21/n, a ≈ 11.5, b ≈ 12.7, c ≈ 13.6 Ǻ, β ≈ 100°, Z = 4 f.u ., while Yb and Lu are also monoclinic, P21/c, a ≈ 10.0, b ≈ 12.6, c ≈ 16 Ǻ, β ≈ 100.6°, Z = 4 f.u.



1983 ◽  
Vol 61 (10) ◽  
pp. 2282-2284 ◽  
Author(s):  
A. Agarwal ◽  
D. P. Khandelwal ◽  
H. D. Bist

The far infrared and Raman spectra of polyerystalline lithium formate monohydrate and the Rayleigh wing scattering of its aqueous solutions are reported. Three new bands in solid and bands due to librations of HCOO− and the quasi-tetrahedral structure of water in solutions have been identified.



1977 ◽  
Vol 55 (18) ◽  
pp. 3218-3226 ◽  
Author(s):  
Arlen Viste ◽  
Donald E. Irish

Raman and infrared spectra have been recorded for polycrystalline samples of TIClO3, TIBrO3, and T1IO3 at room temperature. The vibrational spectra of these rhombohedral (R3m, C3v5) crystals are closely related to each other, and to single crystal Raman spectra of isomorphous RbClO3 and KBrO3 reported by others. Spectral assignments are made. The uni-molecular unit cell yields no correlation field splitting, but lack of a center of inversion leads to TO/LO splitting of each active mode in these uniaxial piezoelectric crystals. Relationships between the thallium(I) halates and the NaN3 and MXY3 perovskite structures are considered.





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