Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS sup 31 P NMR spectroscopy and x-ray crystallography
- Univ. of Nevada, Reno (USA)
- JEOL NMR Application Lab., Peabody, MA (USA)
- Univ. of Warwick, Coventry (England)
- Univ. of Guelph, Ontario (Canada)
A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type L{sub n}AuX (n = 1, L = DBP, DMPP, Ph{sub 3}P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph{sub 3}P, X = Cl; n = 4, L = DBP, DMPP, X = PF{sub 6}) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP){sub 3}AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS {sup 31}P({sup 1}H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS {sup 31}P({sup 1}H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) {angstrom}) the molecule has effective C{sub s} symmetry as evidenced by the observation of two {sup 31}P resonances in a 2:1 intensity ratio in its CP/MAS {sup 31}P({sup 1}H) NMR spectrum. Variable-temperature {sup 31}P({sup 1}H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs.
- OSTI ID:
- 6902189
- Journal Information:
- Inorganic Chemistry; (USA), Vol. 29:3; ISSN 0020-1669
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
GOLD COMPLEXES
CRYSTAL STRUCTURE
HALOGEN COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
CHEMICAL PREPARATION
EXPERIMENTAL DATA
NMR SPECTRA
PHOSPHORUS 31
PROTONS
BARYONS
COMPLEXES
DATA
ELEMENTARY PARTICLES
FERMIONS
HADRONS
INFORMATION
ISOTOPES
LIGHT NUCLEI
NUCLEI
NUCLEONS
NUMERICAL DATA
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
PHOSPHORUS ISOTOPES
SPECTRA
STABLE ISOTOPES
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
400201* - Chemical & Physicochemical Properties
400202 - Isotope Effects
Isotope Exchange
& Isotope Separation