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Synthesis of some phosphino- and arsinobenzenechromium tricarbonyl derivatives and metal carbonyl clusters

1996; NRC Research Press; Volume: 74; Issue: 11 Linguagem: Inglês

10.1139/v96-244

1480-3291

Walter Cullen, Steven J. Rettig, Hongli Zhang,

Metal complexes synthesis and properties

The synthesis of a number of new phosphino- and arsinobenzenechromium tricarbonyl ligands ER 2 C 6 H 5 Cr(CO) 3 (ER 2 = PEt 2 , PPr i 2 , PBu t 2 , PPh 2 , AsPh 2 AsMe 2 ), ER[C 6 H 5 Cr(CO) 3 ] 2 (ER = PEt, PBu t , PPh, AsPh) has been achieved by reacting lithium derivatives of benzenechromium tricarbonyl with appropriate chlorphosphines or iodoarsines. The spectroscopic properties of these ligands are described. The structure of Pr i 2 PC 6 H 5 Cr(CO) 3 was determined by an X-ray crystallographic study. This is the first solid state structure to be reported for a phosphinobenzenechromium tricarbonyl derivative. The structures of four metal carbonyl cluster complexes were also determined. Crystals of Pr i 2 PC 6 H 5 Cr(CO) 3 (3, C 15 H 19 CrO 3 P) are monoclinic, space group P2 1 /c, a = 8.150(2) Å, b = 13.490(2) Å, c = 15.125(1) Å, β = 100.19(1)°, Z = 4; those of Ru 3 (CO) 11 [PPr i 2 C 6 H 5 Cr(CO)3] (15, C 26 H 19 CrO 14 PRu 3 ) are monoclinic, space group P2 1 /n, a = 8.565(2) Å, b = 21.808(3) Å, c = 17.167(3) Å, β = 97.41(2)°, Z = 4; those of Ru 3 (CO) 10 [PPh 2 C 6 H 5 Cr(CO) 3 ] 2 (19, C 32 H 15 CrO 14 PRu 3 ) are orthorhombic, space group Pbca, a = 17.367(4) Å, b = 24.471(5) Å, c = 16.096(3) Å, Z = 8; those of Ru 3 (CO) 10 [PPr i 2 C 6 H 5 Cr(CO) 3 ] 2 •CH 2 Cl 2 (16, C 40 H 38 Cr 2 O 16 P 2 Ru 3 •CH 2 Cl 2 ) are orthorhombic, space group P2 1 2 1 2, a = 13.832(3) Å, b = 17.558(2) Å, c = 10.144(1) Å, Z = 2; and those of Os 3 (CO) 9 [PEt 2 C 6 H 5 Cr(CO) 3 ] 3 (26, C 48 H 45 Cr 3 O 18 Os 3 P 3 ) are trigonal, space group [Formula: see text], a = 15.7558(4) Å, c = 12.662(1) Å, Z = 2. The structures were solved by the Patterson method and were refined by full-matrix least-squares procedures to R = 0.031,0.027, 0.029, 0.025, and 0.029 (R w = 0.027, 0.024, 0.024, 0.023, and 0.025) for 2326, 4110, 3878, 3046, and 4093 reflections with I ≥ 3σ(I), respectively. Key words: metal carbonyl clusters, phosphinobenzenechromium tricarbonyl derivatives, arsinobenzenechromium tricarbonyl derivatives, crystal structures.