Preparation, characterization, and properties of platinum(0) complexes with tri-n-butyl phosphite, tri-n-butylarsine, and tri-n-butylstibine

Abstract

= 600 Hz). IR: 1512 (s), 1440 (s), 1355 (w), 1301 (w), 1282 (s), 1209 (m), 1169 (w), 1154 (w), 1096 (w), 1076 (w), 1006 (w), 969 (w), 921 (w), 874 (s), 852 (w), 829 (m), 784 (w), 647 (w), 496 (w), 438 (w) cm"1.Preparation of [Mo(Ntol)(S2CNEt2)2]20. A portion of PPh3 (0.128 g; 0.49 mmol) was added to a stirred solution of MoO(Ntol)(S2CNEt2)2 (0.500 g; 0.97 mmol) in CH2C12 (25 mL) at room temperature. After 12 h, the violet solution was taken to dryness, and the purple residue was triturated with Et20 (3 X 25 mL), collected by filtration, and dried in vacuo. Analysis of the Et20 washings by IR and 31P NMR spectroscopy revealed the presence of Ph3PO. Elemental analysis of the purple product indicates that the dimeric complex is obtained as the CH2C12 solvate.

Reversible insertion of carbon dioxide into Pt(ii)–hydroxo bonds

“…Complex 2 exhibits a symmetrical pattern for the BIAN proton resonances in the 1 H NMR spectrum and a strong carbonyl infrared band at 1703 cm −1 . Previously reported κ 2 metal carbonate complexes exhibit carbonyl stretching bands in the 1600 to 1694 cm −1 region 7,9,11,[13][14][15][16][31][32][33][34] of the IR spectrum. When the reaction was performed with labelled 13 CO 2 , a signal assignable to the carbonate carbon was observed at 166 ppm; no Pt satellites were apparent.…”

Syntheses, Spectra, and Structures of (Diphosphine)platinum(II) Carbonate Complexes

“…Syntheses. (LL)Pt(CO 3 ) complexes have been known for some time, generally having been prepared either from (LL)Pt(O 2 ) and CO 2 2,5-7 or from (LL)PtCl 2 and Ag 2 CO 3 . − Platinum carbonate complexes have also been observed to form from adventitious “decomposition” reactions of platinum hydride complexes , or, more recently, from reactions of hydroxide or oxalate complexes. ,− The (LL)Pt(O 2 ) route to carbonate complexes did not appear to offer the generality that we needed, particularly for future studies with other metals. In addition, the dioxygen complexes require a multistep synthesis from standard platinum starting materials.…”

“…(Diphosphine)platinum(II) carbonate complexes, (LL)Pt(CO 3 ), are excellent precursors for the preparation of Pt(II) diolate and alditolate complexes, as well as a number of other (LL)Pt II X 2 and (LL)Pt 0 (L‘) compounds − or by treatment of the corresponding dioxygen complex with carbon dioxide. ,− Difficulties we encountered in reproducing the former preparations and limitations of the latter approach led us to undertake a more detailed study. The underlying problem with the silver carbonate route has been resolved, and additional new synthetic routes have been developed.…”