Reactions of organyltriphenylphosphonium bromides with silver bromide in the presence of hydrobromic acid

Abstract

The interaction of 2-hydroxybenzyltriphenylphosphonium, propargyltriphenylphosphonium, benzyltriphenylphosphonium, and bromopropyltriphenylphosphonium bromides with silver bromide produced ionic complexes [Ph3PCH2C6H2(OH-2)Br2-3,5][Br] (1) [C25H20OPBr3, M = 607.11; monoclinic system, sp. gr. P21/с; cell parameters: a = 18.157(11) Å, b = 15.293(8) Å, c = 17.258(9) Å; β = 90.27(3)°, V = 4792(5) Å3, Z = 4; rcalc = 1.682 g/cm3; m = 5.132 mm–1; F(000) = 2380; collection range at 2q: 5.72-52.26°; total reflections 83462; independent reflections 9454, Rint = 0.0546, GOOF = 1.015; R-factor 0.0351]; [Ph3PCHBr2][Br] ∙ DMSO (2) [C21,33H23O1,17S1,17PBr3, M = 606.17; trigonal system, sp. gr. R ; cell parameters: a = 33.379(18) Å, b = 33.379 Å, c = 11.145(6) Å; a = 90.00°, β = 90.00°, g = 120.00°, V = 10753(13) Å3, Z = 18; rcalc = 1.685 g/cm3; m = 5.244 mm–1; F(000) = 5382; collection range at 2q: 6.26-61.20°; total reflections 59595; independent reflections 7328, Rint = 0.0600, GOOF = 1.047; R-factor 0.0411]; [Ph3PCH2Ph]+2[Ag2Br4]2- (3) [C25H22PBr2Ag, M = 621.07; monoclinic system, sp. gr. С2/с; cell parameters: a = 24.825(14) Å, b = 10.215(7) Å, c = 19.910(11) Å; β = 109.98(2)°, V = 4745(5) Å3, Z = 8; rcalc = 1.739 g/cm3; m = 4.294 mm–1; F(000) = 2432; collection range at 2q: 6.34-67.60°; total reflections 89682; independent reflections 9477, Rint = 0.0677, GOOF = 1.007; R-factor 0.0452]; [Ph3P(CH2)3Br]+3[Ag3Br6]3- (4) [C63H63P3Br9Ag3, M = 1955.75; monoclinic system, sp. gr. P2/с; cell parameters: a = 24.59(3) Å, b = 16.41(2) Å, c = 17.99(2) Å, β = 108.25(4)°, V = 6893(15) Å3, Z = 4, rвыч = 1.885 g/cm3; m = 6.167 mm–1; F(000) = 3768; collection range at 2q: 5.88-39.72°; total reflections 35058; independent reflections 6251, Rint = 0.0555, GOOF = 1.048; R-factor 0.0672].