Синтез и строение комплексов висмута [Ph4P]+2[Bi2I8(m2-Et2SO-O)]2– и [Ph4P]+2trans-[Bi2I8(dmso-O)2]2

Abstract

The interaction of bismuth (III) iodide with tetraphenylphosphonium iodide in dimethylsulfoxide and diethylsolfoxide have synthesized bismuth complexes [Ph 4 P] + 2 [Bi 2 I 8 (m 2 -Et 2 SO- O )] 2– ( 1 ) и [Ph 4 P] + 2 trans -[Bi 2 I 8 (dmso- O ) 2 ] 2 - ( 2 ). They have been structurally characterized. The X-ray diffraction pattern has been obtained at 293 K on an automatic diffractometer D8 Quest Bruker (Mo K α -radiation, λ = 0.71073 Å, graphite monochromator) of crystals 1 [C 26 H 24 O 0.5 SI 4 BiP, M 1124.06, the monoclinic syngony, the symmetry group С2/с; cell parameters: а = 27.563(15) Å, b = 9.140(7) Å, с =28.978(17) Å; α = 90.00 degrees, β =119.069(17) degrees, γ = 90.00 degrees; V = 6381(7) Å 3 ; the crystal size 0.43×0.35×0.19 mm; intervals of reflection indexes are –41 ≤ h ≤ 41, –13 ≤ k ≤ 13, –43 ≤ l ≤ 42; total reflections 124163; independent reflections 11658; R int 0.0708; GOOF 1.025; R 1 = 0.0852, wR 2 = 0.1380; residual electron density –3.19/2.61 e/Å 3 ][C 28 H 32 O 2 PS 2 BiI 4 , M 1212.21; the triclinic syngony, the symmetry group Р-1; cell parameters: а = 9.409(10) Å, b = 14.149(16) Å, с =15.745(15) Å; α = 113.85 degrees, β =92.50(4) degrees, γ = 104.05 degrees; V = 1836(3) Å 3 ; the crystal size 0.64×0.43×0.4 mm; intervals of reflection indexes are –15 ≤ h ≤ 15, –23 ≤ k ≤ 24, –25 ≤ l ≤ 26; total reflections 117427; independent reflections 18300; R int 0.0927; GOOF 1.006; R 1 = 0.1366, wR 2 = 0.1369; residual electron density –2.99/2.59 e/Å 3 ] the phosphor atoms have a distorted tetrahedral coordination (the CPC angles are 107.7(3)–112.8(4)° ( 1 ), 107.2(3)–111.2(3)° ( 2 ); the Р–С bond lengths are 1.771(7)–1.823(8) Å ( 1 ), 1.786(6)–1.804(5) Å ( 2 )). The equatorial angles IBiI are 86.22(3)–92.87(3)° ( 1 ), 80.43(8)–95.86(8)° ( 2 ), the axial angles OBiI are 162.71(11)° ( 1 ), и 174.34(11)° ( 2 ); the equatorial Bi–I bond lengths are 2.8882(14)–3.2829(18) Å ( 1 ), 2.928(2)–3.364(3) Å ( 2 ), the axial Bi–I bond lengths are 2.9156(17) Å ( 1 ), 2.928(2) Å ( 2 ), the axial Bi–O bond lengths are 2.747(5)Å ( 1 ), 2.572(5) Å ( 2 ). Complete tables of coordinates of atoms, bond lengths and valence angles for structures 1 and 2 are deposited at the Cambridge Structural Data Bank (no. 1969793, 1969795; deposit@ccdc.cam.ac.uk; https://www.ccdc.cam.ac.uk).