MECHANOCHEMICAL SYNTHESIS OF SOLUBLE COMPLEXES CONTAINING M3S74+ AND M3SE74+ FRAGMENTS FROM POLYMERIC M3Y7BR4 (M = MO, W, Y = S, SE) - THE CRYSTAL-STRUCTURE OF (PPN)2W3S7CL6

被引:59
作者
FEDIN, VP [1 ]
SOKOLOV, MN [1 ]
MYAKISHEV, KG [1 ]
GERASKO, OA [1 ]
FEDOROV, VY [1 ]
MACICEK, J [1 ]
机构
[1] BULGARIAN ACAD SCI,INST APPL MINERAL,BU-1000 SOFIA,BULGARIA
关键词
D O I
10.1016/S0277-5387(00)81263-2
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The interaction of solid W3S7Br4 or W3Se7Br4 with Et4NBr under vibrational mill conditions followed by extraction with acetonitrile resulted in the isolation of (Et4N)2W3S7Br6 (1) and (Et4N)2W3Se7Br6 (2) salts. Treatment of the product of the analogous reaction of Mo3Se7Br4 and Et4NBr with sodium diethyldithiocarbamate (Nadtc) resulted in [Mo3Se7(dtc)3]dtc (4). The M3Y7(4+) (Y = S, Se) cluster fragments are retained in all of these reactions. By dissolving 1 in conc. hydrochloric acid and adding PPNCl, the (PPN)2W3S7Cl6 salt (5) was obtained, for which an X-ray study has been performed. Selected distances for the cluster anion W3(mu-3-S)(mu-2-S2)3Cl6(2-) are 2.7270(7)-2.7445(6) angstrom for W-W, 2.360(3)-2.361(3) angstrom for W-(mu-3-S), 2.032(4)-2.052(4) angstrom for S-S, 2.429(3)-2.459(2) and 2.493(4)-2.519(3) angstrom for W-Cl (for cis and trans positions with respect to mu-3-S, respectively). Rather short distances (3.17-3.21 angstrom) between the chlorine atoms and sulphur atoms of the mu-2-S2 ligands of the adjacent anions were noted. The interaction of 2 with 1,2-bisdiphenylphosphine ethane(dppe) is accompanied by elimination of selenium to produce [W3Se4Br3(dppe)3]Br (6).
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页码:1311 / 1317
页数:7
相关论文
共 24 条
[1]   REACTIONS OF TERTIARY DIPHOSPHINES WITH NICKEL AND NICKEL CARBONYL [J].
CHATT, J ;
HART, FA .
JOURNAL OF THE CHEMICAL SOCIETY, 1960, (MAR) :1378-1389
[2]   SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF 3 NEW TRINUCLEAR GROUP-VI CLUSTERS [J].
COTTON, FA ;
KIBALA, PA ;
MATUSZ, M ;
MCCALEB, CS ;
SANDOR, RBW .
INORGANIC CHEMISTRY, 1989, 28 (13) :2623-2630
[3]   TRIANGULAR TRINUCLEAR CLUSTER COMPOUNDS - MOLYBDENUM AND TUNGSTEN COMPLEXES OF THE TYPE [M3S4(DIPHOS)3CL3]+, [M3S4(DIPHOS)3H3]+ [J].
COTTON, FA ;
LLUSAR, R ;
EAGLE, CT .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1989, 111 (12) :4332-4338
[4]  
DUSS F, 1979, COMPREHENSIVE ORGANI, V3
[5]  
FEDIN VP, 1990, KOORDINATS KHIM+, V16, P291
[6]   TRIANGULAR THIOCOMPLEXES OF MOLYBDENUM - REACTIONS WITH HALOGENS, HYDROHALOGEN ACIDS AND PHOSPHINES [J].
FEDIN, VP ;
SOKOLOV, MN ;
MIRONOV, YV ;
KOLESOV, BA ;
TKACHEV, SV ;
FEDOROV, VY .
INORGANICA CHIMICA ACTA, 1990, 167 (01) :39-45
[7]   TRIANGULAR W3S-7(4+) AND W3S-4(4+) COMPLEXES [J].
FEDIN, VP ;
SOKOLOV, MN ;
GERASKO, OA ;
KOLESOV, BA ;
FEDOROV, VY ;
MIRONOV, AV ;
YUFIT, DS ;
SLOVOHOTOV, YL ;
STRUCHKOV, YT .
INORGANICA CHIMICA ACTA, 1990, 175 (02) :217-229
[8]  
Fedorov V.E., 1985, RUSS CHEM REV+, V54, P408, DOI [DOI 10.1070/RC1985V054N04ABEH003064, 10.1070/rc1985v054n04abeh003064]
[9]  
FEDOROV VY, 1978, IZV SIB OTD AN KHIM, V14, P56
[10]   PREPARATION OF TRIANGULAR AND CUBIC MOLYBDENUM CLUSTERS AS AQUA IONS [J].
KATHIRGAMANATHAN, P ;
MARTINEZ, M ;
SYKES, AG .
POLYHEDRON, 1986, 5 (1-2) :505-506