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PHOSPHORUS-31 NMR STUDIES ON BIS(diphenylphosphino)-METHANE-BRIDGED PALLADIUM-SILVER HETERODINUCLEAR COMPLEXES

Chinese Journal of Structural Chemistry 1991年第1期 70-76页

作者： Lu Shi-JieLanzhou Institute of Chemical Physics, Academia Sinica, 730000

Bis (diphenylphosphino) methane (dppm)-bridged Pd-Ag complexes of nitrate,nitrite, acetate and formate have been prepared by treatment of trans- (NC)2Pd (dppm)2 with suitable silver salts respectively and characterized by elemental analysis, infrared spectroscopy,and by proton,carbon-13,phosphorus-31 nmr spectroscopies. Their 31P- {1H} nmr spectra have been analyzed by using the Bruker PANIC program for spectrum simulation to find the correct chemical shifts of the phosphorus atoms and P-P,P-Ag coupling constants of these complexes, each of which is a mixture of a pair of silver-107 and silver-109 isotopic isomers. A comparison of the 31P nmr data for trans-(NC)2Pd-(μ-dppm)2Ag(NO2) and for fo-oBs-(NC)2Pd(>-dppm)2Ag(NO3) shows that the additional oxygen atom in the nitrate complex withdraws p electron density, rather than s, from the silver moiety. Also a comparison of the 31P nmr data for trans- (NC)2Pd(μ-dppm)2Ag (OOCH) and for trans-(NC)2Pd(μ-dppm)2Ag(OOCCH3) shows that the methyl group in the acet

关键词： PHOSPHORUS-31 NMR STUDIES ON BIS METHANE-BRIDGED PALLADIUM-SILVER HETERODINUCLEAR COMPLEXES diphenylphosphino NC Ag NMR

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SYNTHESIS AND CRYSTAL STRUCTURE OF A HETERODINUCLEAR COMPLEX OF PALLADIUM SILVER WITH BRIDGING BIS-( diphenylphosphino ) METHANE [ 1 ]

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Chinese Journal of Structural Chemistry 1990年第2期 154-158页

作者： F.R.Fronczek,J.Selbin Department of Chemistry Louisiana State University Baton Rouge Louisiana 70803 U.S.A. Department of Chemistry Louisiana State University Baton Rouge Louisiana 70803 U.S.A.

A heterodinuclear complex, trans- dicyano- palladium (Ⅱ)- bis [β- bis (diphenylphosphino)methane]-nitritosilver(Ⅰ),has been prepared by treatment of trans-(NC)2Pd(dppm)2 with AgNO2 and characterized by elementary analysis, ir, nmr, and X-ray crystal structure determination. AgPdC52H44N3O2P4,Mr= 1081. 12,monoclinic,space group P21/c,a=14. 745(7),b= 19. 208(7),c= 17. 486(6) A ,β=94. 99°(2) ,and Z = 4. The final R=0. 032 for 8673 unique reflections. In the molecule,the Pd -Ag distance is 3. 205 A. The palladium moiety has an approximately square planar geometry, and the silver moiety has a severely distorted tetrahedral geometry.

关键词： Ag METHANE SYNTHESIS AND CRYSTAL STRUCTURE OF A HETERODINUCLEAR COMPLEX OF PALLADIUM SILVER WITH BRIDGING BIS diphenylphosphino

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PREPARATION, PROPERTIES, AND MOLECULAR STRUCTURE OF trans-DICYANO BIS[BIS(diphenylphosphino) METHANE]PALLADIUM (Ⅱ)

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Chinese Journal of Structural Chemistry 1992年第1期 20-23页

作者： Selbin J. Fronczek F.R. Baton Rouge U. S. A. Department of Chemistry. Louisiana State University LA 70803

The crystal structure of the title compound has been determined. PdC52H44N2P4, Mr = 927. 2, monoclinic, space group P21 /n, a =12. 102(2), b = 9.997(2), c=20. 254(5)(?),β=93. 80(2)°, V = 2445. 0(?)3, Z = 2, R =0. 075 and Rw = 0. 095 for 3535 observed reflections (I>3σ(I)), The palladium atom is located on the symmetric center and adopts a square planar coordination surroundings with two biphosphine ligands and two cyanide groups. The molecular structure in crystals is different from that in solution in which the molecule is very fluxional, probably due to the rapid alteration in coordination sites between the coordinated and uncoordinated phosphorus atoms of the biphosphine ligands. Their properties are also reported.

关键词： AND MOLECULAR STRUCTURE OF trans-DICYANO BIS[BIS diphenylphosphino METHANE]PALLADIUM PREPARATION PROPERTIES

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