Synthèses et analyses structurales de perchlorates anhydres d'In(III) et de Tl(III) M(ClO4)3 et ClO2M(ClO4)4; (M = In, Tl)

1985 ◽  
Vol 63 (12) ◽  
pp. 3499-3504 ◽  
Author(s):  
Mohieddine Fourati ◽  
Moncef Chaabouni ◽  
Hassine Ferid Ayedi ◽  
Jean-Louis Pascal ◽  
Jacqueline Potier
Keyword(s):  
Thermal Stability ◽  
Vibrational Spectra ◽  
Dynamic Vacuum ◽  
Polymeric Structure ◽  
Space Group ◽  
Ir And Raman

Reactions of chlorine trioxide (Cl2O6) with anhydrous InCl3, TlCl3, and InCl3•4H2O have been investigated. They give two chloryl perchlorato metallates: ClO2In(ClO4)4 and ClO2Tl(ClO4)4, which can be decomposed on heating (80 °C) under dynamic vacuum. They yield respectively In(ClO4)3 and Tl(ClO4)3. Tl(ClO4)3 appears to have weaker thermal stability than In(ClO4)3, which is stable up to 272 °C; the former decomposes starting at 95 °C to give TlO0.5(ClO4)2. In(ClO4)3 and Tl(ClO4)3 have the same space group [Formula: see text]. The best assignment of their ir and Raman vibrational spectra can be made on the basis of a polymeric structure (Asl3 type) with bridging bidentate perchlorato groups strongly bonded to the metal. The ClO2M(ClO4)4 (M = In, Tl) salts are well defined. The cation ClO2+ is unambiguously characterized; it interacts with the anion M(ClO4)4−, which has monodentate and bidentate perchlorate groups.

Dimethylmetallderivate substituierter Pyrrole (Metall = Al, Ga und In) / Dimethylmetal Derivatives of Substituted Pyrroles (Metal = Al, Ga, and In)

1993 ◽  
Vol 48 (11) ◽  
pp. 1437-1447 ◽  
Author(s):  
Jochen Tödtmann ◽  
Wolfgang Schwarz ◽  
Johann Weidlein ◽  
Arne Haaland
Keyword(s):  
Vibrational Spectra ◽  
High Melting ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Substituted Pyrroles ◽  
Derivatives Of ◽  
Ir And Raman

The reactions of indium trimethyl with the substituted pyrroles HNC4H2Me2-2,5 and HNC4Me4-2,3,4,5 (Me = CH3) yield the solid, high melting dimethylindium azolides Me2In—NC4H2Me2-2,5 and Me2In—NC4Me4, respectively. Colorless and crystalline N-methyl-2-dimethylmetal pyrrolides have been prepared from Me2MCl (M = Al, Ga, In) and lithiated N-methyl pyrrole. All compounds were investigated by MS, NMR (1H and 13C), and vibrational spectra (IR and Raman). The X-ray structure determinations of Me2Ga—C4H3NMe and Me2InNC4Me4 show the triclinic space group P T in both cases, with two formula units per cell forming “π-dimers” via short intermolecular M · · · C contacts of 248.1 (Ga) and 257.5 (In) pm.

Kristallstrukturen, Schwingungsspektren und Normalkoordinaten- analysen von trans-[OsO2(ox)2]2– und trans-[OsO2(mal)2]2–/ Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[OsO2(ox)2]2– and trans -[OsO2(mal)2]2–

1998 ◽  
Vol 53 (8) ◽  
pp. 823-828 ◽  
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

Abstract The crystal structures of trans-(Ph4P)2[OsO2(ox)2] (monoclinic, space group P21/n, a = 12.281(2), b = 14.5440(13), c = 13.9810(12) Å, β = 100.000(8)°, Z = 2) and trans- (n-Bu4N)2[OsO2(mal)2] (triclinic, space group P1̄, a = 10.365(4),b = 10.707(3), c - 11.473(5) A, a = 73.00(2), β = 64.44(3), 7 = 82.55(3)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of these complexes were measured at room temperature. Based on the molecular parameters of the X-ray determinations normal coordinate analyses have been performed and the vibrations assigned. The valence force constants of [OsO2(ox)2]2- are fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 5.05, fd(C=O) = 11.2 and fd(C-C) = 4.7 mdyn/Å and of [OsO2(mal)2]2- fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 4.86, fd(C=O) =11.1 and fd(C-C) = 4.07 mdyn/Å.

Syntheses, Single-crystal Structure and Vibrational Spectra of Ca15(CBN)6(C2)2H2

2011 ◽  
Vol 66 (11) ◽  
pp. 1092-1096
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvoa
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Cell Parameter ◽  
Single Crystal Structure ◽  
Boron Powder ◽  
Space Group ◽  
Ir And Raman

Single crystals of Ca15(CBN)6(C2)2H2 were obtained either by the reaction of stoichiometric amounts of graphite, hexagonal BN, and CaH2 with an excess of distilled Ca, or by using graphite, boron powder, Ca3N2, and CaH2 with an excess of distilled Ca. Both reactions took place in silicajacketed Ta ampoules at 1400 K. Crystals of the title compound are transparent dark-red and isopointal to Ca15(CBN)6(C2)2O adopting the cubic space group Ia3̄d (no. 230, Z = 8) with the cell parameter a = 1653.30(17) pm. The vibrational spectra were recorded and are compared with IR and Raman data of isotypic compounds

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-(n-Bu4N)2[ReBr4(NCS)2 ], cis-(n-Bu4N)2[ReBr4(NCSe)2] und cis-(n-Bu4N)2[ReBr4(NCS)(NCSe)] / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of cis-(n-Bu4N)2[ReBr4(NCS)2], cis-(n-Bu4N)2[ReBr4(NCSe)2,] and cis -(n -Bu4N)2[ReBr4(NCS)(NCSe)]

2000 ◽  
Vol 55 (2) ◽  
pp. 178-184 ◽  
Author(s):  
L. Homolya ◽  
W. Preetz
Keyword(s):  
Low Temperature ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Vibrational Spectra ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReBr4(NCS)2] (1) (triclinic, space group P1̄, a = 11.475(6), b = 20.096(16), c = 22.144(11) Å, α = 110.56(6), β = 92.97(5), γ = 99.77(7)°, Z = 4), cis-(n-Bu4N)2[ReBr4(NCS)2] (2) (triclinic, space group P1̄, a = 11.527(3), b = 20.237(7), c = 22.07(2) Å, α = 110.05(4), β = 93.86(6), γ = 99.49(4)°, Z = 4) and cis-{n- Bu4N)2[ReBr4(NCS)(NCSe)] (3) (triclinic, space group P1̄, a = 11.488(2), b = 20.164(6), c = 22.158(5) Å, α = 110.44(2), β = 93.34(2), γ = 99.626(18)°. Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on these molecular parameters the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(ReN) = 1.70 (1), 1.70 (2) and 1.72 (3), fd(ReBr) = 1.36 (1), 1.30 (2) and 1.36 mdyn/Å (3).

OnemoreCompound Containing the CBN4- Ion – Synthesis, Single-crystal Structure and Vibrational Spectra of Ca15(CBN)6(C2)2F2

2010 ◽  
Vol 65 (12) ◽  
pp. 1409-1415 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. Di Salvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Raman Spectra ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Cell Parameter ◽  
Single Crystal Structure ◽  
Space Group ◽  
Ir And Raman

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.

scholarly journals Die Spektren und Kristallstrukturen der Addukte CI5Sb · [N(i-C3H7)CN(i-C3H7)] und Cl4Sn · 2 [N(i-C3H7)CN(i-C3H7)] / Spectra and Crystal Structures of the Adducts Cl5Sb · [N(i-C3H7)CN(i-C3H7)] and Cl4Sn · 2 [N(i-C3H7)CN(i-C3H7)]

1986 ◽  
Vol 41 (10) ◽  
pp. 1223-1229 ◽  
Author(s):  
H.-D. Hausen ◽  
W. Schwarz ◽  
G . Rajca ◽  
J. Weidlein
Keyword(s):  
Crystal Structures ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Unit Cell ◽  
Molar Ratio ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

Abstract Spectra and Crystal Structures of the Adducts C l5Sb • [N(/-C3H 7)C N (i-C3H 7)] and C l4Sn • 2 [N(/-C3H 7)CN(/-C3H 7)j X-Ray, Vibrational Data, Diisopropylcarbodiimide Adducts of SbCl5, SnCl4 Thecarbodiimide adducts Cl5Sb <-(—N (R) = C = N R)(1) and Cl4S n ^ (-N (R) = C = N R) 2(2)(R = /-C3H 7) have been prepared by the reaction o f R —N = C —N — R with SbCl5 in a 1:1 and with SnCl4 in a 2:1 molar ratio, respectively. The vibrational spectra (IR and Raman) of both compounds have been regarded and assigned to the skeleton modes. The X-ray structure determination shows the orthorhombic space group Pna2, with 4 formula units per unit cell for 1. Adduct 2 has a trans-configuration and crystallizes in the triclinic space group P 1 with only one molecule per unit cell.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von (Ph3PNPPh3)[OsF5Cl]·CH2Cl2 und cis-(Ph3PNPPh3)[OsF4Cl2]·CH2Cl2 / Crystal Structures, Vibrational Spectra and Normal Coordinate Analysis of (Ph3PNPPh3) [OsF5Cl]·CH2Cl2 and cis-(Ph3PNPPh3 )[OsF4Cl2]·CH2Cl2

2000 ◽  
Vol 55 (1) ◽  
pp. 45-50
Author(s):  
B. Lorenzen ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Vibrational Spectra ◽  
Normal Coordinate Analysis ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Ir And Raman ◽  
Complex Anions

By careful oxidation of the pure fluorochloroosmates(IV) with BrF3 in dichloromethane the mixed pentavalent complex anions [OsF5Cl]- and cis -[OsF4Cl2]- are formed. X-ray structure determinations on single crystals have been performed of (Ph3PNPPh3)[OsF5Cl]·CH2Cl2 (1) (triclinic, space group P1̄, a = 12.153(5), b = 12.387(5), c = 14.229(5) Å , α = 70.07(1), β = 65.46(1), γ = 72.87(1)°, Z = 2) and cis-(Ph3PNPPh3)[OsF4Cl2]·CH2Cl2 (2) (triclinic, space group P1̄, a = 11.987(2) b = 13.083(2), c = 14.456(2) Å, α = 66.30(1), β = 65.47(1), γ = 71.22(1)°, Z = 2). Based on the molecular parameters of the X-ray determinations the IR and Raman spectra for the anions of 1 and 2 have been assigned by normal coordinate analysis. Due to the mutual trans influences the valence force constants of asymmetrically coordinated octahedral axes F•-Os-Cl′ differ from those of the symmetric F-Os-F axes. The data are for 1: fd(OsF•) = 3.95, fd(OsF) = 4.07, fd(OsCl′) = 2.51 and for 2: fd(OsF•) = 3.45, fd(OsF) = 3.97, fd(OsCl′) = 2.42 mdyn/Å

Synthesis and Characterization of Tris(trimethyltin) Thiophosphate (Me3Sn)3PO3S

1993 ◽  
Vol 48 (12) ◽  
pp. 1781-1783 ◽  
Author(s):  
Abdel-Fattah Shihada
Keyword(s):  
Aqueous Medium ◽  
Raman Spectra ◽  
Mass Spectra ◽  
Ir And Raman Spectra ◽  
Synthesis And Characterization ◽  
Polymeric Structure ◽  
Ir And Raman

(Me3Sn)3PO3S has been prepared from the reaction of Me3SnCl with Na3PO3S • 12 H2O under cooling in aqueous medium. Its IR and Raman spectra are found to be consistent with a polymeric structure with tetra- and penta-coordinated tin atoms. The 31P NMR and mass spectra of (Me3Sn)3PO3S are reported and discussed.

Kristallstruktur und Schwingungsspektren des Di-Blei-Hexaselenohypodiphosphates Pb2P2Se6 / Crystal Structure and Vibrational Spectra of Pb2P2Se6

1984 ◽  
Vol 39 (4) ◽  
pp. 357-361 ◽  
Author(s):  
Robert Becker ◽  
Wolfgang Brockner ◽  
Herbert Schäfer
Keyword(s):  
Crystal Structure ◽  
Raman Spectra ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Far Infrared ◽  
Infrared And Raman Spectra ◽  
Monoclinic System ◽  
Space Group ◽  
Lattice Constants

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.

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