Atomic structure of inclusion complex of 3(o-tolyl)bismuth bis(chloroacetate) with chloroacetic acid

An inclusion complex of tri( o -tolyl) bismuth bis (chloroacetate) with chloroacetic acid ( o -Tol)3Bi[OC(O)CH2Cl]2 HOC(O)CH2Cl (1) was synthesized from tri( o -tolyl)bismuth bis (chloroacetate) and chloroacetic acid in benzene. The structure of adduct 1 was determined by X-ray structural analysis. X-ray analysis of the compound crystal was performed on a D8 Quest Bruker automatic four-circle diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator) at 292 K. 1, P 21/ с , a = 10.8054(2), b = 14.2764(3), c = 12.9748(3) Å, β = 102.677(2)º, V = 1952.73(7) Å3, Z = 4, 0.209 × 0.172 × 0.116 mm, 3.371 30.508º, intervals of reflection indices -15 ≤ h ≤ 15, -20 ≤ k ≤ 20, -18 ≤ l ≤ 18, measured reflections 38696, independent reflections 5964, refinement variables 299, GOOF 1.13, R 1 = 0.0348, wR 2 = 0.076, residual electron density -0.523 / 0.777 e / A3, (calc.) 1.445 g/cm3. In the structure of crystal 1 the Bi atoms have a distorted trigonal bipyramidal coordination with the oxygen atoms in axial positions. The OBiO axial angle in 1 is 175.24 (11). The lengths of the BiO and BiC bonds are 2.258(3)-2.302(3) and 2.211(5), 2.228(5) Å. The chloroacetic acid molecule is linked by a coordination bond through the carboxyl hydrogen atom to the carbonyl oxygen atom of one of the two carboxyl groups of triarylbismuth dicarboxylate. The intermolecular OHO distances (1.9 Å) are shorter than the sum of van der Waals radii O and H by 0.8 Å.