Abstract

The structure of tetra(para-tolyl)antimony compounds p-Tol4SbX [X = Br (1), OC(O)Ph∙PhH (2), OSO2C6Me3-2,4,6 (3)] was established by X-ray diffraction analysis (XRD). According to the X-ray diffraction data, the antimony atoms in complexes 1–3 have a distorted trigonal bipyramidal coordination with three aryl ligands in the equatorial plane, while the axial angles CSbX are 174.75(8), 175.13(9), and 174.51(6). The X-ray diffraction data: (1) [C28H28BrSb, M = 566.16; monoclinic syngony, sp. gr. P21/n; cell parameters: a = 9.868(6) Å, b = 23.312(11) Å, c = 12.106(6) Å; β = 113.15(2), V = 2561(2) Å3, Z = 4; calc = 1.469 g/cm3;  = 2.649 mm–1; F(000) = 1128.0; region 2q collection: 6.4–56.76; –13 ≤ h ≤ 13, –31 ≤ k ≤ 31, –16 ≤ l ≤ 16; total reflections 42998; independent reflections 6359 (Rint = 0.0346); GOOF = 1.080; R-factor 0.0325]; (2) [C41H39O2Sb, M = 685.47; monoclinic syngony, sp. gr. C2/c; cell parameters: a = 28.186(13) Å, b = 15.116(6) Å, c = 17.629(8) Å; β = 91.73(2), V = 7507(6) Å3, Z = 8; calc = 1.213 g/cm3;  = 0.765 mm–1; F(000) = 2816.0; region 2q collection: 6.572–56.996; –37 ≤ h ≤ 37, –20 ≤ k ≤ 20, –23 ≤ l ≤ 23; total reflections 116806; independent reflections 9489 (Rint = 0.0492); GOOF = 1.102; R-factor 0.0363]; (3) [C37H39O3SSb, M = 685.49; monoclinic syngony, sp. gr. P21/n; cell options: a = 12.172(4) Å, b = 18.802(5) Å, c = 15.433(6) Å; β = 108.744(12), V = 3345(2) Å3, Z = 4; calc = 1.361 g/cm3;  = 0.921 mm–1; F(000) = 1408.0; region 2q collection: 5.96–63.02; –16 ≤ h ≤ 17, –27 ≤ k ≤ 27, –22 ≤ l ≤ 21; total reflections 138835; independent reflections 11081 (Rint = 0.0373); GOOF = 1.045; R-factor 0.0304]. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds 1–3 have been deposited at the Cambridge Crystallographic Data Center (CCDC 2182608, 2149953, 2171918; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam. ac.uk).

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