Abstract
Treatment of (μ-H) 3Os 3(CO) 9(μ 3-CH) sequentially with trifluoromethanesulfonic acid followed by a phosphoric or arsonic acid provides compounds of the formula (μ-H) 2Os 3(CO) 9(μ 3η 3-O 3ER) [E P, R Ph( 3), Me( 4); E As, R Ph( 5)] Assignments of important infrared bands for the coordinated oxyanions have been made. The complex (μ-H) 2Os 3(CO) 9(μ,η 3 3O 3 PPh) ( 3) has been studied by variable temperature 13C NMR spectroscopy. The reaction of Os 3(CO) 10(S) 2 (S = C 8H 14,CH 3CN) with Ph 2PO 2H in THF at 55–60°C produces (μ-H)Os 5(CO) 10(μ,η 2O 2PPh 2) ( ca. 60%), the structure of which has been determined by X-ray crystallography.
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