4227-32-1Relevant articles and documents
THE CRYSTAL STRUCTURES OF 10,10'-BIS(PHENOXARSINE) OXIDE AND SELENIDE
Meyers, Edward A.,Applegate, Cynthia A.,Zingaro, Ralph A.
, p. 317 - 328 (2007/10/02)
The reaction between 10,10'-bis(penoxarsine) oxide (I) and HI gives 10-iodophenoxarsine.The latter, on treatment with H2Se give 10,10'-bis(phenoxarsine) selenide (II).The crystal structures of I and II have been determined from single crystal X-ray data.The unit cell for I is monoclinic, P21/c (No. 14) with a = 15.976(3) Angstroem, b = 10.582(2) Angstroem, c = 12.581(2) Angstroem, β = 111.70(1) grad; V = 2018.6 Angstroem3; d(calc.) = 1.65 Mg/m3 at 23 deg C for four molecules per unit cell.From 3279 reflections for which I > 0.5?(I), F > ?(F), R = 0.041 with anisotropic thermal parameters for all non-hydrogen atoms and with fixed positions and thermal parameters for hydrogens.One of the phenoxarsina rings deviates from planarity by approximately 5 grad while the other deviates by more than 24 grad.The (As-O) distances are 1.810(3) and 1.821(3) Angstroem for the flat and bent ring and the (As-O-As) angle is 122.3(1) grad.The bond distances to As and O from C are nearly the same for both rings, but the bond angles with As and the ring O as the apex are systematically larger for the flat ring.For II the unit cell is triclinic, (No. 2) with a = 9.368(1) Angstroem, b = 14.089 Angstroem, c = 9.269(2) Angstroem, α = 111.37(2), β = 113.11(2), γ = 74.76(1); V = 1037.5 Angstroem3, d(calc.) = 1.81 Mg/m3 for two molecules per unit cell at 23 deg C.From 2945 reflections for which I > 0.5?(I), F > ?(F), R = 0.055 with anisotropic thermal parameters for all non-hydrogen atoms and with fixed positions and thermal parameters for hydrogen.One of the phenoxarsina rings deviates by 3 grad from planarity and the other by 8 grad.The (As-Se) bond distances are 2.416(1) and 2.406(1) Angstroem.The (As-Se-As) bond angle is 96.66(4) grad and the corresponding (As-C) and (C-C) distances in the two rings are nearly the same.In comparison with I, the angles with As or O as the central atoms are about the same in both rings of II.