STUDIES ON THE INTERACTIONS OF (ETA5-C5H5)M(CO)2 COMPLEXES (M=CO, RH) WITH 1,2-BIS(PHENYLETHYNYL)BENZENE, AND AN X-RAY CRYSTALLOGRAPHIC CHARACTERIZATION OF ONE OF THE PRODUCTS - (ETA5-C5H5CO)2(C6H5C2C6H4C2C6H5)2
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Title full: Studies on the interactions of (5-C5H5)M(CO)2 complexes (M = Co, Rh) with 1,2-bis(phenylethynyl)benzene, and an x-ray crystallographic characterization of one of the products: (5-C5H5Co)2(C 6H4C2C6 H4C2C6H5)2. The reaction of (5-C5H5)Co(CO)2 (1) and l,2-bis(phenylethynyl)benzene (4) has been shown to produce as major products a dimeric organic compound of composition C44H28, postulated to be 1,2,4-triphenyl-3-(o-phenylethynylphenyl)biphenylene (7), and bis(5-C5H5Co)2(C 6H5C2C6H 4C2C6H5)2 (9). Minor organometallic products also obtained include a bis(4-cyclopentadienone)dicobalt complex (12) and several mononuclear complexes resulting from co-condensation of 4 and 7 with 1. A corresponding reaction betwen (5-C5H5)Rh(CO)2 (2) and 4 has produced several organorhodium complexes in low yield, including a mixed (4-cyclobutadiene)(4-cyclopentadienone)d irhodium derivative (17). Complexes 9, 12 and 17 are derived from the intermolecular condensation of two molecules of 4 with either 1 or 2. An X-ray diffraction investigation of 9 has been undertaken, and unequivocally confirms the unique structural nature of this complex to be that of the b isomer. 9b crystallizes in the monoclinic space group P21/n with cell dimensions: = 10.652(5), b = 23.690(6), c = 17.204(4) , and = 90.21(3); v = 4341(4) 3. The unit cell was found to contain one solvent benzene for each molecule, yielding a calculated density of 1.351(1) g/cm3 with Z = 4. Intensity data were collected using Mo-K radiation ( = 0.71073 ) by the 2 scan method with an automated 4-circle diffractometer (Enraf-Nonius CAD-4). In all, 8286 reflections were scanned, of which 5192 were independent wit an intensity greater than 3. Refinement by full matrix Least squares led to a final unweighted R of 0.037 (Rw = 0.050). The atoms of the (-C5H5)Co(C4) moieties are well-behaved crystallographically and have molecular parameters which are within accepted values of recent determinations of other complexes containing that moiety. 1981.
