SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE ANALYSIS OF DELTA,LAMBDA-MU-HYDROXO-MU-TRIFLUOROACETATO-BIS[BIS(ETHYLENEDIAMINE) CHROMIUM(III)] BROMIDE TRIPERCHLORATE MONOHYDRATE

被引:10
作者
KAAS, K
SPRINGBORG, J
机构
[1] Chemistry Department, Royal Veterinary and Agricultural University, Thorvaldsensvej 40, Frederiksberg C,DK-1871, Denmark
来源
ACTA CHEMICA SCANDINAVICA SERIES A-PHYSICAL AND INORGANIC CHEMISTRY | 1986年 / 40卷 / 08期
关键词
Solutions - Binary alloys - Single crystals - Chlorine compounds - Inorganic compounds - Positive ions - Chromium alloys - Crystal structure;
D O I
10.3891/acta.chem.scand.40a-0515
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Reaction of the dinuclear complex cation Δ,Δ-[(en)2Cr(OH)2Cr(en)2]4+ in aqueous CF3COOH led to the formation of the singly bridged species Δ,Δ-[(CF3COO)(en)2Cr(OH)Cr(en)2(CF3COO)]3+ which was isolated as a perchlorate salt (91 %). This species hydrolyzed in aqueous solution to give the heterobridged cation Δ,Δ-[(en)2Cr(OH)(CF3COO)Cr(en)2]4+ which was isolated as a bromide salt (73 %). The latter cation was characterized by single-crystal structure analysis of the monobromide triperchlorate monohydrate salt. These crystals are orthorhombic, space group Pnma with Z = 4, unit cell dimensions: a = 17.687(3); b = 11.703(3); and c = 15.304(4)Å. The structure was solved and refined to R = 0.059 from 1104 diffractometer-collected intensities. The complex ion contains a crystallographic mirror plane and the conformations of the chelate rings are λλΔ,Δδδ. The bridging six-membered ring is nearly planar. The Cr-Cr separation is 3.616(2)Å. The CF3 group and the ClO4- ions are disordered.
引用
收藏
页码:515 / 521
页数:7
相关论文
共 35 条
[1]  
ANDERSEN P, 1984, ACTA CHEM SCAND A, V38, P593, DOI 10.3891/acta.chem.scand.38a-0593
[2]  
ANDERSEN P, 1986, ACTA CHEM SCAND A, V40
[3]  
BONE SP, 1978, J CHEM SOC DA, V1, P1544
[4]   BINUCLEAR COMPLEXES OF CHROMIUM(III) .2. SYNTHESIS AND PROPERTIES OF THE RACEMIC ISOMERS OF MU-HYDROXO AND DI-MU-HYDROXO BINUCLEAR COMPLEXES OF CHROMIUM(III) WITH ETHYLENEDIAMINE AS A LIGAND [J].
CHRISTENSSON, F ;
SPRINGBORG, J ;
TOFTLUND, H .
ACTA CHEMICA SCANDINAVICA SERIES A-PHYSICAL AND INORGANIC CHEMISTRY, 1980, 34 (05) :317-326
[5]   THERMODYNAMICS AND KINETICS FOR THE EQUILIBRATION BETWEEN MONOHYDROXO AND DIHYDROXO BRIDGED BINUCLEAR TETRAAMMINE CHROMIUM(III) COMPLEXES - SYNTHESIS AND ISOLATION OF THE MONOHYDROXO BRIDGED SPECIES [J].
CHRISTENSSON, F ;
SPRINGBORG, J .
ACTA CHEMICA SCANDINAVICA SERIES A-PHYSICAL AND INORGANIC CHEMISTRY, 1982, 36 (01) :21-30
[6]   EQUILIBRIA BETWEEN MONOHYDROXO-BRIDGED AND DIHYDROXO-BRIDGED BINUCLEAR AMMINERHODIUM(III) COMPLEXES [J].
CHRISTENSSON, F ;
SPRINGBORG, J .
INORGANIC CHEMISTRY, 1985, 24 (14) :2129-2132
[7]   CRYSTAL AND MOLECULAR-STRUCTURES OF THE BIS(TRIPHENYLPHOSPHINE) AND BIS(TRIPHENYL PHOSPHITE) ADDUCTS OF TETRAKIS(TRIFLUOROACETATO)DIRHODIUM(II) [J].
COTTON, FA ;
FELTHOUSE, TR ;
KLEIN, S .
INORGANIC CHEMISTRY, 1981, 20 (09) :3037-3042
[8]   RELATIVISTIC CALCULATION OF ANOMALOUS SCATTERING FACTORS FOR X-RAYS [J].
CROMER, DT ;
LIBERMAN, D .
JOURNAL OF CHEMICAL PHYSICS, 1970, 53 (05) :1891-&
[9]   X-RAY SCATTERING FACTORS COMPUTED FROM NUMERICAL HARTREE-FOCK WAVE FUNCTIONS [J].
CROMER, DT ;
MANN, JB .
ACTA CRYSTALLOGRAPHICA SECTION A-CRYSTAL PHYSICS DIFFRACTION THEORETICAL AND GENERAL CRYSTALLOGRAPHY, 1968, A 24 :321-&
[10]   SYNTHESIS AND CHARACTERIZATION OF THE DIMERIC CHROMIUM(III) COMPLEX DI-MU-HYDROXOBIS [(N,N'-BIS(2-PYRIDYLMETHYL)-1,3-PROPANEDIAMINE) CHROMIUM(III)] PERCHLORATE, [(BISPICTN)CR(OH)]2(CLO4)4.3H2O [J].
FISCHER, HR ;
HODGSON, DJ ;
MICHELSEN, K ;
PEDERSEN, E .
INORGANICA CHIMICA ACTA-ARTICLES AND LETTERS, 1984, 88 (02) :143-150