Scrambling of Metal Precursors: A Strategy to Synthesize Trinuclear [M3(µ-Se)2(dppe)3]2+ (M = Ni, Pd) and Pentanuclear [Pd5(μ3-Se)4(dppe)4]2+ Coordination Clusters
Scrambling of Metal Precursors: A Strategy to Synthesize Trinuclear [M3(µ-Se)2(dppe)3]2+ (M = Ni, Pd) and Pentanuclear [Pd5(μ3-Se)4(dppe)4]2+ Coordination Clusters
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金属前驱体的置乱：合成三核 [M3(µ-Se)2(dppe)3]2 (M = Ni, Pd) 和五核 [Pd5(μ3-Se)4(dppe)4]2 配位团簇的策略
DOI：
10.1007/s10876-023-02458-z
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发表时间：
2024
影响因子：
2.8
通讯作者：
Butcher, Raymond J.
中科院分区：
文献类型：
--
作者：
Kulkarni, Atharva Yeshwant;Lokhande, Saili Vikram;Siddiki, Afsar Ali;Chauhan, Rohit Singh;Butcher, Raymond J.
[PdCl2(Dppe)]与两个当量的吡啶基硒酸酯钠盐反应，得到顺式配合物[Pd{2-SeC5H3(5-R)N}2(Dppe)](R=H，Me)。后者与两个等价物[NiCl2(Dppe)]反应生成了边心三核配合物[Ni3(μ-Se)2(Dppe)3]Cl2(2)和同金属五核聚集体[Pd5(μ3-Se)4(Dppe)4][BPh4]2(3)。同样的反应与[Ni(SeC5H4N)2(Dppe)]和[PdCl2(Dppe)]以1：2的摩尔比相互作用，得到了三核化合物[M3(μ-Se)2(Dppe)3]2+(M=Ni，Pd)和一个未知的不溶基质。通过1H、13C{1H}、31P{1H}、77Se{1H}核磁共振、红外光谱和显微分析对所合成的化合物进行了表征。通过单晶X射线分析确定了配合物[Pd{2-SeC5H3(5-Me)N}2(Dppe)]和[Pd5(μ3-Se)4(Dppe)4][BPh 4]2的分子结构。在配合物[Pd_5(μ_3-Se)_4(Dppe)_4][BPh_4]_2中，钯金属占据了正方锥体几何构型的一角，二聚体单元内的Pd···Pd距离为3.1087°，而轴向钯-赤道距离为3.363°和3.067°。
Reaction of [PdCl2(dppe)] with two equivalents of the sodium salt of pyridyl selenolate affordedcisconfigured complex [Pd{2-SeC5H3(5-R)N}2(dppe)] (R = H, Me). The latter complexes on reacting with two equivalent of [NiCl2(dppe)] yielded an edge centered trinuclear complex [Ni3(μ-Se)2(dppe)3]Cl2(2) and homometallic pentanuclear aggregates of composition [Pd5(μ3-Se)4(dppe)4][BPh4]2(3). Interplaying the same reaction in 1:2 molar ratio with [Ni(SeC5H4N)2(dppe)] and [PdCl2(dppe)], resulted in trinuclear compounds [M3(μ-Se)2(dppe)3]2+(M = Ni, Pd) and an unidentified insoluble matrix. All the synthesized complexes were characterized by1H,13C{1H},31P{1H},77Se{1H} NMR, IR and microanalysis. The molecular structure of the complex [Pd{2-SeC5H3(5-Me)N}2(dppe)] and [Pd5(μ3-Se)4(dppe)4][BPh4]2were established through single crystal X-ray analysis. In complex [Pd5(μ3-Se)4(dppe)4][BPh4]2, the palladium metals occupied the corner of square pyramidal geometry and the Pd···Pd distance within the dimeric unit is 3.1087 Å whereas the axial palladium-equatorial distance are 3.363 Å and 3.067 Å.