Syntheses, characterizations, and reactivities of new 1,4,7-trimethyl-l,4,7-triazacyclononane (Me3tacn) molybdenum and tungsten complexes
作者： Cai-Xia Zhang , Duo-Wen Fang , Jun-Ling Wang , Ai-Quan Jia , Qian-Feng Zhang
DOI: 10.1016/J.ICA.2020.119599
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摘要: Abstract The reported complexes of [(Me3tacn)M0(CO)3] (Me3tacn = 1,4,7-trimethyl-1,4,7-triazacyclononane; M = W, 1a; Mo, 1b), [(Me3tacn)MII(CO)3I](PF6) (M = W, 2a; 2b), [(Me3tacn)MVOCl2](PF6) 3a; 3b), and [(Me3tacn)MVIO3]·4H2O 4a; 4b) were synthesized as tungsten molybdenum precursors according to the works by Wieghardt [20,21,24]. Reaction 2a with sodium dialkyl dithiocarbamate afforded [(Me3tacn)WII(CO)2(S2CNR2)]I (R = Me, 5a; iPr, 6a). Similar reaction using 2b gave rise isolations [(Me3tacn)MoII(CO)2(S2CNR2)](PF6) 5b; 6b; nPr, 7). Hydrolysis 3b in acetonitrile a dimeric complex [{(Me3tacn)MoVO(OH)}2(μ-O)](PF6)2·2MeCN (8). Treatment 4b diisopropyl presence HPF6 yielded [(Me3tacn)MoVIO2S] (9), while similar S8 powder oxotetrasulfido [(Me3tacn)MoIVO(S4)] (10). All are well characterized electronic, infrared, NMR spectroscopies, solid-state structures 1a/b, 2a, 3b, 4a/b, 5a/b, 6a/b, 7–10 have been also established single-crystal X-ray diffraction. electrochemical properties these investigated paper.
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