Structure of bromopropyltriphenylphosphonium and 2-hydroxy,5-bromobenzyltriphenylphosphonium bromides

Abstract

The ionic phosphorus complexes [Ph3P(CH2)3Br]Br (1) and [Ph3PCH2C6H3(OH-2)(Br-5)]Br (2) in whose the phosphorus atoms have distorted tetragonal coordination are structurally characterized. According to the X-ray diffraction data 1 C21H21Br2P, M 464,17; monoclinic syngony, symmetry group P21/c; cell parameters: a = 11,1690(4), b = 10,1561(2), c = 17,5963(6) Å;  = 90,00, β = 104,957(3),  = 90,00; V = 1928,38(13) Å3, Z = 4, calc = 1,599 g/cm3,  = 4,286 mm−1, F(000) = 928,0, 2θ data acquisition range, deg: 4,68−57, crystal size 0,51×0,23×0,14 mm; reflection index ranges –14 ≤ h ≤ 9, –7 ≤ k ≤ 13, –14 ≤ l ≤ 23; total reflections 7693; independent reflections 4783; Rint = 0,0154; GOOF 1,011; R1 = 0,0441, wR2 = 0,1006; residual electron density 1,75/–1,14 e/Å3; 2 C25H21Br2OP, M 528,21; monoclinic syngony, symmetry group P21/n; cell parameters: a = 9,1189(3), b = 10,0544(3), c = 24,2296(7) Å;  = 90,00, β = 95,732(3),  = 90,00; V = 2210,39(12) Å3, Z = 4, calc = 1,587 g/cm3,  = 3,754 mm−1, F(000) = 1056,0, 2θ data acquisition range, deg: 4,64−57, crystal size 0,35×0,26×0,18 mm; reflection index ranges –11 ≤ h ≤ 5, –13 ≤ k ≤ 6, –32 ≤ l ≤ 32; total reflections 8157; independent reflections 5416; Rint = 0,0214; GOOF 1,061; R1 = 0,0810, wR2 = 0,2433; residual electron density 1,57/–2,28 e/Å3]. In organyltriphenylphosphonium cations 1 and 2, the phosphorus atoms have tetragonal coordination, the CPC angles in which varied in the ranges of 106,95(14)111,08(15) and 107,3(3)112,6(3), respectively, the PC distances were 1,791(3)1,797(3) Å and 1,791(6)1,844(6) Å, which is slightly lower than the sum of the covalent radii of the partner atoms (1,83 Å). Complete tables of atomic coordinates, bond lengths and bond angles for the structures have been deposited with the Cambridge Crystallographic Data Centre (No. 2522435 (1), No. 2522473 (2); deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).