185249-77-8Relevant academic research and scientific papers
Synthesis of some phosphino- and arsinobenzenechromium tricarbonyl derivatives and metal carbonyl clusters
Cullen, William R.,Rettig, Steven J.,Zhang, Hongli
, p. 2167 - 2181 (2007/10/03)
The synthesis of a number of new phosphino- and arsinobenzenechromium tricarbonyl ligands ER2C6H5Cr(CO)3 (ER2 = PEt2, PPri2;, PBut2, PPh2, AsPh2 AsMe2), ER[C6H5Cr(CO)3]2 (ER = PEt, PBut, PPh, AsPh) has been achieved by reacting lithium derivatives of benzenechromium tricarbonyl with appropriate chlorophosphines or iodoarsines. The spectroscopic properties of these ligands are described. The structure of Pri2PC6H5Cr(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 Pri2PC6H5Cr(CO)3 (3, C15H19CrO3P) are monoclinic, space group P21/c, a = 8.150(2) A, b = 13.490(2) A, c = 15.125(1) A, β = 100.19(1)°, Z = 4; those of Ru3(CO)11[PPri2C6H 5Cr(CO)3] (15, C26H19CrO14PRu3) are monoclinic, space group P21/n, a = 8.565(2) A, b = 21.808(3) A, c = 17.167(3) A, β = 97.41 (2)°, Z = 4; those of Ru3(CO)10[PPh2C6H 5Cr(CO)3]2 (19, C32H15CrO14PRu3) are orthorhombic, space group Pbca, a = 17.367(4) A, b = 24.471(5) A, c = 16.096(3) A, Z = 8; those of Ru3(CO)10[PPri2C6H 5Cr(CO)3]2·CH2Cl2 (16, C40H38Cr2O16P2Ru 3·CH2Cl2) are orthorhombic, space group P21212, a = 13.832(3) A, b = 17.558(2) A, c = 10.144(1) A, Z = 2; and those of Os3(CO)9[PEt2C6H 5Cr(CO)3]3 (26, C48H45Cr3O18Os3P 3) are trigonal, space group P3, a = 15.7558(4) A, c = 12.662(1) A, 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 (Rw = 0.027, 0.024, 0.024, 0.023, and 0.025) for 2326, 4110, 3878, 3046, and 4093 reflections with I ≥ 3σ(7), respectively.
(Benzyne)chromium tricarbonyl. Preparation and structure of Ru3(CO)9{μ3-P[C6H 5Cr(CO)3]}[μ3-C6H 4Cr(CO)3]and Ru3(CO)7(μ3-C6H 4){μ-PPh[C6H5Cr(CO)3]} 2
Cullen, William R.,Rettig, Steven J.,Zhang, Hongli
, p. 2965 - 2969 (2008/10/08)
Ru3(CO)9{μ3-P[C6H 5Cr(CO)3]}[μ3-C6H 4Cr(CO)3] (2) is prepared by reacting Ru3(CO)12 with PhP[C6H5Cr-(CO)3]2. The crystal structure shows the aryne moiety, C6H4Cr(CO)3, η2 bound to three Ru atoms that are part of a Ru3P butterfly arrangement. A Cr→Ru bond is proposed. The P atom is bound to the C6H5Cr(CO)3 moiety and three Ru atoms. In contrast, the product of the thermal decomposition of Ru3(CO)11PPh2[C6H 5Cr(CO)3] is the μ3-η2-benzyne complex Ru3(CO)7(μ3-η2-C 6H4){μ-PPh-[C6H5Cr(CO) 3]}2 (3). Crystals of 2 are monoclinic, with a = 16.918 (2) A?, b = 10.612 (3) A?, c = 19.241 (2) A?, β = 113.64 (2)°, Z = 4, and space group P21/n, and those of 3·CH2Cl2 are monoclinic, with a = 22.411 (2) A?, b = 17.314 (4) A?, c = 26.191 (4) A?, β = 111.68 (1)°, Z = 8 (two molecules per asymmetric unit), and space group P21/n. The structures were solved by heavy-atom methods and were refined by full-matrix least-squares procedures to R = 0.043 and 0.037 for 6096 and 10119 reflections with I ≥ 3σ(I), respectively.
