Synthesis and structure of fluorine-containing binuclear aryl compounds of antimony [(3-FC⁶H⁴)³SbOC(O)(CF²)³CHF²]²O and [(3-FC⁶H⁴)³SbOC(O)CHF²]²O

Abstract

The interaction of tris(3-fluorophenyl)antimony (3-FC6H4)3Sb with fluorinated carboxylic acids [СHF2(СF2)3C(O)OH and СHF2C(O)OH] in the presence of tert-butylhydroperoxide or hydrogen peroxide in ether produced triarylantimony oxo-compounds [(3-FC6H4)3SbOC(O)(СF2)3CHF2]2O (1) and [(3-FC6H4)3SbOC(O)CHF2]2O (2), respectively. The X-ray structural studies were carried out on an Xcalibur 3automatic diffractometer with a CCD detector according to the standard procedure [MoKα radiation, graphite monochromator, ω-scanning with a step of 1° at T=295(2) K]. Crystals 1 [C46H26F22O5Sb2, M 1320.17; triclinic syngony, symmetry group P-1; cell parameters: a = 11.6986(3), b = 14.2914(6), c = 16.1573(7) Å;  = 68.626(4), β = 75.574(3),  = 83.762(3), V = 2435.74(16) Å3; Z = 2; calc = 1.800 g/cm3; 2 4.3861.66 deg.; total reflections 19943; independent reflections 13056; number of refined parameters 676; Rint = 0.0318, GOOF 1.021; R1 = 0.0532, wR2 = 0.1292; residual electron density (max/min): 1.25/0.59 e/Å3] and (2) [C40H26F10O5Sb2 M 1020.13; monoclinic syngony, symmetry group P21/n; cell parameters: a = 10.0751(3), b = 37.9195(14), c = 10.2486(3) Å;  = 90.00, β = 96.543(3),  = 90.00, V = 3889.9(2) Å3, Z = 4; calc = 1.742 g/cm3; 2 3.2261.42 deg.; total reflections 17909; independent reflections 10417; number of refined parameters 568; Rint = 0.0224; GOOF 1.027; R1 = 0.0391, wR2 = 0.0889; residual electron density (max/min): 1.13/0.85 e/Å3]. In crystals 1 and 2, the molecules have a curved structure of the central fragment with the SbOSb angles of 143.38(18) and 141.17(13), respectively