Synthesis and characterization of Cs2Mo6X14 (X= br or 1) hexamolybdenum cluster halides:: Efficient Mo6 cluster precursors for solution chemistry syntheses

被引:153
作者
Kirakci, K [1 ]
Cordier, S [1 ]
Perrin, C [1 ]
机构
[1] Univ Rennes 1, CNRS, UMR 6511,Inst Chim Rennes, Chim Solide & Inorgan Mol Lab, F-35042 Rennes, France
来源
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 2005年 / 631卷 / 2-3期
关键词
octahedral cluster; molybdenum halides; crystal structures;
D O I
10.1002/zaac.200400281
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Cs2Mo6Br14 (1) and Cs2Mo6I14 (2) have been synthesized by solid state chemistry techniques and structurally characterized by single crystal X-ray diffraction. They crystallize in the P (3) over bar 1c space group (Nr. 163) with the following lattice parameters: a = 10.1925(1) Angstrom, c = 15.0690(3) Angstrom, Z = 2 for 1; a = 10.804(5) Angstrom, c = 16.258(5) A, Z = 2 for 2. These clusters halides, whose structures are related to that of Cs2Mo6Cl8Br6, are built up from discrete [(Mo6X8i)X-6(a)](2-) anionic units (X - Br, 1) stacked according to an hexagonal close-packing arrangement. In the present work, the influence of the halogen on the cesium sites will be evidenced and discussed. Furthermore, a simple high yield preparation method of (TBA)(2)(Mo6X8X6a)-X-i will be proposed starting from (Cs2MoX14)-X-6.
引用
收藏
页码:411 / 416
页数:6
相关论文
共 40 条
[1]  
Alcock N. W., 1970, CRYSTALLOGRAPHIC COM, P271
[2]   AN EMPIRICAL CORRECTION FOR ABSORPTION ANISOTROPY [J].
BLESSING, RH .
ACTA CRYSTALLOGRAPHICA SECTION A, 1995, 51 :33-38
[3]  
BLOMSTRAND, 1959, J PRAKT CHEM, V77, P88
[4]   SYNTHESIS AND CRYSTAL-STRUCTURE OF THE HOMOLOGOUS SERIES PBMO6X14, X=CL, BR, I [J].
BOSCHEN, S ;
KELLER, HL .
ZEITSCHRIFT FUR KRISTALLOGRAPHIE, 1992, 200 (3-4) :305-315
[5]  
BROSSET C, 1945, ARK KEMI MINERAL G A, V20
[6]   Synthesis, crystal structure, NMR, vibrational spectra, and normal coordinate analysis of the cluster anions [(Mo6I8i)Y-6(a)](2-), Y-a=F,Cl,Br,I [J].
Bruckner, P ;
Preetz, W ;
Punjer, M .
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 1997, 623 (01) :8-17
[7]   SIRWARE [J].
Cascarano, G. ;
Altomare, A. ;
Giacovazzo, C. ;
Guagliardi, A. ;
Moliterni, A. G. G. ;
Siliqi, D. ;
Burla, M. C. ;
Polidori, G. ;
Camalli, M. .
ACTA CRYSTALLOGRAPHICA A-FOUNDATION AND ADVANCES, 1996, 52 :C79-C79
[8]   The novel Cs4Nb6F18.5I13.5I6a octahedral niobium cluster fluoro-iodide:: a step towards the Nb6Fi12 cluster core excision [J].
Cordier, S ;
Perrin, C .
JOURNAL OF SOLID STATE CHEMISTRY, 2004, 177 (03) :1017-1022
[9]   Synthesis and characterization of Mo6 chalcobromides and cyano-substituted compounds built from a novel [(Mo6Bri6Yi2)La6]n- discrete cluster unit (Yi = S or Se and La = Br or CN) [J].
Cordier, S ;
Naumov, NG ;
Salloum, D ;
Paul, F ;
Perrin, C .
INORGANIC CHEMISTRY, 2004, 43 (01) :219-226
[10]   CRYSTALLOCHEMISTRY OF SOME NEW NIOBIUM BROMIDES WITH (NB6BR18) UNITS - STRUCTURES OF CSERNB6BR18 AND CS2EUNB6BR18 [J].
CORDIER, S ;
PERRIN, C ;
SERGENT, M .
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 1993, 619 (04) :621-627