Studies of molybdenum-molybdenum bonded species: 1. Synthesis and characterization of a reduction product of Cs3Mo2Cl8H; 2. Mixed sulfur chlorine substituted hexanuclear molybdenum clusters

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1982
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Luly, Matthew
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Chemistry

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A black powder isolated from the reaction of Cs(,3)Mo(,2)Cl(,8)H and zinc in refluxing pyridine, Mo(,1.0)Cl(,1.1)py(,0.8), has been studied. The material is amorphous to x-rays, and the infrared spectrum indicates coordinated pyridine and chlorine. The x-ray photoelectron spectrum indicates one type of molybdenum and shows both terminal and bridging chlorine are present in the ratio of 1.5:1.0. Mo(,1.0)Cl(,1.1)py(,0.8) is stable at elevated temperatures and can be heated in vacuo for over 24 hours at 300(DEGREES)C with little change in composition. The best description of this material seems to be a highly bridged, metal-metal bonded cluster or polymer;Mo(,6)Cl(,12) has been reacted with various sulfur-containing reagents to prepare mixed chlorine sulfide Mo(,6)X(,8) clusters. These clusters have been characterized by x-ray powder diffraction, x-ray photoelectron spectroscopy, and infrared spectroscopy. High reaction temperatures (> 200(DEGREES)C) with high ratios of NaSH to Mo(,6)Cl(,12) (16:1) result in decomposition of the Mo(,6)X(,8) cluster. Reactions of 1 equivalent of Mo(,6)Cl(,12) and 8 equivalents of NaSH at 115(DEGREES)C yield amorphous products. Intermediate conditions produce crystalline Mo(,6)X(,8) derivatives. These products appear to be solid solutions, or have some amorphous impurity present;A FORTRAN IV computer program for analyzing x-ray photo-electron spectra is described. The program smooths the data, makesbaseline and scattering corrections, and fits the corrected spectrawith linear combinations of Gaussian and Cauchy functions. The;results are useful in inferring structural information;*DOE Report IS-T-959. This work was performed under ContractW-7405-eng-82 with the Department of Energy.

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Fri Jan 01 00:00:00 UTC 1982