📜锗烷置于铜 Methyl Chloride体系中,化学反应生成二氯二甲基锗
参考文献:镧系元素的有机金属化合物.64.二甲基锗双(四甲基环戊二烯基)卤化物和镧系元素的烷基衍生物的合成和x射线晶体结构
标题:镧系元素的有机金属化合物.64.二甲基锗双(四甲基环戊二烯基)卤化物和镧系元素的烷基衍生物的合成和x射线晶体结构
摘要:Metathesis Of Me2Gecl2 Or Me2Sncl2 With 2 Equiv Of Lic5Me4H Affords Me2Ge(C5Me4H)2 (1) And Me2Sn(C5Me4H)2 (2),Respectively. The Subsequent Deprotonation Of 1 With Meli Yields Only The Desired Dilithium Salt Me2Ge(C5Me4Li)2 (3) Whereas 2 Forms Me4Sn And Two Lic5Me4H. The Trichlorides Of Neodymium,Samarium,Holmium,And Lutetium React With The Dilithium Salt 3 With The Formation Of Me2Ge(C5Me4)2Lncl2Li(Thf)2 (Ln = Nd (4),Sm (5),Ho (6),Lu (7)). The Reaction Of 4 And 6 With Lich(Sime3)2 Produces Me2Ge(C5Me4)2Lnch(Sime3)2 (Ln = Nd (8),Ho (9)). The New Compounds Have Been Characterized By Elemental Analysis,Mass And NMR Spectra,As Well As X-Ray Structural Analysis Of 5,7,And 9. The Halides 5 And 7 Crystallize In The Monoclinic Space Group P2(1)/c (No. 14) With A = 9.7284 (9),B = 19.397 (1),C = 16.610 (2) Angstrom,Beta = 98.963 (9)-Degrees; Z = 4 Or A = 9.578 (3),B = 19.218 (4),C = 16.525 (4) Angstrom,Beta = 99.73 (2)-Degrees; Z = 4,Respectively. Least-Squares Refinement Led To A Final R Value Of 0.020 (F(O) > 4-Sigma-(F(O))) For 5554 Independent Reflections For 5 Or Of 0.028 (F(O) > 3-Sigma-(F(O))) For 5822 Independent Reflections For 7. Compound 9 Crystallizes In The Monoclinic Space Group P2(1)/m (No. 11) With A = 9.2621 (8),B = 14.216 (2),C = 11.839 (2) Angstrom,Beta = 107.79 (1)-Degrees,Z = 2,And R = 0.023 (F(O) > 4-Sigma-(F(O))) For 2954 Reflections. The Structure Of 9 Shows A Short Ho-C(Methyl) Contact Of 2.774 (4) Angstrom.
Doi:10.1021/om00054A017