Phosphorus vibrational spectroscopy

The purity of the terminal Au-oxo complexes, 3 and 4, was established by several methods including P NMR (3 and 4 have only one phosphorus peak at —8.55 and —13.15 ppm, respectively), cyclic voltammetry, electronic absorption spectroscopy, vibrational spectroscopy, detailed magnetic measurements and elemental analysis on all elements (triplicate analyses for Au) (44). The single peak in the PNMR spectra is consistent with the C2V symmetry of 3 and 4 established by multiple X-ray crystallographic structure determinations and a neutron diffraction study on 3 at liquid He... 

The first fluoroperoxophosphate, (NH4+)P02(02)F H20, has been prepared and characterized by vibrational spectroscopy [64], The peroxide group is bonded in an end-on manner as encountered in simple monoperoxo-derivatives of sulfur and phosphorus. 

Qualitative information on the structure of the colored corrinoids in solution can be extracted rapidly from UVA7is and CD spectra most of the spectroscopic features can be rationalized nowadays by comparison with theoretically calculated spectra. For more precise constitutional information, some of the newly developed methods of mass spectrometry allow the analysis even of the involatile Bi2-derivatives. Modern one-and two-dimensional proton, carbon, nitrogen, and phosphorus NMR spectroscopy has proven a powerful instrument for the delineation of the structure of diamagnetic cobalt-corrins in solution. ESR-spectroscopy has given important information on paramagnetic corrinoid Co -complexes, whether in frozen solutions or bound in corrinoid enzymes. X-ray adsorption fine spectroscopy (EXAFS) spectroscopy and vibrational (IR and Raman) spectroscopy are other spectroscopic techniques used more frequently now in the B12 field. ... 

Ligands such as phosphines (PRj) and arsines (AsRs) (R = alkyl, aryl, halogen, etc.) form complexes with a variety of metals in various oxidation states. Vibrational spectroscopy has been used extensively to determine the structures of these compounds and to discuss the nature of the metal-phosphorus (M-P) bonding. Verkade reviewed spectroscopic studies of M-P bonding with emphasis on cyclic phosphine ligands. 

The initial observation is that PMMA is essentially completely degraded to monomer by heating to 375°C in a sealed tube while heating a mixture of red phosphorus and PMMA under identical conditions yields a solid, non-deqraded, product as well as a lower yield of monomer. One may observe, by 3C NMR spectroscopy, that the methoxy resonance is greatly decreased in intensity and methyl, methoxy phosphonium ions are observed by 31P NMR. Additional carbonyl resonances are also seen in the carbon spectrum, this correlates with a new carbonyl vibration near 1800 cm 1 in the infrared spectrum and may be assigned to the formation of anhydride. The formation of anhydride was also confirmed by assignment of mass spectra obtained by laser desorption Fourier transform mass spectroscopy, LD-FT-MS. 

Yang GC, Xu Y, Hou JB et al (2010) Determination of the absolute configuration of pentacoordinate chiral phosphorus compounds in solution by using vibrational circular dichroism spectroscopy and density functional theory. Chem Eur J 16 2518-2527... 

A review on vibrational and n.m.r. spectroscopy of compounds containing phosphorus-fluorine bonds has been published. The chemistry of phos-phorus(in) fluorides and their co-ordination compounds has been briefly reviewed, and rearrangements of the five-co-ordinate PFg-transition-metal hydride species HM(PF3)4 (M = Co, Rh, or Ir) and [HM(PF3)4] (M = Fe, Ru, or Os), together with M(PFa)5 (M = Fe, Ru, or Os) have been studied. ... 

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