{"title":"Reactions of Pentaphenyl- and Penta(para-tolyl)antimony with Ferrocenedicarboxylic Acid","authors":"V. V. Sharutin","doi":"10.1134/s2634827623600184","DOIUrl":null,"url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Interaction of pentafluorophenyl- and penta(<i>para</i>-tolyl)antimony with ferrocenedicarboxylic acid (molar ratios 1 : 1 and 2 : 1) in toluene (20°C, 24 h) results in the substitution of hydrogen in one or two carboxylate groups, leading to the formation of ferrocenecarboxylates of tetraaryl antimony HOOCС<sub>5</sub>H<sub>4</sub>FeС<sub>5</sub>H<sub>4</sub>C(O)OSbPh<sub>4</sub> (<b>1</b>), HOOCС<sub>5</sub>H<sub>4</sub>FeС<sub>5</sub>H<sub>4</sub>C(O)OSbTol<sub>4</sub> (<b>2</b>), Ph<sub>4</sub>SbC(O)OС<sub>5</sub>H<sub>4</sub>FeС<sub>5</sub>H<sub>4</sub>C(O)OSbPh<sub>4</sub> (<b>3</b>) and <i>p</i>-Tol<sub>4</sub>SbC(O)OС<sub>5</sub>H<sub>4</sub>FeС<sub>5</sub>H<sub>4</sub>C(O)OSbTol<sub>4</sub> (<b>4</b>) with yields up to 83%. Compounds <b>1</b>−<b>4</b> were identified by elemental analysis, IR spectroscopy, and X-ray diffraction analysis for <b>4</b>. The XRD analysis of complex <b>4</b> was conducted on an a D8 Quest Bruker automatic four-circle diffractometer (Мо <i>K</i><sub>α</sub> radiation, λ = 0,71073 Å, graphite monochromator) at 293 K. Crystallographic characteristics of <b>4</b>: monoclinic syngony, space group <i>P</i>2<sub>1</sub>/<i>c</i>, <i>a</i> = 17.227(17) Å, <i>b</i> = 11.064(9) Å, <i>c</i> = 30.59(3) Å, β = 100.00(4)°, <i>V</i> = 5742(9) Å<sup>3</sup>, <i>Z</i> = 4, ρ<sub>calc</sub> = 1.440 g/cm<sup>3</sup>, 2θ 6.02°−49.08°, 124 343 total reflections, 9436 independent reflections, number of refined parameters 684, <i>R</i><sub>int</sub> = 0.1051, <i>GOOF</i> 1.094, <i>R</i><sub>1</sub> = 0.0536, <i>wR</i><sub>2</sub> = 0.1309, residual electron density (max/min) 0.88/–1.21 e/Å<sup>3</sup>. According to XRD analysis, the coordination of antimony atoms in crystal <b>4</b> is distorted octahedral due to the bidentate chelating nature of the carboxylate ligand. Diagonal angles in the two octahedra are 146.4(2)°, 154.0(3)°, 171.0(2)° and 147.4(2)°, 154.8(2)°, 166.9(2)°. The Sb−О distances are 2.296(5), 2.502(5) Å and 2.289(5), 2.453(5) Å, while the Sb−С bonds differ significantly, 2.146(7)−2.166(7) and 2.123(6)−2.165(7) Å. The structural organization of the crystal is mainly governed by С−Н···π interactions.</p>","PeriodicalId":21086,"journal":{"name":"Reviews and Advances in Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2024-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Reviews and Advances in Chemistry","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1134/s2634827623600184","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
Abstract
Interaction of pentafluorophenyl- and penta(para-tolyl)antimony with ferrocenedicarboxylic acid (molar ratios 1 : 1 and 2 : 1) in toluene (20°C, 24 h) results in the substitution of hydrogen in one or two carboxylate groups, leading to the formation of ferrocenecarboxylates of tetraaryl antimony HOOCС5H4FeС5H4C(O)OSbPh4 (1), HOOCС5H4FeС5H4C(O)OSbTol4 (2), Ph4SbC(O)OС5H4FeС5H4C(O)OSbPh4 (3) and p-Tol4SbC(O)OС5H4FeС5H4C(O)OSbTol4 (4) with yields up to 83%. Compounds 1−4 were identified by elemental analysis, IR spectroscopy, and X-ray diffraction analysis for 4. The XRD analysis of complex 4 was conducted on an a D8 Quest Bruker automatic four-circle diffractometer (Мо Kα radiation, λ = 0,71073 Å, graphite monochromator) at 293 K. Crystallographic characteristics of 4: monoclinic syngony, space group P21/c, a = 17.227(17) Å, b = 11.064(9) Å, c = 30.59(3) Å, β = 100.00(4)°, V = 5742(9) Å3, Z = 4, ρcalc = 1.440 g/cm3, 2θ 6.02°−49.08°, 124 343 total reflections, 9436 independent reflections, number of refined parameters 684, Rint = 0.1051, GOOF 1.094, R1 = 0.0536, wR2 = 0.1309, residual electron density (max/min) 0.88/–1.21 e/Å3. According to XRD analysis, the coordination of antimony atoms in crystal 4 is distorted octahedral due to the bidentate chelating nature of the carboxylate ligand. Diagonal angles in the two octahedra are 146.4(2)°, 154.0(3)°, 171.0(2)° and 147.4(2)°, 154.8(2)°, 166.9(2)°. The Sb−О distances are 2.296(5), 2.502(5) Å and 2.289(5), 2.453(5) Å, while the Sb−С bonds differ significantly, 2.146(7)−2.166(7) and 2.123(6)−2.165(7) Å. The structural organization of the crystal is mainly governed by С−Н···π interactions.
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