Structure of organic and organoelemental compounds. Part 4

Abstract

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 (1) [Ph3PCH2C(O)Ph]+[Br], C26H22OPBr, M 461,32; rhombic system, symmetry group Pbca; cell parameters: a = 10,88(2), b = 18,55(4), c = 21,81(4) Å;  = 90,00, β = 90,00,  = 90,00;
V = 4399(15) Å3; Z = 8; cal = 1,393 g/cm3; 2 5,7256,7 deg.; total reflections 64127; independent reflections 5447; number of specified parameters 262; Rint = 0,0813; GOOF 1,129; R1 = 0,0526,
wR2 = 0,1459; residual electron density (max/min); 0,97/1,11 e/Å3], (2) HON=CHC6H4(NO2-3), C7H6N2O3, M 166,14; monoclinic system, symmetry group P21/n; cell parameters: a = 3,764(3),
b = 7,002(7), c = 28,56(2) Å; β = 91,34(4) deg., V = 752,6(11) Å3, Z = 4; calc = 1,466 g/сm3; 2 656,78 deg.; total reflections 24593; independent reflections 1880; number of specified parameters 110; Rint = 0,0317; GOOF 1,067; R1 = 0,0527, wR2 = 0,1299; residual electron density (max/min); 0,15/0,25 e/Å3], (3) [Ph3PCH2C6H4(OH-2)]+[Br] ∙ H2O, C25H24BrO2P, M 467,31; triclinic system, symmetry group P–1; cell parameters: a = 9,699(9), b = 13,455(11), c = 18,340(16) Å;  = 87,01(3), β = 77,01(4),
 = 74,42(4); V = 2246(3) Å3, Z = 2; calc = 1,382 г/см3; 2 5,6656,74 deg.; total reflections 74580; independent reflections 11176; number of specified parameters 533; Rint = 0,0360; GOOF 1,015;
R1 = 0,0334, wR2 = 0,0789; residual electron density (max/min); 0,32/0,70 e/Å3], (4) [Ph3P(CH2)4Br]+[Br], C22H23PBr2, M 478,19; monoclinic system, symmetry group P21/c; cell parameters: a = 12,219(11), b = 10,455(9), c = 17,254(15) Å;  = 90,00, β = 104,58(4),  = 90,00;
V = 2133(3) Å3; Z = 4; выч = 1,489 g/сm3; 2 6,2457,32 deg.; total reflections 51137; independent reflections 5420; number of specified parameters 226; Rint = 0,0413; GOOF 1,073; R1 = 0,0324,
wR2 = 0,0718; residual electron density (max/min); 0,26/0,86 e/Å3], (5) [Ph3P(CH2)2OH]+[Br], C20H20PBrO, M 387,24; monoclinic system, symmetry group C2/c; cell parameters: a = 14,319(6),
b = 12,724(6), c = 19,976(11) Å;  = 90,00, β = 92,52(2),  = 90,00; V = 3636(3) Å3; Z = 8;
calc = 1,15 г/см3; 2 5,8464,16 deg.; total reflections 67306; independent reflections 6355; number of specified parameters 209; Rint = 0,0390; GOOF 1,039; R1 = 0,0614, wR2 = 0,1774; residual electron density (max/min); 3,43/0,86 e/Å3].