Structural features of tetraphenylantimony carboxylates Ph4SbOC(O)R (R = CH2Cl, CH2Br, CH2l, C6H3F2-2,3) and tetraphenylantimony nitrate hydrate Ph4SbONO2 ∙ H2O

The structure of tetraphenylantimony carboxylates Ph4SbOC(O)R [R = CH2Cl (1), CH2Br (2), CH2l (3), C6H3F2-2,3) (4)] and nitrate Ph4SbONO2 ∙ H2O (5) was established by X-ray diffraction analysis (XRD). According to the XRD data, the antimony atoms in complexes 1-5 have the coordination of a distorted trigonal bipyramid with an electronegative ligand in the axial position. The CSbO axial angles are 174.05(7); 171.6(2), 170.3(2); 173.10(12); 177.93(5); 178.02(9), 168.11(9), and 169.33(9)° respectively. The X-ray diffraction data: (1) [C26H22O2ClSb, M = 523.64; rhombic system, sp. gr. Pbca; cell parameters: a = 14.382(8) Å, b = 16.681(10) Å, c = 19.270(11) Å; β = 90.00°, V = 4623(5) Å3, Z = 8; rcalc = 1.505 g/cm3; m = 1.328 mm-1; F(000) = 2096.0; region 2q collection: 5.64-56.6°; -19 ≤ h ≤ 19, -22 ≤ k ≤ 21, -23 ≤ l ≤ 25; total reflections 69348; independent reflections 5710 (Rint = 0.0398); GOOF = 1.067; R-factor 0.0261]; (2) [C52H46O4Br2Sb2, M = 1138.19; triclinic syngony, sp. gr. P-1; cell parameters: a = 11.096(13) Å, b = 12.510(13) Å, c = 17.62(2) Å; a = 78.01(6)°, β = 89.35(7)°, g = 89.71(5)°, V = 2393(5) Å3, Z = 2; rcalc = 1.577 g/cm3; m = 2.841 mm-1; F(000) = 1120.0; region 2q collection: 5.16-69.06°; -16 ≤ h ≤ 16, -14 ≤ k ≤ 14, -23 ≤ l ≤ 23; total reflections 89320; independent reflections 11788 (Rint = 0.0568); GOOF = 1.034; R-factor 0.0519]; (3) [C26H22O2SbI, M = 615.09; monoclinic syngony, sp. gr. P21/c; cell parameters: a = 12.779(6) Å, b = 10.864(4) Å, c = 17.542(9) Å; β = 100.18(3)°, V = 2397(2) Å3, Z = 4; rcalc = 1.704 g/cm3; m = 2.458 mm-1; F(000) = 1192.0; region 2q collection: 6.02-71.46°; -20 ≤ h ≤ 20, -17 ≤ k ≤ 17, -28 ≤ l ≤ 28; total reflections 70960; independent reflections 11043 (Rint = 0.0510); GOOF = 1.018; R-factor 0,0537]; (4) [C31H23O2F2Sb, M = 587.24; triclinic syngony, sp. gr. P-1; cell parameters: a = 9.862(13) Å, b = 10.154(13) Å, c = 14.298(2) Å; a = 84.03(6)°, β = 82.76(7)°, g = 68.41(5)°, V = 1318.2(5) Å3, Z = 2; rcalc = 1.479 g/cm3; m = 1.086 mm-1; F(000) = 588.0; region 2q collection: 6.08-74.28°; -16 ≤ h ≤ 16, -17 ≤ k ≤ 17, -24 ≤ l ≤ 24; total reflections 88852; independent reflections 13477 (Rint = 0.0353); GOOF = 1.026; R-factor 0.0359]; (5) [C72H62N3O10Sb3, M = 1494.50; monoclinic syngony, sp. gr. P21/n; cell parameters: a = 23.072(7) Å, b = 10.427(3) Å, c = 27.040(10) Å; β = 95.860(13)°, V = 6472(4) Å3, Z = 4; rcalc = 1.534 g/cm3; m = 1.305 mm-1; F(000) = 2992.0; region 2q collection: 5.6-62.16°; -33 ≤ h ≤ 29, -15 ≤ k ≤ 15, -39 ≤ l ≤ 39; total reflections 228547; independent reflections 20667 (Rint = 0.0432); GOOF = 1.041; R-factor 0.0303]. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds 1-5 are deposited at the Cambridge Crystallographic Data Center (CCDC 2169943, 2170138, 2213768, 2170205, 2147525; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).