Synthesis and structure of diphenylbismuth 2-phenylcarboranylcarboxylate

Diphenylbismuth 2-phenylcarboranylcarboxylate (1) has been obtained by the interaction between triphenylbismuth and 2-phenylcarboranylcarboxylic acid in benzene in 91% yield. The compound has been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction analysis the target product 1 is a benzene solvate and has a polymer structure [C48H56O4B20Bi2, М = 1331.09; the triclinic system, space group Р 1 ; a 10.602(7), b 13.211(10), c 20.07(2) Å; α 93.47(4), β 90.02(4), γ 90.01(3) degrees; V 2806(4) Å3; Z 2; ρcalc 1.575 g/cm3; µ 6.304 mm-1; F (000) 1284.0; crystal size 0.55×0.11×0.07 mm; 2θ for data collection 5.26-56.98 degrees; index ranges -13 ≤ h ≤ 13, -16 ≤ k ≤ 16, -25 ≤ l ≤ 25, total reflections 60631; independent reflections 11732; Rint 0.0938; variables 727; GOOF 1.013; R 1 = 0.0338; wR 2 = 0.0628; residual electron density 1.50/-1.05 e/Å3]. The crystal contains two types of crystallographically independent molecules (a and b), the crystallographic parameters of which are slightly different from each other. Bismuth atoms have a bisphenoid coordination with the apically located oxygen atoms of carboxylate substituents. Two phenyl ligands and an electron lone pair are in the equatorial plane. The OBiO axial angles are 159.62(12)° and 159.95(12)°. The CSbC equatorial angles are 103.4(2)° and 103.0(2)° in molecules a and b, respectively. The Bi-C bond lengths are 2.232(6), 2.303(7) Å (a) and 2.240(5), 2.300(7) Å (b); they are comparable with the similar distances for the previously structurally characterized diarylbismuth carboxylates. Through interactions of bismuth atoms with oxygen atoms, molecules of one layer in a crystal form the [···Bi(Ph)2-O-C(R)=O···]n polymer chains along the crystallographic axis a . Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data Bank (No. 1957181; deposit@ccdc.cam.ac.uk; http:// www.ccdc.cam.ac.uk/data_request/cif).