首例氧化磷杂戊二烯五羰基铬(0)和钼(0)配合物的合成、结构和反应。

First examples of oxaphosphirane pentacarbonylchromium(0) and -molybdenum(0) complexes: synthesis, structures and reactions.

机构信息

Institut für Anorganische Chemie der Rheinischen Friedrich-Wilhelms-Universität Bonn, Gerhard-Domagk-Str., 1, D-53121, Bonn, Germany.

出版信息

Dalton Trans. 2011 Mar 21;40(11):2654-65. doi: 10.1039/c0dt01509a. Epub 2011 Feb 10.

DOI:10.1039/c0dt01509a

PMID:21308136

Abstract

Synthesis of the first oxaphosphirane chromium(0) and molybdenum(0) complexes of the type [{(R(1)PCH(R(2))-O}M(CO)(5)] (R(1) = C(5)Me(5)) (8a-e, 15a-e) and (R(1) = CH(SiMe(3))(2)) (9a-e, 16a-e) via reaction of dichloro(organo)- (1, 2, 10, 11) and chloro(organo)phosphane complexes (3,4,12) with lithium bases and aldehydes 7a-e is reported. Furthermore, bicyclic 1,3-oxaphospholane complexes 17 and 18 have been obtained via O-protonation of oxaphosphirane complexes 8a and 15a with HCl. All complexes were characterized by NMR, IR spectroscopic, mass spectrometric investigations and, in addition, single-crystal X-ray structures of complexes 8a-e, 9a,c, 15a,b,e, 16a-c, 17, 18 are presented and discussed.

摘要

合成了第一个氧杂膦烷铬（0）和钼（0）配合物，类型为[{（R(1)PCH(R(2))-O}M(CO)(5)]（R(1)=C(5)Me(5))（8a-e，15a-e）和（R(1)=CH(SiMe(3))(2))（9a-e，16a-e）通过反应二氯（有机）-（1,2,10,11）和氯（有机）膦配合物（3,4,12）与锂碱和醛 7a-e。此外，通过氧杂膦烷配合物 8a 和 15a 与 HCl 的 O-质子化，得到了双环 1,3-氧杂磷杂环戊烷配合物 17 和 18。所有配合物均通过 NMR、IR 光谱、质谱研究进行了表征，此外，还呈现和讨论了配合物 8a-e、9a,c、15a,b,e、16a-c、17、18 的单晶 X 射线结构。