Chakraborty D, Chandrasekhar V, Bhattacharjee M, Krätzner R, Roesky H W, Noltemeyer M, Schmidt H G
Institut für Anorganische Chemie, Universität Göttingen, Tammannstrasse 4, D-37077 Göttingen, Germany.
Inorg Chem. 2000 Jan 10;39(1):23-6. doi: 10.1021/ic9907361.
Reactions of Ph2P(O)(OH) and t-BuP(O)(OSiMe3)(OH) with Ti(O-i-Pr)4 in equimolar ratios gave titanium phosphonates of the type [(O-i-Pr)3Ti(mu-O)2PR1R2]2 (1, R1 = R2 = Ph; 2, R1 = t-Bu, R2 = OSiMe3) as colorless crystalline solids in moderate yields. Reactions of Ph2P(O)(OH) and the isopropoxides of zirconium and hafnium resulted in products of the composition [(O-i-Pr)3M(mu-O-i-Pr)2(mu-OPOPh2)M(O-i-Pr)2]Ph2P(O)(OH) (M = Zr (3), Hf (4)) in high yields. The compounds were characterized by 1H, 31P, and 29Si NMR, infrared (IR), and mass spectroscopic (MS) techniques. The molecular structures of 2 and 3 were confirmed by X-ray crystallography.
二苯基膦酸（Ph2P(O)(OH)）和叔丁基膦酸（t-BuP(O)(OSiMe3)(OH)）与四异丙氧基钛（Ti(O-i-Pr)4）以等摩尔比反应，生成了[(O-i-Pr)3Ti(μ-O)2PR1R2]2型（1，R1 = R2 = Ph；2，R1 = t-Bu，R2 = OSiMe3）的钛膦酸盐，为无色结晶固体，产率适中。二苯基膦酸（Ph2P(O)(OH)）与锆和铪的异丙醇盐反应，高产率得到了组成为[(O-i-Pr)3M(μ-O-i-Pr)2(μ-OPOPh2)M(O-i-Pr)2]Ph2P(O)(OH)（M = Zr (3)，Hf (4)）的产物。这些化合物通过1H、31P和29Si核磁共振、红外（IR）和质谱（MS）技术进行了表征。2和3的分子结构通过X射线晶体学得到了证实。
