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The First Molybdenum(VI) and Tungsten(VI) Oxoazides MO2(N3)2, MO2(N3)2⋅2 CH3CN, (bipy)MO2(N3)2, and [MO2(N3)4]2− (M=Mo,W) 下载免费PDF全文
Ralf Haiges Juri Skotnitzki Zongtang Fang David A. Dixon Karl O. Christe 《Angewandte Chemie (International ed. in English)》2015,54(33):9581-9585
Molybdenum(VI) and tungsten(VI) dioxodiazide, MO2(N3)2 (M=Mo, W), were prepared through fluoride–azide exchange reactions between MO2F2 and Me3SiN3 in SO2 solution. In acetonitrile solution, the fluoride–azide exchange resulted in the isolation of the adducts MO2(N3)2⋅2 CH3CN. The subsequent reaction of MO2(N3)2 with 2,2′‐bipyridine (bipy) gave the bipyridine adducts (bipy)MO2(N3)2. The hydrolysis of (bipy)MoO2(N3)2 resulted in the formation and isolation of [(bipy)MoO2N3]2O. The tetraazido anions [MO2(N3)4]2− were obtained by the reaction of MO2(N3)2 with two equivalents of ionic azide. Most molybdenum(VI) and tungsten(VI) dioxoazides were fully characterized by their vibrational spectra, impact, friction, and thermal sensitivity data and, in the case of (bipy)MoO2(N3)2, (bipy)WO2(N3)2, [PPh4]2[MoO2(N3)4], [PPh4]2[WO2(N3)4], and [(bipy)MoO2N3]2O by their X‐ray crystal structures. 相似文献
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《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2018,130(27):8211-8215
The reaction of [(Cp*Mo)2(μ‐Cl)2B2H6] ( 1 ) with CO at room temperature led to the formation of the highly fluxional species [{Cp*Mo(CO)2}2{μ‐η2:η2‐B2H4}] ( 2 ). Compound 2, to the best of our knowledge, is the first example of a bimetallic diborane(4) conforming to a singly bridged Cs structure. Theoretical studies show that 2 mimics the Cotton dimolybdenum–alkyne complex [{CpMo(CO)2}2C2H2]. In an attempt to replace two hydrogen atoms of diborane(4) in 2 with a 2e [W(CO)4] fragment, [{Cp*Mo(CO)2}2 B2H2W(CO)4] ( 3 ) was isolated upon treatment with [W(CO)5⋅thf]. Compound 3 shows the intriguing presence of [B2H2] with a short B−B length of 1.624(4) Å. We isolated the tungsten analogues of 3 , [{Cp*W(CO)2}2B2H2W(CO)4] ( 4 ) and [{Cp*W(CO)2}2B2H2Mo(CO)4] ( 5 ), which provided direct proof of the existence of the tungsten analogue of 2 . 相似文献
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The Molybdenum(V) and Tungsten(VI) Oxoazides [MoO(N3)3], [MoO(N3)3⋅2 CH3CN], [(bipy)MoO(N3)3], [MoO(N3)5]2−, [WO(N3)4], and [WO(N3)4⋅CH3CN] 下载免费PDF全文
Prof. Dr. Ralf Haiges Juri Skotnitzki Zongtang Fang Prof. Dr. David A. Dixon Prof. Dr. Karl O. Christe 《Angewandte Chemie (International ed. in English)》2015,54(51):15550-15555
A series of novel molybdenum(V) and tungsten(VI) oxoazides was prepared starting from [MOF4] (M=Mo, W) and Me3SiN3. While [WO(N3)4] was formed through fluoride–azide exchange in the reaction of Me3SiN3 with WOF4 in SO2 solution, the reaction with MoOF4 resulted in a reduction of MoVI to MoV and formation of [MoO(N3)3]. Carried out in acetonitrile solution, these reactions resulted in the isolation of the corresponding adducts [MoO(N3)3?2 CH3CN] and [WO(N3)4?CH3CN]. Subsequent reactions of [MoO(N3)3] with 2,2′‐bipyridine and [PPh4][N3] resulted in the formation and isolation of [(bipy)MoO(N3)3] and [PPh4]2[MoO(N3)5], respectively. Most molybdenum(V) and tungsten(VI) oxoazides were fully characterized by their vibrational spectra, impact, friction and thermal sensitivity data and, in the case of [WO(N3)4?CH3CN], [(bipy)MoO(N3)3], and [PPh4]2[MoO(N3)5], by their X‐ray crystal structures. 相似文献
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