Cluster oxalate complexes [W3(μ3-Q)(μ2-Q)3 (C2O4)3(H2O)3]2- (Q = S, Se):: Mechanochemical synthesis and crystal structure

被引：7
|
作者：
Sokolov, MN [1 ]
Gushchin, AL [1 ]
Naumov, DY [1 ]
Gerasko, OA [1 ]
Fedin, VP [1 ]
机构：
[1] Russian Acad Sci, Nikolaev Inst Inorgan Chem, Novosibirsk 630090, Russia
来源：
JOURNAL OF CLUSTER SCIENCE | 2005年 / 16卷 / 03期
关键词：
tungsten; oxalate; cluster; crystal structure; mechanochemistry;
D O I：
10.1007/s10876-005-0026-9
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
Mechanochemical reaction of cluster coordination polymers (1)(infinity)[W(3)Q(7)Br(4)] (Q = S, Se) with solid K2C2O4 leads to the cluster core excision with the formation of anionic complexes [W(3)Q(7)(C2O4)(3)](2-). Extraction of the reaction mixture with water followed by crystallization gives crystalline K-2[W3S7(C2O4)(3)] center dot 0.5KBi-. 5H(2)O (main product) and K-2[W-3(mu(3)-S)(mu(2)-S)(3)(H2O)(3)(C2O4)(3)]center dot 0.5H(2)C(2)O(4)center dot 3H(2)O (1) (minor product). In the case of the Se cluster, the W3Se7 complex could not be isolated, and the treatment of the aqueous extract with PPh3 gave K-2[W-3(mu(3)-Se)(mu(2)-Se)(3)(H2O)(3)(C2O4)(3)] center dot H2O (2) in a low yield. Alternatively, it was obtained from [W3Se4(H2O)(9)](4+) and K2C2O4 in high yield. Both 1 and 2 were characterized by X-ray structure analysis.
引用
收藏
页码：309 / 318
页数：10
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