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Synthesis and Crystal Structure of an Incomplete Cubane-type Mo_3S_4 Cluster with the N-N-O Type Tridentate Ligand: {Mo_3S_4[NH_2CH_2CH(O)CH_2NH_2]_3}(DTP)·(H_2O)_2·(DMF) 被引量:1

Synthesis and Crystal Structure of an Incomplete Cubane-type Mo_3S_4 Cluster with the N-N-O Type Tridentate Ligand: {Mo_3S_4[NH_2CH_2CH(O)CH_2NH_2]_3}(DTP)·(H_2O)_2·(DMF)
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摘要 A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPROH) in a mixed organic solvent, and its crys- tal structure was determined with the following data: Mo3S6PC16H48O8N7, Mr = 977.76, triclinic, space group P1, Z = 2, a = 10.319(2), b = 12.843(3), c = 15.335(3) ?, α = 65.26(3), β = 82.18(3), γ = 70.67(3)o, V = 1741.7(6) ?3, Dc = 1.864 g/cm3, μ = 1.517 mm-1, F(000) = 988, the final R = 0.0794 and wR = 0.2111 for 6318 observed reflections (I>2σ(I)). The structure analysis indicates that all DTP ligands of Mo3S4(DTP)4(H2O) are replaced and each DAPRO molecule acts as a tri- dentate ligand chelating to each Mo atom of the Mo3S4 core. Different from the precursor, the clus- ter symmetry is elevated to C3. In addition, the UV-spectrum of the title compound was measured. A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPROH) in a mixed organic solvent, and its crys- tal structure was determined with the following data: Mo3S6PC16H48O8N7, Mr = 977.76, triclinic, space group P1, Z = 2, a = 10.319(2), b = 12.843(3), c = 15.335(3) ?, α = 65.26(3), β = 82.18(3), γ = 70.67(3)o, V = 1741.7(6) ?3, Dc = 1.864 g/cm3, μ = 1.517 mm-1, F(000) = 988, the final R = 0.0794 and wR = 0.2111 for 6318 observed reflections (I>2σ(I)). The structure analysis indicates that all DTP ligands of Mo3S4(DTP)4(H2O) are replaced and each DAPRO molecule acts as a tri- dentate ligand chelating to each Mo atom of the Mo3S4 core. Different from the precursor, the clus- ter symmetry is elevated to C3. In addition, the UV-spectrum of the title compound was measured.
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2005年第7期751-754,735,共5页 结构化学(英文)
基金 This work was supported by the State Key Basic Research and Development Plan of China (001CB108906)the NNSF of China (20173063) NSF of Fujian Province (E0020001)
关键词 molybdenum-sulfur cluster crystal structure alkaline ligand ligand substitution reaction molybdenum-sulfur cluster, crystal structure, alkaline ligand, ligand substitution reaction
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