Carbonylcobalt(I) complexes. The crystal and molecular structure of [Co(CO)(dppm)2]ClO4 |
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| Institution: | 1. Instituto de Física de São Carlos, Universidade de São Paulo, CP 369, 13560-970 São Carlos, SP, Brazil;2. Université Paris-Saclay, Faculté de Pharmacie, CNRS UMR 8076, 92296 Châtenay-Malabry, France;3. Institut Curie, CNRS UMR 9187, INSERM U1196 Chimie et Modélisation pour la Biologie du Cancer, 91405 Orsay, France;1. Rare Disease & LCM Laboratories, Daiichi Sankyo Co., Ltd, 1-2-58 Hiromachi, Shinagawa-ku, Tokyo 140-8710, Japan;2. Biologics & Immuno-Oncology Laboratories, Daiichi Sankyo Co., Ltd, 1-2-58 Hiromachi, Shinagawa-ku, Tokyo 140-8710, Japan;3. Modality Research Laboratories, Daiichi Sankyo Co., Ltd, 1-2-58 Hiromachi, Shinagawa-ku, Tokyo 140-8710, Japan;4. Pain & Neuroscience Laboratories, Daiichi Sankyo Co., Ltd, 1-2-58 Hiromachi, Shinagawa-ku, Tokyo 140-8710, Japan;5. Drug Metabolism & Pharmacokinetics Research Laboratories, Daiichi Sankyo Co., Ltd, 1-2-58 Hiromachi, Shinagawa-ku, Tokyo 140-8710, Japan;1. Graduate School of Pharmaceutical Sciences, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113-0033, Japan;2. Pharmaceutical Research Center, Shionogi & Co. Ltd., Futaba-cho, Toyonaka, Osaka 561-0825, Japan;3. Laboratory for Metabolomics, RIKEN Center for Integrative Medical Sciences, Suehiro-cho, Tsurumi-ku, Yokohama, Kanagawa 230-0045, Japan;1. Nikolaev Institute of Inorganic Chemistry, Siberian Branch of Russian Academy of Sciences, 3, Acad. Lavrentiev Ave., Novosibirsk 630090, Russian Federation;2. N. N. Vorozhtsov Novosibirsk Institute of Organic Chemistry, Siberian Branch of Russian Academy of Sciences, 9, Acad. Lavrentiev Ave., Novosibirsk 630090, Russian Federation |
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| Abstract: | New anionic carbonylcobalt(I) complexes X2Co(CO)2(PPh3)](PR4) (X=Cl, PR4 = PBzPh3 (I); X = Br, PR4 = PEtPh3 (II)) have been prepared by reduction of the cobalt(II) halides with NaBH4 in the presence of PPh3 and the phosphonium salt PR4X. Cleavage of halide bridges in dimeric or polymeric XCo(PPh3)2]n and XCo(PPh3)]n gives the neutral dicarbonyl derivatives XCo(CO)2PPh3)2. Treatment of ClCo(CO)2(PPh3)2 with alkylating agents gives the known σ- and η- organocobalt(I) derivatives, and reactions with TIClO4 in the presence of various amounts of different mono- and bi-dentate phosphines give the cationic tricarbonyl Co(CO)3(PPh3)2]+, dicarbonyl Co(CO)2(PMePh2)3]+ and monocarbonyl Co(CO)L4]+ complexes (L4 = 4P(OMe)3, 2 dppe and 2dppm). The dppm complex crystallizes in the monoclinic space group P21/c with a 17.895(6), b 10.751(2), c 24.687(4) Å, β 98.92(1)°, and Dcalc 1.35 g cm−3 for Z = 4. A final R value of 0.077 ( Rw = 0.061), based on 2656 observed reflections, was obtained. The cobalt atom exhibits a distorted trigonal bipyramidal geometry. The perchlorate anion is severely disordered or freely rotating. |
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