LIGAND SUBSTITUTION PROCESSES IN TETRANUCLEAR CARBONYL CLUSTERS .10. X-RAY STRUCTURAL CHARACTERIZATION OF PRODUCTS RESULTING FROM REACTIONS OF CO4(CO)9(HC(PPH2)3, WITH PHOSPHINE-LIGANDS
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The solid-state geometry of Co4(CO)g(PMe3)(tripod) (I), Co4(CO)7(dppm)(tripod) (II), and Co4(CO)7(PMe3)2(tripod) (III) were determined by single-crystal X-ray diffraction studies. I crystallizes in an orthorhombic cell Pbca with a = 16.864 (5) , b = 16.989 (3) , and c = 34.676 (9) with eight molecules per unit cell, II crystallizes in a monoclinic cell P21/c with a = 12.001 (4) , b= 21.955 (10) , c = 25.329 (9) , and = 99.40 (3) with four molecules per unit cell. III crystallizes in an orthorhombic cell Pca21 with a = 24.831 (6) , = 11.999 (2) , and c= 19.191 (4) with four molecules per unit cell. The structures were refined to the following values; I to R =0.0626 and Rw= 0.0589, II to R = 0.0900 and Rw= 0.0910, and III to R = 0.0706 and Rw= 0.0663. The solid-state structures were used to substantiate the solution structural assignments based on IR and 31P and 13C NMR spectroscopy and to assist in identifying the specific site of ligand dissociation in this series of clusters. 1986, American Chemical Society. All rights reserved.