Abstract― The reaction of ferrocenedicarboxylic acid, sulfosalicylic acid, and pentaarylantimony Ar5Sb (Ar = Ph, p-Tol) in benzene was found to afford fully substituted organoantimony derivatives of ferrocenedicarboxylic and sulfosalicylic acids 1, 2, and 3. The structures of the compounds after recrystallization from a benzene-octane mixture were determined by X-ray crystallography. Crystals of 1 [C68H64FeO4Sb2, FW 1244.54; monoclinic system, symmetry group C21/c; cell parameters: a = 16.9983(2) Å, b = 10.94570(10) Å, c = 30.3224(3) Å; β = 99.8220(10)°; V = 5559.04(10) Å3; Z = 4; ρcalcd = 1.487 g/cm3; 2θ range 5.28−138.76 deg; total reflections 32 707; independent reflections 10 281; 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, FW 1132.33; monoclinic system, symmetry group P21/n; cell parameters: a = 12.40720(10) Å, b = 10.30830(10) Å, c = 36.7290(4) Å; β = 94.1110(10)°, V = 4685.45(8) Å3, Z = 4; ρcalcd = 1.605 g/cm3; 2θ range 4.82−138.56 deg; total reflections 27 748; 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, FW 1206.78; monoclinic system, symmetry group P21/c; cell parameters: a = 20.9246(3) Å, b = 13.5375(2) Å, c = 21.4222(3) Å; β = 111.284(2)°, V = 5654.30(16) Å3, Z = 4; ρcalcd = 1.4175 g/cm3; 2θ range 4.54−160 deg; total reflections 48 463; independent reflections 11 892; 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 and 2 have a distorted octahedral configuration, taking into account the coordination of carbonyl oxygen atoms to the metal atom. Structure of 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 were found to structure crystal 3 (H(7)∙∙∙O(4)=S 1.98 Å, H(7)∙∙∙O(5)=S 2.60 Å). (CCDC nos. 2320709 for 1, 2320711 for 2, 2320717 for 3; deposit@ccdc.cam.ac.uk; <a href="http://www.ccdc.cam.ac.uk">http:www.ccdc.cam.ac.uk</a>).

Structual Features of Polyfunctional Tetraarylantimony Carboxylates

期刊论文
发表日期：

2025年3月1日

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V. V. Sharutin

摘要

Abstract―

The reaction of ferrocenedicarboxylic acid, sulfosalicylic acid, and pentaarylantimony Ar₅Sb (Ar = Ph, p-Tol) in benzene was found to afford fully substituted organoantimony derivatives of ferrocenedicarboxylic and sulfosalicylic acids 1, 2, and 3. The structures of the compounds after recrystallization from a benzene-octane mixture were determined by X-ray crystallography. Crystals of 1 [C₆₈H₆₄FeO₄Sb₂, FW 1244.54; monoclinic system, symmetry group C2₁/c; cell parameters: a = 16.9983(2) Å, b = 10.94570(10) Å, c = 30.3224(3) Å; β = 99.8220(10)°; V = 5559.04(10) Å³; Z = 4; ρ_calcd = 1.487 g/cm³; 2θ range 5.28−138.76 deg; total reflections 32 707; independent reflections 10 281; number of specified parameters 684; R_int = 0.0496; GOOF 1.062; R₁ = 0.0345, wR₂ = 0.0853; residual electron density (max/min) 0.76/−0.90 e/Å³], 2 [C₆₀H₄₈FeO₄Sb₂, FW 1132.33; monoclinic system, symmetry group P2₁/n; cell parameters: a = 12.40720(10) Å, b = 10.30830(10) Å, c = 36.7290(4) Å; β = 94.1110(10)°, V = 4685.45(8) Å³, Z = 4; ρ_calcd = 1.605 g/cm³; 2θ range 4.82−138.56 deg; total reflections 27 748; independent reflections 8680; number of specified parameters 604; R_int = 0.0367; GOOF 1.033; R₁ = 0.0277, wR₂ = 0.0709; residual electron density (max/min) 0.86/−0.81 e/Å³], 3 [C₆₃H₆₂O₇SSb₂, FW 1206.78; monoclinic system, symmetry group P2₁/c; cell parameters: a = 20.9246(3) Å, b = 13.5375(2) Å, c = 21.4222(3) Å; β = 111.284(2)°, V = 5654.30(16) Å³, Z = 4; ρ_calcd = 1.4175 g/cm³; 2θ range 4.54−160 deg; total reflections 48 463; independent reflections 11 892; number of specified parameters 699; R_int = 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 and 2 have a distorted octahedral configuration, taking into account the coordination of carbonyl oxygen atoms to the metal atom. Structure of 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 were found to structure crystal 3 (H(7)∙∙∙O(4)=S 1.98 Å, H(7)∙∙∙O(5)=S 2.60 Å). (CCDC nos. 2320709 for 1, 2320711 for 2, 2320717 for 3; deposit@ccdc.cam.ac.uk; http:www.ccdc.cam.ac.uk).