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. 2010 Dec 8;67(Pt 1):m42. doi: 10.1107/S1600536810050506
Experimental. Reaction: bis(diphenylphosphino)-1,2-dimethylhydrazine: 146 mg (0.34 mmol), (THT)AuCl: 200 mg (0.68 mmol), THF: 2 ml, DCM: 5 ml, Yield: 89% Grey crystals or white precipitate. Crystals are insoluble in organic and highly polar solvents. 1H NMR: (CDCl3, 300 MHz) δH 7.85 (dd, Arom, J (1H-31P) = 13.2, J (1H-1H) = 8.1), 7.52 (t, Arom, J (1H-1H) = 9.40 Hz), 7.40 (dd, Arom, J (1H-31P) = 17.7, J (1H-1H) = 7.4), 2.76 (d, CH3, 3J = 7.8 Hz). 13C NMR: Compound too insoluble in NMR solvents. 31P NMR: (CDCl3, 121 MHz) δP 87.1. MS: No useful information could be obtained. EA: Calc: (Au2Cl2P2N2C26H26) C 34.96%, H 2.93%, N 3.14% Found: C 35.29%, H 2.93%, N 3.13%. MP: 228 - 230 °C.
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.