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首页> 外文期刊>Inorganica Chimica Acta >An approach to megalo-boranes. Mixed and multiple cluster fusions, involving iridaborane and platinaborane cluster compounds. Crystal structure determinations by conventional and synchrotron methods
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An approach to megalo-boranes. Mixed and multiple cluster fusions, involving iridaborane and platinaborane cluster compounds. Crystal structure determinations by conventional and synchrotron methods

机译：硼烷的一种方法。混合和多簇融合，涉及iridaborane和platinaborane簇化合物。通过常规方法和同步加速器方法确定晶体结构

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Several new macropolyhedral metallaboranes have been isolated from thermolytic mixed cluster fusion reactions involving metallaboranes and molten B_(10)H_(14) as solvent. Co-thermolysis of B_(10)H_(14) with nine-vertex [(CO)(PMe_3)_2HIrB_8H_(12)] (1) engenders 18-vertex [(CO)(PMe_3)_2IrB_(17)H_(20)] (3), via double cluster fusion; this has the 18-vertex configuration of syn-B_(18)H_(22), but with a metal atom in the 10-position. From the same reaction, triple cluster fusion engenders 28-vertex [(PMe_3)_2IrB_(26)H_(24)Ir(CO)(PMe_3)_2] (4), which structurally is based on an intimate interfusion of closed 10-vertex and 12-vertex subclusters, to generate a tetrahedral tetraboron core that also has a more open commo one-boron linkage to a nido nine-vertex {IrB_8} subcluster. Compound 4 exhibits interesting consequences of cluster-crevice formation and introduces the concept of globular megalo-borane structures that have borons-only cores surrounded by boron-hydride sheaths. Examination for incipient megalo-borane globular behaviour in another system, viz. [IrCl(PPh_3)_3] (7) with anti-B_(18)H_(22), reveals a four-atom core feature in 19-vertex [(PPh_3)HIrB_(18)H_(18)(PPh_3)] (6), which has a closo-type {IrB_(10)} 11-vertex subcluster fused to a nido 10-vertex {B_(10)} subcluster to generate a four-atom {IrB_3} tetrahedron. Examination for mixed cluster fusion in other systems reveals the generation of [(PMe_2Ph)_2Pt-anti-B_(18)H_(20)] (8), from the co-thermolysis of [(PMe_2Ph)_2PtB_8H_(12)] (2) and B_(10)H_(14), and examination for multiple cluster fusion reveals the formation of 30-vertex [(PMe_2Ph)_2(PMe_2C_6H_4)_2Pt_2B_(28)H_(32)] (10), 29-vertex [(PMe_2Ph)_2PtB_(28)H_(32)] (11) and 27-vertex [(PMe_2Ph)_2PtB_(26)H_(26)(PMe_2Ph)] (12) from the same reaction. Structurally, compound 10 is based on a 10-vertex arachno-{6,9-Pt_2B_8} unit linked, via one B-B two-electron two-centre bond each, to each, to two 10-vertex nido-{B_(10)} units; it also exhibits molecular condensation in the form of two P-phenylene ortho-cycloboronations. Compound 11 is based on the 19-vertex [(PMe_2Ph)_2Pt-#eta#~4-anti-B_(18)H_(22)] configuration with an additional 10-vertex nido-{B_(10)H_(13)} moiety bound to the non-platinated subcluster via one B-B two-electron two-centre bond. Compound 12 is based on two nido 11-vertex {PtB_(10)} units joined by a single commo Pt vertex, with one of these units conjoined to an arachno eight-boron unit via a two-boron common edge and an open bridging {B-H(exo)-Pt-#mu#-B_2} link. Thermolysis of [(PMe_2Ph)_2PtB_8H_(12)] (2) with the pre-formed double-cluster compound anti-B_(18)H_(12) generates triple-contiguity 27-vertex [(PMe_2Ph)PtB_(26)H_(26)(PMe_2Ph)] (13) which, structurally, consists of a nido 11-vertex {PtB_(10)} unit that is fused to a second 11-vertex nido {PtB_(10)} unit with a triangular {PtB_2} face in common, and also fused to a 10-vertex nido {B_(10)} unit with a {B_2} edge in common. The sequence 12 -> 11 -> 10 -> 13 -> 4 represents a progression of increasing intimacy of cluster fusion. Small crystals of compounds 3, 11 and 12 necessitated synchrotron X-radiation for sufficient diffraction intensity.
机译：已从涉及金属labaranes和熔融的B_（10）H_（14）作为溶剂的热解混合簇融合反应中分离了几种新的大面体金属labaranes。 B_（10）H_（14）与九个顶点[[CO）（PMe_3）_2HIrB_8H_（12）]（1）的共热解产生18个顶点[（CO）（PMe_3）_2IrB_（17）H_（20） ]（3），通过双簇融合;它具有syn-B_（18）H_（22）的18顶点配置，但金属原子位于10位。根据相同的反应，三重簇融合产生了28个顶点[（PMe_3）_2IrB_（26）H_（24）Ir（CO）（PMe_3）_2]（4），其结构是基于封闭10顶点的紧密融合和12顶点子簇，以生成四面体四硼核，该四面体四硼硼核也具有与nido九顶点{IrB_8}子簇更开放的公共单硼键。化合物4表现出簇状缝隙形成的有趣结果，并引入了球形的硼烷结构的概念，该结构具有仅硼的核被氢化硼鞘包围。在另一个系统中检查巨硼烷球状行为，即。 [IrCl（PPh_3）_3]（7）与抗B_（18）H_（22），揭示了19顶点[（PPh_3）HIrB_（18）H_（18）（PPh_3）]中的四原子核心特征6），其具有融合到nido 10顶点{B_（10）}子簇的closo型{IrB_（10）} 11顶点子簇，以生成四原子{IrB_3}四面体。在其他系统中对混合簇融合的检查揭示了[[PMe_2Ph）_2PtB_8H_（12）]的共热解[[PMe_2Ph）_2Pt-anti-B_（18）H_（20）]（8）的产生（2 ）和B_（10）H_（14），检查多簇融合发现形成了30个顶点[（PMe_2Ph）_2（PMe_2C_6H_4）_2Pt_2B_（28）H_（32）]（10），29个顶点[（ PMe_2Ph）_2PtB_（28）H_（32）]（11）和27个顶点[（PMe_2Ph）_2PtB_（26）H_（26）（PMe_2Ph）]（12）。从结构上讲，化合物10基于10个顶点的arachno- {6,9-Pt_2B_8}单元，每个单元通过一个BB两电子两中心键相互连接至两个10个顶点的nido- {B_（10） } 单位;它还以两个对亚苯基邻环硼烷的形式表现出分子缩合。化合物11基于19个顶点[（PMe_2Ph）_2Pt-＃eta＃〜4-anti-B_（18）H_（22）]构型，另外具有10个顶点nido- {B_（10）H_（13） }部分通过一个BB两电子两中心键与未镀铂亚簇结合。化合物12基于两个nido 11顶点{PtB_（10）}单元，该单元通过单个Comm Pt顶点连接，其中一个单元通过两硼共同边缘和开放式桥接{ BH（exo）-Pt-＃mu＃-B_2}链接。 [（PMe_2Ph）_2PtB_8H_（12）]与预先形成的双簇化合物抗-B_（18）H_（12）的热解生成三连续27-顶点[（PMe_2Ph）PtB_（26）H_（ 26）（PMe_2Ph）]（13），其结构上由一个nido 11顶点{PtB_（10）}单元组成，该单元与具有三角形{PtB_2}的第二个11顶点nido {PtB_（10）}单元融合面，并且也融合到具有{B_2}边的10顶点nido {B_（10）}单元上。序列12-> 11-> 10-> 13-> 4表示簇融合的亲密性增加。为了获得足够的衍射强度，化合物3、11和12的小晶体需要同步辐射X射线。

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