Synthesis and Structure of Tetraphenylantimony N,N-Diethyldithiocarbamate

Tetraphenylantimony chloride was reacted with sodium N,N-diethyldithiocarbamate in water to obtain tetraphenylantimony N,N-diethyldithiocarbamate in 98% yield. According to X-ray diffraction data, the configuration of the molecule of tetraphenylantimony diethyldithiocarbamate is distorted octahedron, and the Sb-S bond lengths are 2.705(2) and 2.771(2) Å.     

Tetraphenylantimony Carbonate. Synthesis and Structure

Pentaphenylantimony Ph₅Sb was reacted with triphenylantimony carbonate in toluene to obtain tetraphenylantimony carbonate. The structure of monoclinic crystals of tetraphenylantimony carbonate was studied.     

Synthesis and Structure of (4-Acetyl-3-hydroxyphenoxy)tetraphenylantimony

Pentaphenylantimony was reacted with 4-acetyl-1,3-dihydroxybenzene in toluene at elevated temperature to obtain (4-acetyl-3-hydroxyphenoxy)tetraphenylantimony in 93% yield. According to X-ray diffraction data, the antimony atom in (4-acetyl-3-hydroxy-phenoxy)tetraphenylantimony has a distorted trigonal-bipyramidal configuration. The Sb-O and Sb-C distances are 2.237(1) and 2.112(1), 2.114(2), 2.118(2), 2.170(2) Å, respectively, and the CSbO angle is 177.86(5)°.     

Tetraphenylantimony(V) hexachloroplatinate, tetrachloroaurate, and hexachlorostannate [Ph4Sb] 2+ [PtCl6]2?, [Ph4Sb]+[AuCl4]?, and [Ph4Sb] 2+ [SnCl6]2?: Synthesis and crystal structures

The reactions of tetraphenylantimony with hexachloroplatinic and chloroauric acids in benzene afford bis(tetraphenylantimony) hexachloroplatinate (I) and tetraphenylantimony tetrachloroaurate (II), respectively. Compound II is also synthesized from tetraphenylantimony chloride and chloroauric acid in acetone. Bis(tetraphenylantimony) hexachlorostannate (III) is synthesized from tin dichloride and tetraphenylantimony chloride in acetone or from tin tetrachloride and tetraphenylantimony chloride in benzene. The crystal structures of compounds I–III are determined by X-ray diffraction analysis. The antimony atoms in the [Ph₄Sb]⁺ cations have a distorted tetrahedral coordination (CSbC bond angles range from 105.7(1)° to 118.5(1)° (I), from 106.2(3)° to 114.4(3)° (II), and from 106.0(1)° to 117.1(1)° (III)). The Sb-C bond lengths vary in intervals of 2.094(2)–2.098(2), 2.087(7)–2.111(7), and 2.093–2.100(3) ?, respectively. The coordination of the Pt and Sn atoms in complexes I and III is close to an ideal octahedral coordination with ClPtCl and ClSnCl bond angles of 88.68(2)°–91.32(3)° and 88.84(3)°–91.16(3)°, respectively. The square coordination of the Au atom in complex II is slightly distorted: the Au-Cl bond lengths are 2.266(2)–2.277(2) ?, the ClAuCl bond angles are equal to 89.7(1)°–90.5(1)°, the root-mean-square deviation of the atoms from the coordination plane being 0.004 ?. Original Russian Text ? V.V. Sharutin, V.S. Senchurin, O.A. Fastovets, A.P. Pakusina, O.K. Sharutina, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 5, pp. 373–379.     

Synthesis and Structure of Tetraphenylantimony Nitrate

The reaction of pentaphenylantimony with triphenylantimony dinitrate in toluene gives tetraphenylantimony nitrate in 99% yield. The X-ray diffraction data show that the antimony atom in the molecule of tetraphenylantimony nitrate has a distorted trigonal-bipyramidal coordination with axial location of the oxygen atom of the nitrate group. The Sb-O, Sb_{a x}, and Sb-C_{e q} bond lengths in two independent molecules of tetraphenylantimony nitrate are 2.498(3), 2.548(2); 2.134(3), 2.138(3); and 2.101(3)-2.112 Å.     

Synthesis and structure of tetraphenylantimony cyanamide

The reactions of tetraphenylantimony chloride and bromide with carbamide were used to obtain tetraphenylantimony cyanamide in yields of 52 and 48%, respectively. According to X-ray diffraction data, the antimony atom has a distorted trigonal bipyramidal coordination with axial cyanamide and aryl groups [axial CSbN angle 177.76(7)°, Sb-C 2.107(2)-2.167.2, Sb-N 2.3383(18) Å].     

Synthesis and Structure of Bis(tetraphenylantimony) Tetrafluorophthalate

Oxidation of pentaphenylantimony with atmospheric oxygen in toluene on heating gives -oxo-bis(tetraphenylantimony) (yield 63%). Its reaction with tetrafluorophthalic anhydride gives bis(tetraphenylantimony) tetrafluorophthalate (yield 94%). According to single-crystal X-ray diffraction data, the antimony atoms in the molecule of bis(tetraphenylantimony) tetrafluorophthalate have a distorted trigonal bipyramidal coordination with the following geometries: Sb-O bond lengths 2.357(3) and 2.283(3) Å, Sb-C bond lengths 2.108(4)-2.141(4) and 2.100(5)-2.158(4) Å, and CSbO angles 177.42(14)° and 176.18(14)°.     

Synthesis and structure of [(μ4-succinato)hexadecaphenyltetraantimony] triiodide solvate with benzene [(Ph4Sb)2O2CCH2CH2CO2(Ph4Sb)2][I3]2 · 4PhH

Russian Journal of Coordination Chemistry - The reaction of bis(tetraphenylantimony) succinate with iodine in benzene affords [(μ4-succinato) hexadecaphenyltetraantimony] triiodide solvate...     

Thermodynamic Properties of Ph4Sb(OC(O)C≡CPh)

Russian Journal of Physical Chemistry A - The temperature dependence of the specific heat capacity of tetraphenylantimony phenylpropiolate Ph4Sb(OC(O)C≡CPh) in the range of 6–450 K is...     

μ-Oxo-Bis(Tetraphenylantimony): Synthesis,Structure, and Reactions

Heating of a solution of pentaphenylantimony in toluene in atmospheric oxygen affords -oxo-bis(tetraphenylantimony) (I) in a 63% yield. The latter compound can be converted to bis(tetraphenylantimony) carbonate or phthalate by the action of carbon dioxide or phthalic anhydride, respectively. According to X-ray diffraction data, the antimony atoms in compound Ihave a distorted trigonal-bipyramidal coordination (Sb–O 2.0050(4) Å, the SbOSb angle 151.71(9)°). The molecule of bis(tetraphenylantimony) phthalate is composed of two equal fragments, and its Sb atoms also have trigonal-bipyramidal coordination (Sb–O 2.2421(8) Å; Sb–C 2.176(1), 2.115(1), 2.130(1), and 2.137(1) Å).     

Tetraphenylantimony Phenylglyoxylate: Synthesis and Structure

Pentaphenylantimony reacts with phenylglyoxylic acid in toluene to give tetraphenylantimony phenylglyoxylate in 88% yield. X-ray data show that the antimony atom in tetraphenylantimony phenylglyoxylate has the trigonal bipyramidal coordination with the oxygen atom in the axial position. The SbÄC distances are 2.114(4), 2.119(4), 2.142(4), and 2.173(4) Å; SbÄO distance, 2.299(3) Å; and C _a SbO angle, 178.7(1)°.     

Phenylation of Antimony(V) Organic Compounds with Pentaphenylantimony. The Structure of Tetraphenylantimony Chloride

Tetraphenylantimony chloride and bromide were synthesized through the reaction of pentaphenylantimony with diphenylantimony trichloride or tribromide taken at a molar ratio of 2 : 1 in toluene. When the initial compounds were taken at a molar ratio of 1 : 1, triphenylantimony dichloride or dibromide was formed. The phenylation of triphenylantimony sulfate with pentaphenylantimony yielded tetraphenylantimony sulfate. According to the X-ray diffraction data, the antimony atom in the tetraphenylantimony chloride molecule has a distorted trigonal bipyramidal configuration with the chlorine atom in the axial position. The Sb–Cl distance is equal to 2.686(1) and Sb–C distances are equal to 2.113(4) and 2.165(4) Å (av. 2.130 Å).     

Voltammetric study of the transfer of fluoride ion at the nitrobenzene / water interface assisted by tetraphenylantimony.

The transfer of F- ion assisted by an organometallic complex cation tetraphenylantimony (TPhSb+) across the polarized nitrobenzene / water (NB / W) interface has been studied by means of ion-transfer voltammetry. A well-defined voltammetric wave was observed within the potential window at the NB / W interface when tetraphenylantimony tetrakis(4-chlorophenyl) borate and F- ion were present in NB and W, respectively. The voltammogram can be interpreted as being due to the reversible transfer of F- ion assisted by the formation of the TPhSbF complex through the coordination of F- to Sb atom in NB. The formal formation constant of TPhSbF in NB has been determined to be 10(1.95 +/- 0.2 M(-1). No voltammetric wave due to the TPhSb(+)-assisted transfer of other anions such as Cl-, Br, I-, NO3-, CH3COO- and H2PO4(-) ions has been observed within the potential window.     

Synthesis and Structure of Tetra- and Triarylantimony Oximates

Reactions of pentaphenyl- and penta-p-tolylantimony with benzophenone oxime or triarylantimony bis(benzophenone oximate) yield tetraarylantimony benzophenone oximates. Triarylantimony bis(benzophenone oximates) were prepared by oxidative addition from triarylstibine and benzophenone oxime in the presence of hydrogen peroxide. X-ray diffraction analysis was performed to show that benzophenone oxime is a dimer and tetraphenylantimony benzophenone oximate has a trigonal bipyramidal antimony atom and an axial oxime oxygen atom.     

Thermodynamic properties of tetraphenylantimony 1-adamantanecarboxylate

Journal of Thermal Analysis and Calorimetry - In the present work for the first time, the temperature dependence of the heat capacity $$C_{\text{p}}^{\text{o}}$$ = f(T) of tetraphenylantimony...     

Tetraphenylantimony perrhenate and tetraphenylantimony chlorate: Syntheses and structures

The reaction of tetraphenylantimony chloride with sodium perrhenate or potassium chlorate yields tetraphenylantimony perrhenate (I) and tetraphenylantimony chlorate (II), respectively. Complex I was also synthesized from pentaphenylantimony and triphenylantimony diperrhenate in toluene. According to X-ray diffraction, crystals I and II consist of almost regular tetrahedral tetraphenylstibonium cations (CSbC, 109.4(2)°–109.5(7)° in I and 109.1(1)°–109.6(1)° in II) and [ReO₄]^? (OreO, 107.6(3)°–113.3(5)°) and [ClO₃]^? (OClO, 96.3(9)°, 116.4(5)°) anions, respectively. The average Sb-C bond lengths (2.094(3) Å in I, 2.097(2) Å in II) are close to the sum of the covalent radii of the Sb and C atoms. The average distances Re-O in complex I (1.672(4) Å) and Cl-O in complex II (1.315 Å) correspond to multiple bonds.     

The structure of tetraarylantimony halides and tetraphenylantimony isothiocyanate

X-ray diffraction analysis is used to study tetraphenylantimony fluoride (I), tetra-p-tolylantimony (II), and tetraphenylantimony isothiocyanate (III), where Sb atom has a distorted trigonal-bipyramidal coordination. The Sb-C bond lengths in I–III lie a range of 2.102(1)–2.183(1) Å; the Sb-F, Sb-Cl, and Sb-N distances are equal to 2.0530(8) Å, 2.7319(7) Å, and 2.507(2)Å, respectively, in I, II, and III.Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 2, 2005, pp. 117–124.Original Russian Text Copyright © 2005 by Sharutin, Sharutina, Pakusina, Smirnova, Pushilin.     

Synthesis and Structure of Tetra- and Triarylantimony Oximates

Pentaphenyl- and penta-p-tolylantimony were reacted with benzophenone oxime or triarylantimony bis(benzophenonoximate) in toluene to obtain tetraarylantimony benzophenonoximate. Triarylantimony bis(benzophenonoximates) were prepared by oxidative addition from tryarylstibine and oxime in ether in the presence of hydrogen peroxide. X-ray diffraction analysis of tetraphenylantimony benzophenonoximate was performed to show that coordination of the antimony atom is trigonal-bipyramidal and the oxime oxygen atom is axial.     

Spectroscopic Evidence for Ternary Surface Complexes in the Lead(II)-Malonic Acid-Hematite System

Using extended X-ray absorption fine structure (EXAFS) and attenuated total reflectance Fourier-transform infrared (ATR-FTIR) measurements, we examined the sorption of Pb(II) to hematite in the presence of malonic acid. Pb L(III)-edge EXAFS measurements performed in the presence of malonate indicate the presence of both Fe and C neighbors, suggesting that a major fraction of surface-bound malonate is bonded to adsorbed Pb(II). In the absence of Pb(II), ATR-FTIR measurements of sorbed malonate suggest the formation of more than one malonate surface complex. The dissimilarity of the IR spectrum of malonate sorbed on hematite to those for aqueous malonate suggest at least one of the sorbed malonate species is directly coordinated to surface Fe atoms in an inner-sphere mode. In the presence of Pb, little change is seen in the IR spectrum for sorbed malonate, indicating that geometry of malonate as it coordinates to sorbed Pb(II) adions is similar to the geometry of malonate as it coordinates to Fe in the hematite surface. Fits of the raw EXAFS spectra collected from pH 4 to pH 8 result in average Pb-C distances of 2.98 to 3.14 ?, suggesting the presence of both four- and six-membered Pb-malonate rings. The IR results are consistent with this interpretation. Thus, our results suggest that malonate binds to sorbed Pb(II) adions, forming ternary metal-bridging surface complexes. Copyright 2001 Academic Press.     

Tetraphenylantimony Diphenacylphosphinate: Synthesis and Structure

Tetraphenylantimony diphenacylphosphinate was synthesized by reacting pentaphenylantimony with diphenacylphosphinic acid or triphenylantimony bis(diphenacylphosphinate) in toluene (with a yield up to 88%). According to X-ray diffraction data, the antimony atom in tetraphenylantimony diphenacylphosphinate molecule has a trigonal bipyramidal coordination to the axial oxygen atom. The four Sb-C and one Sb-O distances and C_axSbO angle are equal to 2.102(2), 2.104(2), 2.104(2), 2.169(2), 2.347(1) Å and 176.69(5)°, respectively.