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Abstract <p>The structures of tetraphenylantimony carboxylates Ph<sub>4</sub>SbOC(O)R (where R is CH<sub>2</sub>Cl (<b>1</b>), CH<sub>2</sub>Br (<b>2</b>), CH<sub>2</sub>I (<b>3</b>), and C<sub>6</sub>H<sub>3</sub>F<sub>2</sub>-2.3) (<b>4</b>)] and nitrate Ph<sub>4</sub>SbONO<sub>2</sub> ∙ H<sub>2</sub>O (<b>5</b>) were established by single-crystal X-ray diffraction. According to X-ray diffraction data, the antimony atoms in complexes <b>1</b>–<b>5</b> have the coordination of a distorted trigonal bipyramid with an electronegative ligand in the axial position. The axial angles of CSbO are 174.05(7)°, 171.6(2)°, 170.3(2)°, 173.10(12)°, 177.93(5)°, 178.02(9)°, 168.11(9)°, 169.33(9)°, respectively. X-ray diffraction data: (<b>1</b>) [C<sub>26</sub>H<sub>22</sub>O<sub>2</sub>ClSb, <i>M</i> = 523.64; rhombic crystal system, space group <i>Pbca</i>; cell parameters: <i>a</i> = 14.382(8) Å, <i>b</i> = 16.681(10) Å, <i>c</i>&#xa0;= 19.270(11) Å; β = 90.00°, <i>V</i> = 4623(5) Å<sup>3</sup>, <i>Z</i> = 8; ρ<sub>calcd</sub> = 1.505 g/cm<sup>3</sup>; μ = 1.328 mm<sup>–1</sup>; <i>F</i>(000) = 2096.0; 2θ range: 5.64°–56.6°; –19 ≤ <i>h</i> ≤ 19, –22 ≤ <i>k</i> ≤ 21, –23 ≤ <i>l</i> ≤ 25; total reflections 69&#xa0;348; independent reflections 5710 (<i>R</i><sub>int</sub> = 0.0398); <i>GOOF</i> = 1.067; <i>R</i>-factor 0.0261]; (<b>2</b>) [C<sub>52</sub>H<sub>46</sub>O<sub>4</sub>Br<sub>2</sub>Sb<sub>2</sub>, <i>M</i> = 1138.19; triclinic crystal system, space group <i>P</i>-1; cell parameters: <i>a</i> = 11.096(13) Å, <i>b</i> = 12.510(13) Å, <i>c</i> = 17.62(2) Å; α = 78.01(6)°, β = 89.35(7)°, γ = 89.71(5)°, <i>V</i> = 2393(5) Å<sup>3</sup>, <i>Z</i> = 2; ρ<sub>calcd</sub> = 1.577 g/cm<sup>3</sup>; μ&#xa0;= 2.841 mm<sup>–1</sup>; <i>F</i>(000) = 1120.0; 2θ range: 5.16°–69.06°; –16 ≤ <i>h</i> ≤ 16, –14 ≤ <i>k</i> ≤ 14, –23 ≤ <i>l</i> ≤ 23; total reflections 89 320; independent reflections 11 788 (<i>R</i><sub>int</sub> = 0.0568); <i>GOOF</i> = 1.034; <i>R</i>-factor 0.0519]; (<b>3</b>)&#xa0;[C<sub>26</sub>H<sub>22</sub>O<sub>2</sub>SbI, <i>M</i> = 615.09; monoclinic crystal system, space group <i>P</i>2<sub>1</sub>/<i>c</i>; cell parameters: <i>a</i> = 12.779(6) Å, <i>b</i> = 10.864(4) Å, <i>c</i> = 17.542(9) Å; β = 100.18(3)°, <i>V</i> = 2397(2) Å<sup>3</sup>, <i>Z</i> = 4; ρ<sub>calc</sub> = 1.704&#xa0;g/cm<sup>3</sup>; μ = 2.458 mm<sup>–1</sup>; <i>F</i>(000) = 1192.0; 2θ range: 6.02°–71.46°; –20 ≤ <i>h</i> ≤ 20, –17 ≤ <i>k</i> ≤ 17, ‒28 ≤ <i>l</i> ≤ 28; total reflections 70&#xa0;960; independent reflections 11&#xa0;043 (<i>R</i><sub>int</sub> = 0.0510); <i>GOOF</i> = 1.018; <i>R</i>-factor 0.0537]; (<b>4</b>) [C<sub>31</sub>H<sub>23</sub>O<sub>2</sub>F<sub>2</sub>Sb, M = 587.24; triclinic crystal system, space group <i>P</i>-1; cell parameters: <i>a</i>&#xa0;= 9.862(13) Å, <i>b</i> = 10.154(13) Å, <i>c</i> = 14.298(2) Å; α = 84.03(6)°, β = 82.76(7)°, γ = 68.41(5)°, <i>V</i> = 1318.2(5) Å<sup>3</sup>, <i>Z</i> = 2; ρ<sub>calcd</sub> = 1.479 g/cm<sup>3</sup>; μ = 1.086 mm<sup>–1</sup>; <i>F</i>(000) = 588.0; 2θ range: 6.08°–74.28°; ‒16 ≤ <i>h</i> ≤ 16, –17 ≤ <i>k</i> ≤ 17, –24 ≤ <i>l</i> ≤ 24; total reflections 88&#xa0;852; independent reflections 13&#xa0;477 (<i>R</i><sub>int</sub>&#xa0;= 0.0353); <i>GOOF</i> = 1.026; <i>R</i>-factor 0.0359]; (<b>5</b>) [C<sub>72</sub>H<sub>62</sub>N<sub>3</sub>O<sub>10</sub>Sb<sub>3</sub>, <i>M</i> = 1494.50; monoclinic crystal system, space group <i>P</i>2<sub>1</sub>/<i>n</i>; cell parameters: <i>a</i> = 23.072(7) Å, <i>b</i> = 10.427(3) Å, <i>c</i> = 27.040(10) Å; β = 95.860(13)°, <i>V</i> = 6472(4) Å<sup>3</sup>, <i>Z</i> = 4; ρ<sub>calcd</sub> = 1.534 g/cm<sup>3</sup>; μ = 1.305 mm<sup>–1</sup>; <i>F</i>(000) = 2992.0; 2θ range: 5.6°–62.16°; –33 ≤ <i>h</i> ≤ 29, –15 ≤ <i>k</i> ≤ 15, –39 ≤ <i>l</i> ≤ 39; total reflections 228&#xa0;547; independent reflections 20 667 (<i>R</i><sub>int</sub> = 0.0432); <i>GOOF</i> = 1.041; <i>R</i>-factor 0.0303]. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds <b>1</b>–<b>5</b> are deposited at the Cambridge Crystallographic Data Center (CCDC nos. 2169943, 2170138, 2213768, 2170205, 2147525; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).</p>

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Structural Features of Tetraphenylantimony Carboxylates Ph4SbOC(O)R (R = CH2Cl, CH2Br, CH2I, C6H3F2-2.3) and Tetraphenylantimony Nitrate Hydrate Ph4SbONO2 ∙ H2O

  • 期刊论文

  • 发表日期：

    2025年6月1日

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  • V. V. Sharutin,
  • O. K. Sharutina

摘要

Abstract

The structures of tetraphenylantimony carboxylates Ph4SbOC(O)R (where R is CH2Cl (1), CH2Br (2), CH2I (3), and C6H3F2-2.3) (4)] and nitrate Ph4SbONO2 ∙ H2O (5) were established by single-crystal X-ray diffraction. According to X-ray diffraction 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 axial angles of CSbO are 174.05(7)°, 171.6(2)°, 170.3(2)°, 173.10(12)°, 177.93(5)°, 178.02(9)°, 168.11(9)°, 169.33(9)°, respectively. X-ray diffraction data: (1) [C26H22O2ClSb, M = 523.64; rhombic crystal system, space group 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; ρcalcd = 1.505 g/cm3; μ = 1.328 mm–1; F(000) = 2096.0; 2θ range: 5.64°–56.6°; –19 ≤ h ≤ 19, –22 ≤ k ≤ 21, –23 ≤ l ≤ 25; total reflections 69 348; independent reflections 5710 (Rint = 0.0398); GOOF = 1.067; R-factor 0.0261]; (2) [C52H46O4Br2Sb2, M = 1138.19; triclinic crystal system, space group P-1; cell parameters: a = 11.096(13) Å, b = 12.510(13) Å, c = 17.62(2) Å; α = 78.01(6)°, β = 89.35(7)°, γ = 89.71(5)°, V = 2393(5) Å3, Z = 2; ρcalcd = 1.577 g/cm3; μ = 2.841 mm–1; F(000) = 1120.0; 2θ range: 5.16°–69.06°; –16 ≤ h ≤ 16, –14 ≤ k ≤ 14, –23 ≤ l ≤ 23; total reflections 89 320; independent reflections 11 788 (Rint = 0.0568); GOOF = 1.034; R-factor 0.0519]; (3) [C26H22O2SbI, M = 615.09; monoclinic crystal system, space group 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; ρcalc = 1.704 g/cm3; μ = 2.458 mm–1; F(000) = 1192.0; 2θ range: 6.02°–71.46°; –20 ≤ h ≤ 20, –17 ≤ k ≤ 17, ‒28 ≤ l ≤ 28; total reflections 70 960; independent reflections 11 043 (Rint = 0.0510); GOOF = 1.018; R-factor 0.0537]; (4) [C31H23O2F2Sb, M = 587.24; triclinic crystal system, space group P-1; cell parameters: a = 9.862(13) Å, b = 10.154(13) Å, c = 14.298(2) Å; α = 84.03(6)°, β = 82.76(7)°, γ = 68.41(5)°, V = 1318.2(5) Å3, Z = 2; ρcalcd = 1.479 g/cm3; μ = 1.086 mm–1; F(000) = 588.0; 2θ range: 6.08°–74.28°; ‒16 ≤ h ≤ 16, –17 ≤ k ≤ 17, –24 ≤ l ≤ 24; total reflections 88 852; independent reflections 13 477 (Rint = 0.0353); GOOF = 1.026; R-factor 0.0359]; (5) [C72H62N3O10Sb3, M = 1494.50; monoclinic crystal system, space group 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; ρcalcd = 1.534 g/cm3; μ = 1.305 mm–1; F(000) = 2992.0; 2θ range: 5.6°–62.16°; –33 ≤ h ≤ 29, –15 ≤ k ≤ 15, –39 ≤ l ≤ 39; total reflections 228 547; independent reflections 20 667 (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 nos. 2169943, 2170138, 2213768, 2170205, 2147525; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).