Structural features of tris(2-metoxy-5-chlorophenyl)bismuth solvate with benzene

According to X-ray diffraction analysis, the bismuth atoms in two triphenylbismuth molecules (1) [C36H30Bi2, M 880.56; triclinic system, symmetry group P1 ; cell parameters: a = 5.787(3), b = 14.203(7), c = 19.667(14) Å; a = 72.61(3), β = 81.68(4), g = 78.34(2) deg.; V = 1504.5(16) Å3; crystal size 0.46×0.16×0.15 mm; reflection index intervals -7 ≤ h ≤ 7, -18 ≤ k ≤ 18, -25 ≤ l ≤ 25; total reflections 32105; independent reflections 6933; Rint 0,0437; GOOF 1.093; R1 = 0.0290, wR2 = 0.0609; residual electron density 0.48/-1.87 e/Å3] have a distorted trigonal coordination with a lone electron pair at the fourth vertex. The Bi-C bond lengths vary in the range 2.246(5)-2.260(5) Å, the CBiC angles are 92.56(16)-95.24(15)°. In the tris(2-methoxy-5-chlorophenyl)bismuth solvate with benzene (2) [C24H21O3Cl3Bi, M 672.74; monoclinic system, symmetry group P21/n; cell parameters: a = 8.920(5), b = 21.362(7), c = 13.649(5) Å; a = 90.00, β = 107.33(2), g = 90.00 deg.; V = 2482.8(17) Å3; crystal size 0.5×0.11×0.09 mm; reflection index intervals -11 ≤ h ≤ 11, -28 ≤ k ≤ 28, -17 ≤ l ≤ 17; total reflections 40401; independent reflections 5924; Rint 0.0334; GOOF 1.150; R1 = 0.0269, wR2 = 0.0623; residual electron density 0.48/-2.02 e/Å3] a distorted trigonal coordination with a lone electron pair at the fourth vertex is also observed. The Bi-C bond lengths (2.253(3)-2.267(3) Å) are significantly longer than similar bonds in 1 due to the presence of intramolecular Bi∙∙∙O contacts (3.09, 3.08, 3.05 Å). Despite the increase in the volume of bidentate 2-methoxy-5-chlorophenyl ligands, the values of the CBiC angles (90.26(12)-92.96(12)°) are noticeably lower, indicating less steric hindrance in 2. Complete tables of atomic coordinates, bond lengths, and bond angles were deposited in the Cambridge Structural Data Bank (No. 2333440 (1), 2044008 (2); deposit@ccdc.cam.ac.uk; https://www.ccdc.cam.ac.uk).