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在氩气保护下,以邻位-碳硼烷、正丁基锂、硒粉和CpCo(CO)I2为起始原料,合成、分离得到配合物CpCo(Se2C2B10H10)(1)、(CpCo)2(Se2C2B10H10)(2)和(CpCo)4(μ3-Se)4Co2(μ3-Se2C2B10H10)4Co·CH2Cl2(3),并用元素分析、质谱、IR、1H NMR及X-射线单晶衍射对配合物(3)进行了表征。晶体属正交晶系,空间群P212121,其晶胞参数为:a=1.307 20(13)nm,b=1.391 37(11)nm,c=3.885 33(15)nm,β=90°,Z=4,V=7.066 6(9)nm3,μ=7.890 mm-1,Dc=2.138 g·cm-3,F(000)=4 268,R1=0.054 3,wR2=0.136 3。配合物中4个(Se2C2B10H10)2-配体和4个单硒基团形成了1个Co7Se12核。
The complexes CpCo (Se2C2B10H10) (1), (CpCo) 2 and CpCo (CO) 2 were synthesized and separated under ortho-position using carborane, n-butyllithium, (Se2C2B10H10) (2) and (CpCo) 4 (μ3-Se) 4Co2 (μ3-Se2C2B10H10) 4Co · CH2Cl2 (3) were synthesized and characterized by elemental analysis, mass spectrometry, IR, 1H NMR and X-ray single crystal diffraction. 3) Characterized. The crystal belongs to the orthorhombic and space group P212121 with unit cell parameters of a = 1.307 20 (13) nm, b = 1.391 37 (11) nm, c = 3.885 33 = 4, V = 7.066 6 (9) nm3, μ = 7.890 mm-1, Dc = 2.138 g · cm -3, F (000) = 4 268, R1 = 0.054 3, wR2 = 0.136 3. Four (Se2C2B10H10) 2 - ligands and four single selenium groups in the complex formed a Co7Se12 core.