摘要
The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a = 15.359(2), b = 18.378(3), c = 24.952(2) A, β = 102.268(4)°, V = 6882.3(1 6) A^3, Mr = 1348.34, Z = 4, Dc = 1.301 g/cm^3, F(000) = 2832 and μ= 0.424 mm^-1 The final R = 0.0606 and wR = 0.1552 for 9396 observed reflections (I 〉 2σ(I)). I contains a [Mo2O3]^3 core in triangular bi-pyralnidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three ,μ-O atoms from C6H5CH2OC6H4O^- bridging ligands. The Mo…Mo distance is 3.30(8) A, indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2 has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.
The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a = 15.359(2), b = 18.378(3), c = 24.952(2) A, β = 102.268(4)°, V = 6882.3(1 6) A^3, Mr = 1348.34, Z = 4, Dc = 1.301 g/cm^3, F(000) = 2832 and μ= 0.424 mm^-1 The final R = 0.0606 and wR = 0.1552 for 9396 observed reflections (I 〉 2σ(I)). I contains a [Mo2O3]^3 core in triangular bi-pyralnidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three ,μ-O atoms from C6H5CH2OC6H4O^- bridging ligands. The Mo…Mo distance is 3.30(8) A, indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2 has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.
基金
This research was supported by NNSFC (No. 90203017 29733090), NBRP (2004CB7201005) and SKLSC