Structure of organic and organoelemental compounds. Part 5

The structure of five organic compounds was determined using X-ray diffraction analysis. X-ray diffraction analysis of compounds was carried out on an automatic four-circle diffractometer D8 Quest Bruker (Mo Kα radiation, λ = 0,71073 Å, graphite monochromator) at 293 K. Crystals (Ph4Sb)2CO3 (1): C49H40O3Sb2, M 920.31; triclinic syngony, symmetry group P-1; cell parameters: a = 10.114(7), b = 13.975(8), c = 15.607(13) Å; a = 73.98(3)°, β = 79.86(5)°, g = 74.39(3)°; V = 2030(2) Å3; Z = 2; rcalc = 1.506 g/cm3; 2q 5.8-52.98 deg.; total reflections 46058; independent reflections 8373; number of refined parameters 488; Rint = 0.0263; GOOF 1.131; R1 = 0.0235, wR2 = 0.0520; residual electron density (max/min) 0.85/-0.55 e/Å3]; p-Tol4SbOC6H3(Cl-2)(F-4) (2): C34H31ClFOSb, M 631.79; triclinic syngony, symmetry group P-1; cell parameters: a = 10.104(10), b = 11.932(14), c = 13.582(18) Å; a = 84.41(6)°, β = 71.39(5)°, g = 74.70(5)°; V = 1497(3) Å3, Z = 2; rcalc = 1.402 g/cm3; 2q 6.14-63.32 deg.; total reflections 93012; independent reflections 9959; number of refined parameters 347; Rint = 0.0322; GOOF 1.049; R1 = 0.0299, wR2 = 0.0713; residual electron density (max/min); 1.20/-0.72 e/Å3], Ph4SbOC(O)CF2CF2C(O)OSbPh4∙PhH (3): C58H46F4O4Sb2, M 1126.47; monoclinic syngony, symmetry group C2; cell parameters: a = 26.096(18), b = 10.011(9), c = 38.74(3) Å; β = 90.63(3)°; V = 10119(14) Å3, Z = 4; rcalc = 1.479 g/cm3; 2q 6.046-54.31 deg.; total reflections 124576; independent reflections 22324; number of refined parameters 1209; Rint = 0.0670; GOOF 1.039; R1 = 0.0465, wR2 = 0.0739; residual electron density (max/min); 0.52/0.53 e/Å3]; [Ph4Sb(DMSO)][PdBr3(DMSO)] (4): C28H32Br3O2PdS2Sb, M 932.52; orthorhombic syngony, symmetry group P212121; cell parameters: a = 9.430(6), b = 15.859(11), c = 22.186(13) Å; a = 90.00 = β = 90.00°, g = 90.00°; V = 3183(4) Å3; Z = 8; rcalc = 1.867 g/cm3; 2q 5.68-43.98 deg.; total reflections 28787; independent reflections 4023; number of refined parameters 339; Rint = 0.0291; GOOF 1.044; R1 = 0.0186, wR2 = 0.0431; residual electron density (max/min); 0.7/-0.59 e/Å3]; [Ph3PAm]2[Bi2I8](MeOCH2CH2OMe) (5): C25H31BiI4OP, M 1095.05; triclinic syngony, symmetry group P-1; cell parameters: a = 11.026(6), b = 12.875(8), c = 13.419(6) Å; a = 62.580(15)°, β = 76.155(14)°, g = 79.07(2)°; V = 1634.8(14) Å3; Z = 2; rcalc = 2.225 g/cm3; 2q 5.98-67.58 deg.; total reflections 93637; independent reflections 13068; number of refined parameters 291; Rint = 0.0454; GOOF 1.064; R1 = 0.0367, wR2 = 0.0693; residual electron density (max/min); 1.03/-2.04 e/Å3].