Structural features of polyfunctional tetraarylantimony carboxylates

From ferrocenedicarboxylic acid, sulfosalicylic acid and pentaarylantimony Ar5Sb (Ar = Ph, p-Tol) in benzene, fully substituted organoantimony derivatives of ferrocenedicarboxylic and sulfosalicylic acids 1-3 were obtained, the structure of which after recrystallization from a benzene-octane mixture was proven by X-ray diffraction analysis. Structures 1-3 were established by X-ray diffraction. Crystals 1 [C68H64FeO4Sb2, M 1244.54; monoclinic syngony, symmetry group C21/c; cell parameters: a = 16.9983(2), b = 10.94570(10), c = 30.3224(3) Å; β = 99.8220(10)°; V = 5559.04(10) Å3; Z = 4; rcalc = 1.487 g/cm3; 2q 5.28-138.76 degrees; total reflections 32707; independent reflections 10281; number of specified parameters 684; Rint = 0.0496; GOOF 1.062; R1 = 0.0345, wR2 = 0.0853; residual electron density (max/min) 0.76/-0.90 e/Å3], 2 [C60H48FeO4Sb2, M 1132.33; monoclinic syngony, symmetry group P21/n; cell parameters: a = 12.40720(10), b = 10.30830(10), c = 36.7290(4) Å; β = 94.1110(10) deg., V = 4685.45(8) Å3, Z = 4; rcalc = 1.605 g/cm3; 2q 4.82-138.56 degrees; total reflections 27748; independent reflections 8680; number of specified parameters 604; Rint = 0.0367; GOOF 1.033; R1 = 0.0277, wR2 = 0.0709; residual electron density (max/min) 0.86/-0.81 e/Å3], 3 [C63H62O7SSb2, M 1206.78; monoclinic syngony, symmetry group P21/c; cell parameters: a = 20.9246(3), b = 13.5375(2), c = 21.4222(3) Å; β = 111.284(2) deg., V = 5654.30(16) Å3, Z = 4; rcalc = 1.4175 g/cm3; 2q 4.54-160 degrees; total reflections 48463; independent reflections 11892; number of specified parameters 699; Rint = 0.0443; GOOF 1.024; R1 = 0.0327, wR2 = 0.0907; residual electron density (max/min) 0.93/-0.85 e/Å3]. The antimony atoms in molecules 1, 2 have a distorted octahedral configuration, taking into account the coordination of the carbonyl oxygen atoms to the metal atom. Structure 3 contains tetrahedral tetraaryl stibonium cations, the antimony atoms in which are coordinated with the oxygen atoms of sulfo groups (Sb∙∙∙O(5)=S 2.601 Å), and the same oxygen atom is coordinated with the ortho-hydrogen atom of one of the tolyl groups (H(46)∙∙∙O(5)=S 2.60 Å). Water molecules provide a structure to crystal 3 (H(7)∙∙∙O(4)=S 1.98 Å, H(7)∙∙∙O(5)=S 2.60 Å). (CCDC 2320709 for 1, 2320711 for 2, 2320717 for 3; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).