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Electron Precise Group 5 Dimetallaheteroboranes [{CpV(μ-EPh)}2{μ-η2:η2-BH3E}] and [{CpNb(μ-EPh)}2{μ-η2:η2-B2H4E}] (E = S or Se)
Inorganic Chemistry ( IF 4.6 ) Pub Date : 2018-01-16 00:00:00 , DOI: 10.1021/acs.inorgchem.7b02305 Monojit Ghosal Chowdhury 1 , Subrat Kumar Barik 1 , Koushik Saha 1 , Bakthavachalam Kirubakaran 1 , Abhishek Banerjee 1 , Venkatachalam Ramkumar 1 , Sundargopal Ghosh 1
Inorganic Chemistry ( IF 4.6 ) Pub Date : 2018-01-16 00:00:00 , DOI: 10.1021/acs.inorgchem.7b02305 Monojit Ghosal Chowdhury 1 , Subrat Kumar Barik 1 , Koushik Saha 1 , Bakthavachalam Kirubakaran 1 , Abhishek Banerjee 1 , Venkatachalam Ramkumar 1 , Sundargopal Ghosh 1
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Synthesis and structural elucidation of various electron precise group 5 dimetallaheteroboranes have been described. Room temperature reaction of [Cp2VCl2] with Li[BH3(EPh)], generated from the treatment of LiBH4·THF and Ph2E2 (E = S or Se), for 1 h in toluene, followed by thermolysis, led to the formation of bimetallic complexes [{CpV(μ-EPh)}2{μ-η2:η2-BH3E}], 1 and 2 (1: E = S and 2: E = Se), and [{CpV(μ-SePh)}2{μ-η2:η2-BH(OC4H8)Se}], 3. One of the striking features of these compounds is that they represent a rare class of distorted tetrahedral clusters having bridging hydrogens. Evaluating the skeletal electron pairs and bonding types, compounds 1, 2, and 3 may be considered as isoelectronic with our earlier reported [(CpV)2(B2H6)2]. In an attempt to synthesize the Nb analogues of 1–3, room temperature reactions of [CpNbCl4] and Li[BH3(EPh)] (E = S or Se) were carried out that afforded compounds [{CpNb(μ-EPh)}2{μ-η2:η2-B2H4E}], 4 and 5 (4: E = S and 5: E = Se). The solid-state X-ray structures of both 4 and 5 exemplify electronically saturated [M2B3] systems, and their geometries are analogous to that of [(Cp*MoCl)2B3H7]. For the extension of this work, reaction of [Cp*TaCl4] (Cp* = η5-C5Me5) with Li[BH3(SePh)] was carried out that yielded a tantalaselenaborane cluster [(Cp*Ta)2(μ-Se)B3H6Se(C6H5)] (6). All the new compounds have been characterized using 1H, 11B{1H}, 13C{1H} NMR, UV–vis absorption, and IR spectroscopy, mass spectrometry, and X-ray diffraction studies.
中文翻译：
电子精密组5 Dimetallaheteroboranes [{CPV（μ-EPH）} 2 {μ-η 2：η 2 -BH 3 é}]和[{CPNB（μ-EPH）} 2 {μ-η 2：η 2 -B 2 H 4 E}]（E = S或Se）
已经描述了各种电子精确的5族双金属杂多异戊二烯的合成和结构阐明。[Cp 2 VCl 2 ]与Li [BH 3（EPh）]在LiBH 4 ·THF和Ph 2 E 2（E = S或Se）中的室温反应在甲苯中进行1 h，然后热解，导致双金属络合物的形成[{CPV（μ-EPH）} 2 {μ-η 2：η 2 -BH 3 é}]，1和2（1：E = S和2：E = Se）的和[{CPV（μ-SEPH）} 2 {μ-η 2：η2 -BH（OC 4 H 8）Se}]，3。这些化合物的显着特征之一是它们代表了罕见的一类具有桥连氢原子的扭曲的四面体簇。评价骨骼电子对和接合类型，化合物1，2，和3可被认为是等电子的与我们之前的报道[（CPV）2（B 2 H ^ 6）2 ]。在试图合成的铌类似物1 - 3，的[CpNbCl室温反应4 ]和Li [BH 3（EPH）]（E = S或Se）情况下进行的，得到化合物[{CPNB（μ-EPH）} 2 {μ-η 2：η 2 -B 2 ħ 4 ë}]，4和5（4： E = S和5：E = Se）。4和5的固态X射线结构都是电子饱和[M 2 B 3 ]系统的示例，其几何结构类似于[（Cp * MoCl）2 B 3 H 7 ]的几何结构。用于扩展这项工作的，混合[Cp * TACL的反应4 ]（CP * =η 5 -C 5进行了具有Li [BH 3（SePh）]的Me 5的反应，得到了檀香糖硒化硼烷簇[（Cp * Ta）2（μ-Se）B 3 H 6 Se（C 6 H 5）]（6）。所有新化合物均使用1 H，11 B { 1 H}，13 C { 1 H} NMR，UV-vis吸收，IR光谱，质谱和X射线衍射研究进行了表征。
更新日期：2018-01-16
中文翻译：
电子精密组5 Dimetallaheteroboranes [{CPV（μ-EPH）} 2 {μ-η 2：η 2 -BH 3 é}]和[{CPNB（μ-EPH）} 2 {μ-η 2：η 2 -B 2 H 4 E}]（E = S或Se）
已经描述了各种电子精确的5族双金属杂多异戊二烯的合成和结构阐明。[Cp 2 VCl 2 ]与Li [BH 3（EPh）]在LiBH 4 ·THF和Ph 2 E 2（E = S或Se）中的室温反应在甲苯中进行1 h，然后热解，导致双金属络合物的形成[{CPV（μ-EPH）} 2 {μ-η 2：η 2 -BH 3 é}]，1和2（1：E = S和2：E = Se）的和[{CPV（μ-SEPH）} 2 {μ-η 2：η2 -BH（OC 4 H 8）Se}]，3。这些化合物的显着特征之一是它们代表了罕见的一类具有桥连氢原子的扭曲的四面体簇。评价骨骼电子对和接合类型，化合物1，2，和3可被认为是等电子的与我们之前的报道[（CPV）2（B 2 H ^ 6）2 ]。在试图合成的铌类似物1 - 3，的[CpNbCl室温反应4 ]和Li [BH 3（EPH）]（E = S或Se）情况下进行的，得到化合物[{CPNB（μ-EPH）} 2 {μ-η 2：η 2 -B 2 ħ 4 ë}]，4和5（4： E = S和5：E = Se）。4和5的固态X射线结构都是电子饱和[M 2 B 3 ]系统的示例，其几何结构类似于[（Cp * MoCl）2 B 3 H 7 ]的几何结构。用于扩展这项工作的，混合[Cp * TACL的反应4 ]（CP * =η 5 -C 5进行了具有Li [BH 3（SePh）]的Me 5的反应，得到了檀香糖硒化硼烷簇[（Cp * Ta）2（μ-Se）B 3 H 6 Se（C 6 H 5）]（6）。所有新化合物均使用1 H，11 B { 1 H}，13 C { 1 H} NMR，UV-vis吸收，IR光谱，质谱和X射线衍射研究进行了表征。
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