无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2005年
6期
846-851
,共6页
三(3,5-二甲基-1-吡唑)硼氢%钼配合物%碳硼烷%硫族元素%晶体结构
三(3,5-二甲基-1-吡唑)硼氫%鉬配閤物%碳硼烷%硫族元素%晶體結構
삼(3,5-이갑기-1-필서)붕경%목배합물%탄붕완%류족원소%정체결구
hydrotris(3,5-dimethyl-1-pyrazolyl)borate%molybdenum complex%carborane%chalcogenolato%crystal structures
三齿单核三(3,5-二甲基-1-吡唑)硼氢钼配合物Tp*Mo(O)Cl2(1)(Tp*=三(3,5-二甲基-1-吡唑)硼氢HB(C3H(Me2)N2)3)与含硫族元素碳硼烷的锂盐[(THF)3LiE2C2B10H10(THF)]2[E=S(2a),Se(2b),Te(2c)]反应得到了单核配合物Tp*Mo(O)E2C2B10H10[E=S(3a),Se(3b),Te(3c)],产率较好.配合物3a～3c通过红外光谱和元素分析表征,解析了3b的X-射线单晶结构.在空气中,配合物3a可以生成一新颖的含氧桥的双核钼的配合物[HMe2Pz][Tp*Mo(O)(μ2-O)2Mo(O)S2C2B10H10]4a.解析了4a的X-射线单晶结构.Mo-Mo间键长为0.254 83(12)nm,为单键相互作用.
三齒單覈三(3,5-二甲基-1-吡唑)硼氫鉬配閤物Tp*Mo(O)Cl2(1)(Tp*=三(3,5-二甲基-1-吡唑)硼氫HB(C3H(Me2)N2)3)與含硫族元素碳硼烷的鋰鹽[(THF)3LiE2C2B10H10(THF)]2[E=S(2a),Se(2b),Te(2c)]反應得到瞭單覈配閤物Tp*Mo(O)E2C2B10H10[E=S(3a),Se(3b),Te(3c)],產率較好.配閤物3a～3c通過紅外光譜和元素分析錶徵,解析瞭3b的X-射線單晶結構.在空氣中,配閤物3a可以生成一新穎的含氧橋的雙覈鉬的配閤物[HMe2Pz][Tp*Mo(O)(μ2-O)2Mo(O)S2C2B10H10]4a.解析瞭4a的X-射線單晶結構.Mo-Mo間鍵長為0.254 83(12)nm,為單鍵相互作用.
삼치단핵삼(3,5-이갑기-1-필서)붕경목배합물Tp*Mo(O)Cl2(1)(Tp*=삼(3,5-이갑기-1-필서)붕경HB(C3H(Me2)N2)3)여함류족원소탄붕완적리염[(THF)3LiE2C2B10H10(THF)]2[E=S(2a),Se(2b),Te(2c)]반응득도료단핵배합물Tp*Mo(O)E2C2B10H10[E=S(3a),Se(3b),Te(3c)],산솔교호.배합물3a～3c통과홍외광보화원소분석표정,해석료3b적X-사선단정결구.재공기중,배합물3a가이생성일신영적함양교적쌍핵목적배합물[HMe2Pz][Tp*Mo(O)(μ2-O)2Mo(O)S2C2B10H10]4a.해석료4a적X-사선단정결구.Mo-Mo간건장위0.254 83(12)nm,위단건상호작용.
Reactions of tridentate mononuclear hydrotris (3,5-dimethyl-l-pyrazolyl) borate molybdenum(Ⅴ) complex Tp*Mo(O)Cl2 (1) (Tp*=hydrido-tris 3,5-dimethyl-1-pyrazolyl-borate, HB(C3H(Me2)N2)3) with dilithium dichalcogenolate carboranes [(THF)3LiE2C2B10H10(THF)]2 [E=S(2a), Se(2b), Te(2c)] afforded mononuclear complexes Tp*Mo(O)E2C2B10H10 [E=S(3a), Se(3b), Te(3c)] in moderate yields. Complexes 3a～3c have been characterized by IR and elemental analysis. The molecular structure of 3b was determined by X-ray crystallographic analysis. In the air 3a can convert into a novel binuclear oxo molybdenum complex [HMe2Pz][Tp*Mo(O)(μ2-O)2Mo(O)S2C2B10H10] 4a. The molecular geometry of 4a has been determined by a single crystal X-ray structure analysis. According to the short Mo-Mo distance (0.254 83(12) nm), direct metal-metal interaction exists. CCDC: 263618, 3b; 263619, 4a.
