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Preparation of (Nb(eta/sup 5/-C/sub 5/Me/sub 5/)Cl/sub 2/)/sub 2/ and Nb(eta/sup 5/-C/sub 5/Me/sub 5/)(3-hexyne)Cl/sub 2/

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00183a033· OSTI ID:6492764

NbMe/sub 2/(dimethyl)Cl/sub 3/, prepared from NbCl/sub 3/ and ZnMe/sub 2/, reacts well with LiC/sub 5/Me/sub 5/ to yield Nb(eta/sup 2/-C/sub 5/Me/sub 5/)Me/sub 2/Cl/sub 2/. This substance reacts relatively rapidly with molecular hydrogen to produce a green crystalline compound which is similar to (Ta(eta/sup 5/-C/sub 5/Me/sub 5/)ClH)/sub 2/ in color and form. Evidence is presented to suggest that the Nb product is not in the hydride form and is (Nb(eta/sup 5/-C/sub 5/Me/sub 5/)Cl/sub 2/)/sub 2/. The ir spectrum and the /sup 1/HNMR signal do not show the presence of the hydride. The mass spectrum of the product prepared in a reaction in which H/sub 2/ was used and one in which D/sub 2/ was used each exhibits only a parent ion consistent with (Nb(eta/sup 5/-C/sub 5/Me/sub 5/)Cl/sub 2/)/sub 2/. The dimer formulation is supported by experimental results, as well. The dimer reacts with 3-hexyne to prouce a purple analogue of the Ta acetylene complexes, NB(eta/sup 5/-C/sub 5/Me/sub 5/)(3-hexyne)Cl/sub 2/. 17 references.

Research Organization:
Massachusetts Inst. of Tech., Cambridge
DOE Contract Number:
AC02-78ER04949
OSTI ID:
6492764
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 23:15; ISSN INOCA
Country of Publication:
United States
Language:
English