Single-crystal structure and 5.0.deg.K polarized electronic spectra of bis(monothioacetylacetonato)nickel(II). Far-infrared and Raman spectra of bis(monothioacetylacetonato)metal(II) complexes

1974 ◽  
Vol 96 (8) ◽  
pp. 2353-2359 ◽  
Author(s):  
Olavi Siiman ◽  
Donald D. Titus ◽  
Charles D. Cowman ◽  
James Fresco ◽  
Harry B. Gray

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 (8) ◽  
pp. 874-879 ◽  
Author(s):  
Robert Becker ◽  
Wolfgang Brockner ◽  
Herbert Schäfer

Abstract Pb2P2S6 crystallizes in the monoclinic system, space group Pn with the lattice constants a = 940.2(4) pm, b= 746.6(3) pm, c = 661.2(3) pm, β = 91.53(5)°. The compound is isotypic to the monoclinic modification II of Sn2P2S6 . In the structure there are discrete P2S4-6 -anions.Far infrared, infrared and Raman spectra of this compound have been recorded. The observed frequencies are assigned on the basis of P2S4-6 units with C2h symmetry in the crystal. DTA-data have been determined and interpreted.



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.



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.



2016 ◽  
Vol 71 (4) ◽  
pp. 327-332 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo

AbstractTransparent colorless crystals of NaA5[C6N9]2 · 4 H2O (A = Rb, Cs) were obtained by blending aqueous solutions of Na3[C6N9] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group P21/m (no. 11) with the cell parameters a = 815.56(16), b = 1637.7(4) and c = 1036.4(3) pm, and β = 110.738(12)° for NaRb5[C6N9]2 · 4 H2O and a = 843.32(6), b = 1708.47(11) and c = 1052.42(7) pm, and β = 112.034(2)° for NaCs5[C6N9]2 · 4 H2O, respectively. Raman spectra of the title compounds complement our results.



1983 ◽  
Vol 38 (12) ◽  
pp. 1575-1580 ◽  
Author(s):  
Claus Wibbelmann ◽  
Wolfgang Brockner ◽  
Brigitte Eisenmann ◽  
Herbert Schäfer

Tl2P2S6 crystallizes in the orthorhombic system, space group Immm, Z = 2 with the lattice constantsa = 793.2(4) pm, b = 689.2(4) pm, c = 901.9(5) pm.In the structure there are discrete P2S62- -anions. The P2S62- -ion was found to be a hexa-thiometadiphosphate group where the two P atoms are linked by two S bridges.Far infrared, infrared and Raman spectra of this compound have been recorded. The observed frequencies are assigned on the basis of P2S62- units with D2h symmetry in analogy to the isoelectronic Al2Cl6



2010 ◽  
Vol 65 (12) ◽  
pp. 1409-1415 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. Di Salvo

Single crystals of Ca15(CBN)6(C2)2F2 were obtained by the reaction of graphite, hexagonal BN and CaF2 with an excess of distilled Ca metal in silica-jacketed Ta ampoules at 1300 K. The title compound is transparent red and crystallizes isopointal to Ca15(CBN)6(C2)2O adopting the cubic space group Ia 3̄d (no. 230, Z = 8) with the cell parameter a = 1653.6(4) pm. Its vibrational spectra are compared with IR and Raman data of similar compounds from the literature and with the newly measured Raman spectra of Ca5(BC2)(C2)Cl3 and Ca9(BC2)2Cl8.



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