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新颖五核Mo/Cu/S簇合物[MoOS_3Cu_4(α-MePy)_6Br_2]的合成及晶体结构

Synthesis and Crystal Structure of a Novel Pentanuclear Mo/Cu/S Cluster Compound [MoOS_3Cu_4(α-MePy)_6Br_2]
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摘要 Reaction of(NH 4) 2MoOS 3 with CuBr and AgBr(molar ratio=1∶4∶1) in α-MePy produced dark red crystals of [MoOS 3Cu 4(α-MePy) 6Br 2]. The product was characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in a triclinic system with space group P1 and unit cell parameters a=0.950 9(3) nm, b=1.066 8(2) nm, c=2.153 6(3) nm, α=94.846(9)°, β=92.054(7)°, γ=99.299(8)°, V=2.145 5(8) nm 3, Z=2, D c=1.828 g·cm -3, F(000)=1 168, μ=42.79 cm -1, R=0.049 and R w=0.051. The compound consists of a nido-shaped MoS 3Cu 3 cluster unit and a four-membered CuBrCuS ring by sharing the same Cu3—S3 bond. The Mo atom and the four Cu atoms adopt a distorted tetrahedral geometry coordination. The Mo…Cu1, Mo…Cu2 and Mo…Cu3 distances are 0.271 1(3), 0 269 8(2), and 0.268 1(1) nm, respectively. Reaction of(NH 4) 2MoOS 3 with CuBr and AgBr(molar ratio=1∶4∶1) in α-MePy produced dark red crystals of [MoOS 3Cu 4(α-MePy) 6Br 2]. The product was characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in a triclinic system with space group P1 and unit cell parameters a=0.950 9(3) nm, b=1.066 8(2) nm, c=2.153 6(3) nm, α=94.846(9)°, β=92.054(7)°, γ=99.299(8)°, V=2.145 5(8) nm 3, Z=2, D c=1.828 g·cm -3, F(000)=1 168, μ=42.79 cm -1, R=0.049 and R w=0.051. The compound consists of a nido-shaped MoS 3Cu 3 cluster unit and a four-membered CuBrCuS ring by sharing the same Cu3—S3 bond. The Mo atom and the four Cu atoms adopt a distorted tetrahedral geometry coordination. The Mo…Cu1, Mo…Cu2 and Mo…Cu3 distances are 0.271 1(3), 0 269 8(2), and 0.268 1(1) nm, respectively.
出处 《高等学校化学学报》 SCIE EI CAS CSCD 北大核心 2004年第5期814-816,共3页 Chemical Journal of Chinese Universities
基金 国家自然科学基金 (批准号 :2 0 2 710 3 6) 江苏省教育厅自然科学研究基金(批准号:0 2KJB15 0 0 0 1) 南京大学配位化学国家重点实验室开放基金 江苏省有机合成重点实验室开放基金资助
关键词 杂核金属含硫簇合物 合成 晶体结构 五核钼/铜/硫簇合物 Mo/Cu/S cluster Synthesis Crystal structure
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参考文献12

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