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As found from X-ray data (Figure
[1]
), the copper atom in the structure of (Ph2PCl)3CuI adopts a tetrahedral coordination. The copper and chlorine atoms are situated
on either sides of the plane of phosphorus atoms. The Cu(1) atom is deviated from
the plane of P(1), P(2) and P(3) atoms to 0.75 Å. Also, the chlorine atoms are antiperiplanar
to the iodine atom, the torsion angle ClPCuI is equal to 167° on an average. X-ray
investigation of structure 1 was carried out on Bruker Smart CCD 1000 diffractometer at 293 K. Crystals are monoclinic,
a = 20.381(4), b = 9.462(2), 20.411(4) Å, β = 112.395(4)°, space group P21/c, Z = 4 M = 852.3, F(000) = 1696, µ[MoK& agr;] = 18.25 cm-1. Intensities of 27979 reflections were measured and 10473 independent reflections
were used for further refinement. The refinement was converged to wR2 = 0.0623 and GOF = 0.980 for all independent reflections [R1 = 0.0325 was calculated against F2 for 5790 observed reflections with I > 2 σ(I)].
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For example: 2-(2-Pyridyl)ethynyldiphenylphosphane(3g): Yield: 93%; light yellow solid; mp 32 °C. 31P{H} NMR (162.6 MHz, CDCl3): δ = -34.44 (s). 1H NMR (400 MHz, CDCl3): δ = 6.98 (m, 1 H), 7.19 (m, 1 H), 7.21 (m, 7 H), 7.37 (m, 1 H), 7.61 (dt, 4 H,
J = 1.4 Hz), 8.43 (m, 1 H). 13C NMR (100.6 MHz, CDCl3): δ = 86.11 (d, J = 9.8 Hz), 106.22, 122.74, 126.78, 128.15 (d, J = 7.6 Hz), 128.69, 132.30 (d, J = 21.3 Hz), 134.79 (d, J = 7.5 Hz), 135.55, 142.04, 149.46. (3-Methoxyprop-1-ynyl)(diphenyl)phosphane(3j): Yield: 49%; light yellow oil; bp 160 °C/0.1 Torr. 31P{H} NMR (162.6 MHz, CDCl3): δ = -34.62 (s). 1H NMR (400 MHz, CDCl3): δ = 3.31 (s, 3 H), 4.17 (s, 2 H), 7.24 (m, 6 H), 7.61 (dt, 4 H, J = 1.7 Hz). 13C NMR (100.6 MHz, CDCl3): δ = 57.23, 60.20, 83.22 (d, J = 7.6 Hz), 104.36, 128.26 (d, J = 7.6 Hz), 128.72, 132.14 (d, J = 21.3 Hz), 135.59.
