110717-83-4Relevant academic research and scientific papers
Synthesis of metallacarborane clusters derived from the monocarbon carborane 9-(CH3)2S-7-[((CH3)3Si) 2CH]CB10H11
Quintana, William,Ernest, Robin L.,Carroll, Patrick J.,Sneddon, Larry G.
, p. 166 - 172 (1988)
A single-crystal X-ray study of 9-Ph3P-7-[((CH3)3Si)2CH]CB 10H11 (I) has confirmed that the compound has a structure based on an 11-vertex nido cage geometry. Crystal data for I: space group P21/n; Z = 4; a = 17.154 (3) ?, b = 11.999 (2) ?, c = 17.469 (4) ?, β = 108.2 (1)°; V = 3414.2 ?3. The structure was refined to a final R = 0.061 and Rw = 0.073 for the 2916 reflections having Fo2 > 3μ(Fo2). The dimethyl sulfide analogue of I, 9-(CH3)2S-7-[((CH3)3Si) 2CH]CB10H11, has been shown to be a versatile ligand for transition metals. The reaction of 9-(CH3)2S-7-[((CH3)3Si) 2CH]CB10H11 and (η-C5H5)Co(CO)2 in refluxing toluene resulted in a complex mixture from which three metallacarborane products could be characterized. Compounds II and III were shown to be the isomeric sandwich complexes 7-(CH3)2S-2-(η-C5H 5)-1-[((CH3)3Si)2CH]-2,1-CoCB 10H9 and 12-(CH3)2S-2-(η-C5H 5)-1-[((CH3)3Si)2CH]-2,1-CoCB 10H9, respectively. Also isolated in trace amounts was the zwitterionic compound IV, 12-[(η-C5H5)Co(η-C5H4)] +[2-(η-C5H5)-1-[((CH3) 3Si)2CH]-2,1-CoCB10H9]-. Reaction of [(η-C5H5)Ni(CO)]2 and 9-(CH3)2S-7-[((CH3)3Si) 2CH]CB10H11 gave 2-(η-C5H6)-1-[((CH3)3Si) 2CH]-2,1-NiCB10H10 (V), while reaction of the carborane with cobalt vapor and toluene gave 2-(η6-C6H5CH3)-1-[((CH 3)3Si)2CH]-2,1-CoCB10H10 (VI). The sandwich structures of compounds of V and VI were confirmed by single-crystal X-ray crystallographic studies. Crystal data for V: space group P1; Z = 2; a = 8.856 (1) ?, b = 17.165 (5) ?, c = 8.647 (1) ?, α = 103.14 (1)°; β = 114.51 (1)°; γ = 85.63 (2)°; V = 1164.5 ?3. The structure was refined to a final R = 0.056 and Rw = 0.069 for the 3726 reflections having Fo2 > 3σ(Fo2). Crystal data for VI: space group P1; Z = 2; a = 8.803 (2) ?, b = 18.007 (5) ?, c = 8.663 (2) ?, α = 101.09 (2)°, β = 114.16 (2)°, γ = 83.07 (2); V = 1228.1 ?3. The structure was refined to a final R = 0.087 and Rw = 0.096 for the 2355 reflections having Fo2 > 3σ(Fo2).
