Triphenylantimony and Pentaphenylantimony as Initial Compounds in the Synthesis of Pentavalent Antimony Phenyl Derivatives. Structure of Triphenylantimony, Bis(3,4-Difluorobenzoato)Triphenylantimony and Tetraphenylantimony Carbonate

A. N. Efremov, V. V. Sharutin

Abstract


In this work, the structure of triphenylantimony (1) has been clarified. By the interaction of equimolar amounts of pentaphenylantimony solvate (Ph5Sb∙0.5PhH, 2) with 3,4-difluorobenzoic acid in benzene Bis(3,4-difluorobenzoato)triphenylantimony Ph3Sb[OC(O)C6H3F2-3,4]2 (3) has been obtained for structural characterization. The structure of the triclinic modification of tetraphenylantimony carbonate (4) has also been clarified. According to the data of X-ray diffraction analysis carried out at 293 K on an automatic four-circle D8 Quest Bruker diffractometer (two-coordinate CCD detector, MoKα radiation, λ = 0.71073 Å, graphite monochromator), the crystals are characterized as follows: C36H30Sb2 (1), M 706.10; triclinic system, space group Р1 ̅; cell parameters: a = 10.941(11), b = 11.825(16), c = 13.747(13) Å;  = 102.57(5), β = 104.22(5),
 = 108.35(6); V = 1550(3) Å3; Z = 2; crystal size 0.5×0.44×0.11 mm; index ranges –13 ≤ h ≤ 14, –15 ≤ k ≤ 15, –17 ≤ l ≤ 17; reflections collected 37455; independent reflections 6837; Rint 0.0252; GOOF 1.121; R1 = 0.0257, wR2 = 0.0605; the largest diff. peak/hole 0,23 /–0,84 e/Å3; C32H21O4F4Sb (3), M 667.24; monoclinic system, space group С2/с; cell parameters:
a = 12.652(5), b = 22.466(10), c = 11.561(5) Å; β = 120.027(15); V = 2845(2) Å3; Z = 4; crystal size 0.5×0.45×0.12 mm; index ranges –16 ≤ h ≤ 16, –28 ≤ k ≤ 28, –14 ≤ l ≤ 14; reflections collected 27275; independent reflections 3163; Rint 0.029; GOOF 1.107; R1 = 0.0372, wR2 = 0.1058; the largest diff. peak/hole 1.61/–0.53 e/Å3; C49H40O3Sb2 (4), M 920.31; triclinic system, space group Р1 ̅; cell parameters: a = 10.093(4), b = 13.994(5), c = 15.665(6) Å;  = 73.917(15),
β = 79.76(2),  = 74.312(15); V = 2034.0(13) Å3; Z = 2; crystal size 0.26×0.22×0.05 mm; index ranges –12 ≤ h ≤ 12, –17 ≤ k ≤ 17, –20 ≤ l ≤ 20; reflections collected 50553; independent reflections 9006; Rint 0.0333; GOOF 1.066; R1 = 0.0239, wR2 = 0.0522; the largest diff. peak/hole 0.77/–0.43 e/Å3. The antimony atoms in 3 have a distorted trigonal-bipyramidal coordination with the oxygen atoms in axial positions (the OSbO angle is 174.13(12)°, the Sb–C and Sb–O distances are 2.101(3)–2.118(4) Å and 2.118(3) Å). The structural organization in crystals 3 and 4 is due to weak intermolecular contacts of the О•••Н–C type, 2.49 and 2.56 Å, respectively. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 2117872 for 1, No. 2121388 for 3, No. 2121833 for 4; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).

Keywords


solvate; pentaphenylantimony; benzene; bis(3,4-difluorobenzoato triphenylantimony; synthesis; structure; triphenylantimony; tetraphenylantimony carbonate; X-ray diffraction analysis

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