Preparation and chemical and spectroscopic properties of bis(difluorophosphino) selenide
作者:David E. J. Arnold、Ernest R. Cromie、David W. H. Rankin
DOI:10.1039/dt9770001999
日期:——
Bis(difluorophosphino) selenide has been prepared by the exchange reactions of PBrF2 and PCLF2 with Se(SiH3)2 and Se(SnBu3)2. It has been characterised by vrbrational, mass, n.m.r., and photoelectron spectroscopy. Spectroscopic results have also been obtained for bis(difluorophosphino) sulphide, prepared by analogous methods. Both compounds react with Brønsted acids to give PF2HSe or PF2HS, and a difluorophos-phine
通过PBrF 2和PCLF 2与Se(SiH 3)2和Se(SnBu 3)2的交换反应制备了双(二氟膦基)硒化物。它的特征是可变光谱,质谱,核磁共振和光电子能谱。通过类似方法制备的双(二氟膦基)硫化物也获得了光谱结果。两种化合物均与布朗斯台德酸反应生成PF 2 HSe或PF 2 HS,以及该酸的二氟膦衍生物。通过与乙硼烷反应生成单硼烷加合物,以及从[Mo(C 7 H 8)(CO)4 ]。后一反应说明了这些化合物作为螯合双齿配体的潜在用途。与氯一起,硒化物产生PCl 3 F 2和PClF 2 Se。
Reactions between carbonylhydridotris(triphenylphosphine)iridium(I) and difluorophosphine oxide, sulphide, and selenide: identification of ionic intermediates
作者:E. A. V. Ebsworth、Philip G. Page、David W. H. Rankin
DOI:10.1039/dt9840002569
日期:——
Carbonylhydridotris(triphenylphosphine)iridium(I)(1) reacts with PF2HY (Y = O, S, or Se) at 190 K in CH2Cl2 to give [Ir(CO)H2(PPh3)3][PF2Y](2), identified by n.m.r. spectroscopy. When the solutions were allowed to warm above 220 K, PPh3 was liberated and complexes [Ir(CO)H2(PPh3)2(P′F2Y)] were formed [Y = Se, (3a); S, (3b); or O, (3c)]. Complexes (3a) and (3b) were initially produced in two isomeric
Preparation, structures, and reactions of some difluorothiophosphonate and difluoroselenophosphonate complexes of platinum(II)
作者:J. Andrew S. Duncan、E. A. V. Ebsworth、Robert O. Gould、C. Lynn Jones、David W. H. Rankin、John D. Whitelock
DOI:10.1039/dt9810001028
日期:——
have been prepared by the reaction of trans-[PtH(PEt3)2X] with PF2H(Y). The reactions have been studied at low temperatures using 31P and 19F n.m.r. spectroscopy; the formation of [PtIVH2(PEt3)2(PF2Y)X] and [PtIIH(PEt3)2(PF2Y)] as intermediates was observed, and a mechanism has been proposed. The complexes [Pt(PEt3)2(PF2Y)X](X = H, Cl, Br, or l) were also prepared by reaction of [Pt(PEt3)3X][BPh4] with
配合物[Pt(PEt 3)2(PF 2 Y)X](X = Cl,Br或I; Y = S或Se)已通过反式-[PtH(PEt 3)2 X的反应]制备。 PF 2 H(Y)。已经在低温下使用31 P和19 F nmr光谱研究了反应;观察到了作为中间体的[Pt IV H 2(PEt 3)2(PF 2 Y)X]和[Pt II H(PEt 3)2(PF 2 Y)]的形成,并提出了机理。络合物[Pt(PEt3)[Pt(PEt 3) 3 X] [BPh 4 ]与PF 2 H(Y)的反应也可以制备2(PF 2 Y)X](X = H,Cl,Br或l):氢化物配合物在室温下稳定。获得反式-[PtCl(PEt 3) 2(PF 2 S)]的X射线晶体结构。晶体是正交晶体,空间群Pbcn, a = 1.1597(2), b = 1.3355(2), c = 1.3632(3)nm。该结构已用934衍射仪数据解决,并已用876数据精修到R=