7783-55-3Relevant articles and documents
Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)]...
Boshaala, Ahmed M. A.,Simpson, Stephen J.,Autschbach, Jochen,Zheng, Shaohui
, p. 9279 - 9292 (2008)
Full title: Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)], [RuBr2(η6-cymene)(PF 2{NMe2})]. Treatment of the dimers [RuX2(η6-cymene)] 2 with PF3 in hot heptane produces the compounds [RuX 2(η6-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(η6-cymene) (PF2{NMe2})] and [RuX2(η6- cymene)(P{NMe2}3)]. Reaction of the dimers [RuX 2(η6-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. 1H, 13C, 31P, and 19F NMR spectra have been obtained where appropriate together with (1H-1H) correlation spectroscopy (COSY) and (13C-1H)-HETCORR spectra of selected compounds. The variation of 1J( 31P-19F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(η6-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(η6- cymene)(PF2{NMe2})] and [RuI2(η 6-cymene)(P{NMe2}3)] at 294 K.
+[Al(ORF)4]-, the salt of a homopolyatomic phosphorus cation
Koechner, Tobias,Engesser, Tobias A.,Scherer, Harald,Plattner, Dietmar A.,Steffani, Alberto,Krossing, Ingo
, p. 6529 - 6531 (2012)
Positive at last: The first condensed-phase homopolyatomic phosphorus cation [P9]+ was prepared using a combination of the oxidant [NO]+ and weakly coordinating anion, [Al{OC(CF 3)3}4]-. [P9]+ consists of two P5 cages linked by a phosphonium atom to give a D2d-symmetric Zintl cluster. NMR (see picture), Raman, and IR spectroscopy, mass spectrometry, and quantum-chemical calculations confirmed the structure. Copyright
PREPARATION AND NUCLEAR MAGNETIC RESONANCE SPECTRA OF AMINODIFLUOROPHOSPORANE
Rankin, David W. H.,Wright, John G.
, p. 2049 - 2050 (1980)
Aminodifluorophosphorane has been prepared by the reaction in solution of difluorophosphine and ammonia.N.m.r. spectra indicate that the fluorine atoms are in axial positions and that the amino-group atoms lie in a plane perpendicular to the equatorial plane.At 215 K there is no evidence for rotation about the P-N bond or for fluxional behaviour.The compound is thermally unstable, and has not been isolated.
EPR Spectrum of CuPF3
Histed, M.,Howard, J. A.,Jones, R.,Tomietto, M.
, p. 1141 - 1143 (1992)
CuPF3 is formed from Cu atoms and PF3 on solid adamantane at 77 K in a rotating cryostat.It has the magnetic parameters a63 = 4205 +/- 10 MHz, a31 = 1100 +/- 10MHz, a19 = 90 +/- 10MHz, and g = 1.999 +/- 0.002, has a 2A1 electronic ground state in the point group C3v, and can be considered to be a copper-centered radical and not a phosphoranyl formed by addition of a Cu atom to PF3.About 70percent of the unpaired spin is located in the metal 4s orbital, 8percent in the P 3s orbital, and 0.5percent in the F 2s orbitals for a total unpaired spin s population of 78.5percent.The remaining 21.5percent of unpaired spin is probably located in Cu 4p orbital.Cu3 is also formed in adamantane and does not appear to react with PF3.Cu7 rather than CuPF3 is formed in solid cyclohexane and is also unreactive toward PF%.
Yost, M.,Anderson, T. F.
, p. 624 - 627 (1934)
1,3,2-Dithiaphospholanes with an annelated 1,2-dicarba-closo- dodecaborane(12) unit: Formation and reactivity
Wrackmeyer, Bernd,Klimkina, Elena V.,Milius, Wolfgang
, p. 5021 - 5043 (2014/04/03)
1,3,2-Dithiaphospholanes were prepared, containing an annelated 1,2-dicarba-closo-dodecaborane(12) unit, bearing halogens (F, Cl, Br, and I), H, NEt2, OEt groups, or organo substituents (R = i-Pr, t-Bu, Cy, 3,5-Me2-C6H3-CH2, Ph) at phosphorus. The t-Bu derivative was structurally characterised as its sulfide. The organo-substituted derivatives escape the ring strain by irreversible (R = t-Bu; X-ray analysis) or reversible dimerisation, by which 10-membered rings are formed. Using 1,1-bis(dichlorophosphino)methane, another dimer containing a 14-membered ring could be isolated and structurally characterised. The preferred conformation of the 1,3,2-dithiaphospholanes depends on the nature of the substituent at phosphorus. For instance, the substituents R = t-Bu, NEt 2 prefer the equatorial position, as indicated by diagnostic NMR data, supported by DFT calculations [B3LYP/6-311+G(d,p) level of theory]. The calculations also predict the tendency for dimerisation, and calculated NMR parameters are in good agreement, in most cases, with experimental data.
