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Metal alkoxides - models for metal oxides. 9. Hydridoditungsten alkoxides: W/sub 2/(H)(O-i-Pr)/sub 8/Na diglyme and W/sub 2/(H)(I)(OCH/sub 2/-t-Bu)/sub 6/(H/sub 2/NMe). Further investigations of the reaction between W/sub 2/(NMe/sub 2/)/sub 6/(M identical with M) and i-PrOH leading to W/sub 3/(H)/sub 2/(O-i-Pr)/sub 14/

Journal Article · · J. Am. Chem. Soc.; (United States)
DOI:https://doi.org/10.1021/ja00262a007· OSTI ID:6038273

Reaction between W/sub 2/(NMe/sub 2/)/sub 6/(M identical with M) and i-PrOH (>>6 equiv), which leads to the known compound W/sub 4/(H)/sub 2/(O-i-Pr)/sub 14/, is shown to be critically dependent on the presence of the liberated amine. The addition of i-PrOH (>>6 equiv) to hydrocarbon solutions of W/sub 2/(O-t-Bu)/sub 6/ or W/sub 2/(O-i-Pr)/sub 6/(HNMe/sub 2/)/sub 2/ does not lead to W/sub 4/(H)/sub 2/(O-i-Pr)/sub 14/ but rather yields an oliomeric species (W(O-i-Pr)/sub 3/)/sub n/. From the reaction between W/sub 2/(O-t-Bu)/sub 6/ in hexane/ROH and NaOR (1 equiv), hexane-insoluble compounds are formed: NaW/sub 2/(H)(OR)/sub 8/, where R = i-Pr and CH/sub 2/-t-Bu. Extraction into hexane solution by the addition of diglyme (1 equiv) yields W/sub 2/(H)(O-i-Pr)/sub 8/Na diglyme, which has been characterized by NMR studies and a single-crystal X-ray diffraction study. Crystal data for W/sub 2/(H)(O-i-Pr)/sub 8/Na diglyme at -155 /sup 0/C are the following: a = 24.087 (8) A, b = 16.540 (5) A, c = 12.747 (4) A, ..beta.. = 125.71 (1)/sup 0/, Z = 4,d/sub calcd/ = 1.608 g cm/sup -3/, and space group P2/sub 1//a; for W/sub 2/(H)(I)(OCH/sub 2/-t-Bu)/sub 6/(H/sub 2/NMe) at -158 /sup 0/C a = 18.159 (5) A, b = 10.873 (2) A, c = 11.599 (3) A, ..cap alpha.. = 77.30 (1)/sup 0/, ..beta.. = 109.37 (1)/sup 0/, ..gamma.. = 96.55 (2)/sup 0/, Z = 2,d/sub calcd/ = 1.656 g cm/sup -3/, and space group P1. 31 references, 7 figures, 7 tables.

Research Organization:
Indiana Univ., Bloomington
OSTI ID:
6038273
Journal Information:
J. Am. Chem. Soc.; (United States), Journal Name: J. Am. Chem. Soc.; (United States) Vol. 108:2; ISSN JACSA
Country of Publication:
United States
Language:
English