Synthesis and Structure of Triphenylbismuth Dinitrite and Dinitrate

Triphenylbismuth dinitrate (I) and triphenylbismuth dinitrite (II) were synthesized through the reaction of triphenylbismuth dichloride with silver nitrate in an acetone–alcohol (1 : 1) solution or with sodium nitrite in acetone–water (1 : 1) solution. According to X-ray diffraction data, bismuth atoms in Iand II have a distorted trigonal bipyramidal configuration. The intramolecular Bi···N(1,2) contacts in II (2.997(3), 2.982(4) Å) are shorter than similar contacts in I(3.038(3), 3.031(3) Å); the Bi···O(2,4) distances in II and Bi···O(2,5) distances in I are equal to 2.879(2), 2.913(3) and 2.893(3), 2.896(3) Å, respectively.     

Vitamin D Level in Summer and Winter Related to Measured UVR Exposure and Behavior

The influence of the summer UVR exposure on serum-25-hydroxyvitamin D (25(OH)D) in late summer and winter was investigated in an open study on 25 healthy, adult volunteers. The UVR exposure dose in standard erythema dose (SED) was monitored continuously during a summer season with personal, electronic wristwatch UVR dosimeters and sun exposure diaries. Constitutive and facultative skin pigmentation was measured in September. 25(OH)D was measured in September and February and was in mean 82 nmol/L ± 25 (mean ± SD) in September and 56 nmol/L ± 19 (mean ± SD) in February. The received cumulative UVR dose measured during a mean of 121 days was 156 SED ± 159 (mean ± SD). The following UVR exposure parameters correlated with 25(OH)D in September and February, respectively: (1) The cumulative UVR dose ( r  = 0.53; P  < 0.01) and ( r  = 0.43; P  = 0.03); (2) Mean daily hours with UVR measurements monitored by the dosimeter ( r  = 0.64, P  = 0.001) and ( r  = 0.53; P  = 0.007); (3) Days "with sun-exposed upper body" ( r  = 0.58, P  = 0.003) and ( r  = 0.50; P  = 0.01); (4) Facultative pigmentation ( r  = 0.47; P  < 0.02) and ( r  = 0.7; P  < 0.001); (5) Constitutive pigmentation ( r  = 0.06, n.s.) and ( r  = 0.43, P  = 0.03). Neither days "sunbathing" nor days with "sunscreen applied" correlated with 25(OH)D. The fall in 25(OH)D during winter was dependent on the entry value.     

3,3′‐Dinitro‐2,2′‐dithiodipyridine

In the title compound, C₁₀H₆N₄O₄S₂, (I), the molecule has a centre of inversion. The structure is a positional isomer of 5,5′‐dinitro‐2,2′‐dithiodipyridine [Brito, Mundaca, Cárdenas, López‐Rodríguez & Vargas (2007). Acta Cryst. E 63 , o3351–o3352], (II). The 3‐nitropyridine fragment of (I) shows excellent agreement with the bonding geometries of (II). The most obvious differences between them are in the S—S bond length [2.1167 (12) Å in (I) and 2.0719 (11) Å in (II)], and in the C—C_ipso—N_ring [119.8 (2)° in (I) and 123.9 (3)° in (II)] and S—C—C [122.62 (18)° in (I) and 116.0 (2)° in (II)] angles. The crystal structure of (I) has an intramolecular C—H...O interaction, with an H...O distance of 2.40 (3) Å, whereas this kind of interaction is not evident in (II). The molecules of (I) are linked into centrosymmetric R⁴₄(30) motifs by a C—H...O interaction. There are no aromatic π–π stacking and no C—H...π(arene) interactions. Compound (I) can be used as a nucleophilic tecton in self‐assembly reactions with metal centres of varying lability.     

Polarographische und oszillopolarographische Untersuchungen in Trimethylphosphat

Zusammenfassung Das polarographische und oszillopolarographische Verhalten der Perchlorate von Tl(I), Rb(I), K(I), Na(I), Ba(II), Zn(II), Cd(II), Mn(II), Co(II), Ni(II) sowie von Bisbiphenylchrom(I) jodid wurde in wasserfr. Trimethylphosphat (0,1M-Tetraäthylammoniumperchlorat) untersucht. Die Halbwellenpotentiale bei 25° gegen die gesättigte wäßr. Kalomelelektrode werden auf die Bisbiphenylchrom(I)jodid-Skala bezogen.Die Beziehung zwischen Donorzahl des Lösungsmittels undE _1/2 ist erfüllt. Eine Ausnahme, welche auf Chelatbildung zurückzuführen sein dürfte, bilden die in Trimethylphosphat gemessenen Werte für Mn(II), Co(II) und Ni(II).

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Polarographic and oscillopolarographic investigations in trimthhyl phosphate

Polarographic and oscillopolarographic investigations have been carried out on the perchlorates of Tl(I), Rb(I), K(I), Na(I), Ba(II), Zn(II), Cd(II), Mn(II), Co(II), Ni(II) and of bisbiphenylchromium(I)iodide in anhydrous trimethylphosphate (0,1M tetraethylammoniumperchlorate). The half-wave potentials at 25° vs. the aqueous saturated calomel electrode are referred to the bisbiphenylchromium(I)iodide-scale. The relationship between donor number of the solvent andE _1/2 is observed. An exception is given for Mn(II), Co(II) and Ni(II) in trimethylphosphate, which is regarded as due to chelate formation.

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Mit 5 Abbildungen     

Structures involving unshared electron pair. The Crystal Structures of As(OCOCH3)3 and As2O(OCOCH3)4

As₂O(OCOCH₃)₄, reported now for the first time, was obtained, besides As(OCOCH₃)₃ by dissolving As₂O₃ in acetic anhydride. The crystals of As(OCOCH₃)₃ (A) (monoclinic, space group Cc, Z = 4, a = 9.970(2), b = 13.203(2), c = 8.272(1) Å, β = 117.01(2)°) and of As₂O(OCOCH₃)₄ (B) (monoclinic, space group P2₁/n, Z = 4, a = 13.966(5), b = 8.127(4), c = 12.706(4) Å, β = 95.14(1)°) are built up from discrete molecules defined by chemical formulae As(OCOCH₃)₃ and (CH₃OCO)₂As? O? As(OCOCH₃)₂, respectively. The molecular structure of both compounds is based on the AsO₃ pyramid: in (A) with the As? O bonds of 1.841(6) Å and the O? As? O angle of 89.9(3)° as a mean, in (B) with slightly different values and with the As? O? As angle of 127.7(4)° at the bridging oxygen atom. The additional weak chelating contacts are at the distances As…O from 2.625(9) to 2.745(10) Å in (A) and from 2.72(1) to 2.84(2) in (B). The actual arsenic coordination can be described as very distorted octahedral in (A) and square-pyramidal in (B).     

Synthesis and characterization of heterobimetallic Ni(II)–Zn(II) complexes from bis(2-hydroxy-1 -naphthaldehyde)succinoyldihydrazone

Monometallic zinc(II) and nickel(II) complexes, [Zn(H₂nsh)(H₂O)] (1) and [Ni(H₂nsh)(H₂O)₂] (2), have been synthesized in methanol by template method from bis(2-hydroxy-1-naphthaldehyde)succinoyldihydrazone (H₄nsh). Reaction of monometallic complexes with alternate metal(II) acetates as a transmetallator in 1 : 3 molar ratio resulted in the formation of heterobimetallic complexes [NiZn(nsh)(A)₃] and [ZnNi(nsh)(A′)₂] (A = H₂O (3), py (4), 2-pic (5), 3-pic (6), 4-pic (7)), (A′ = H₂O (8), py (9), 2-pic (10), 3-pic (11), and 4-pic (12)). The complexes have been characterized by elemental analyzes, mass spectra, molar conductance, magnetic moments, electronic, EPR, and IR spectroscopies. All of the complexes are non-electrolytes. Monometallic zinc(II) is diamagnetic while monometallic nickel(II) complex and all heterobimetallic complexes are paramagnetic. The metal centers in heterobimetallic complexes are tethered by dihydrazone and naphthoxo bridging. Zinc(II) is square pyramidal; nickel(II) is six-coordinate distorted octahedral except [ZnNi(nsh)(A)₂], in which nickel(II) has square-pyramidal geometry. The displacement of metal center in monometallic complexes by metal ion has been observed in the resulting heterobimetallic complexes.     

Synthesis and Structure of Triphenylbismuth Bis(Fluorobenzoates)

The reaction between triphenylbismuth, hydrogen peroxide, and 3,4,5-trifluorobenzoic or pentafluorobenzoic acid (molar ratio 1 : 1 : 2, respectively) in ether gave triphenylbismuth bis(3,4,5-trifluorobenzoate) (I) and triphenylbismuth bis(pentafluorobenzoate) (II) in 74 and 89% yields, respectively. The structures of compounds I and II were established by X-ray diffraction. The Bi atoms have a distorted trigonal-bipyramidal coordination with acylate groups in the axial positions. The OBiO angles are 170.2(2)° and 171.5(2)° in I and II, respectively. The Bi–C(Ph)_eq bond lengths vary in the range of 2.187(6)–2.204(5) Å, the Bi–O(acyl) lengths are 2.256(5) Å in I, and 2.281(5) and 2.318(5) Å in II. In the crystals I and II, the Bi and carbonyl O atoms are involved in intramolecular interactions (Bi···O(=C) 2.926(5)–3.176(5) Å), which increase the equatorial CBiC angles on the side of these contacts to 136.2(3)° and 138.6(2)° in I and II, respectively.     

Studies on the Stereochemistry of 2-(Nitromethylidene)-Heterocycles

The ¹H-NMR spectra of 2-(nitromethylidene)pyrrolidine ( 7 ), 1-methyl-2-(nitromethylidene)imidazolidind ( 10 ) and 3-(nitromethylidene)tetrahydrothiazine ( 11 ) in CDCl₃ and (CD₃)₂SO indicate that these compounds have the intramolecularly H-bonded structures (Z)- 7 , (E)- 10 and (Z)- 11 while the N-methyl derivative 8 of 7 is (E)-configurated in both solvents. 1-Benzylamino-1-(methyltio)-2-nitroehtylene ( 13 ), an acylic model, has the H-bonded configuration (E)- 13 in CDCl₃ and in (CD₃)₂SO. 2-(Nitromethylidene)thiazolidine ( 3 ) has the (E)-configuration in CDCl₃ but exists in (CD₃)₂SO as a mixture of (Z)- and (E)-isomers with the former predominating. Both species are detected to varying proportions in a mixture of the two solvents. ¹⁵N-NMR spectroscopy of 3 ruled out unambiguously the nitronic acid structure 6 and the nitromethyleimine structure 5 . The N-methyl derivative 4 of 3 is (Z)-configurated in (CD₃)₂SO. Comparison of the olefinic proton shifts of (Z)- 3 and (Z)- 4 with those of analogues and also of 1,1-bis(methylti)-2-nitroethylene ( 12 ) shows decreased conjugation of the lone pair of electrons of the ring N-atom in (Z)- 3 and (Z)- 4 . This is also supported by ¹³C-NMR studies. Plausible explanations for the phenomenon are offered by postulating that the ring N-atoms are pyramidal in (Z)- 3 and (Z)- 4 and planar in other cases or, alternatively, that the conjugated nitroenamine system gets twisted due to steric interaction between the NO₂-group and the ring S-atom. Single-crystal X-ray studies of 3 and 8 show that the former exists in the (Z)-configuration and the latter in (E)-configuration; the ring N-atom in the former has slightly more pyramidal character than in the latter.     

Spectral study of the complexation of Nd(III) with glutathione reduced (GSH) in the presence and absence of Zn(II) in aquated organic solvents

Studies on the difference in energy parameters and comparative absorption spectrophotometry involving 4f-4f transitions on Nd(III) and glutathione reduced (GSH) in the absence and presence of Zn(II) have been carried out in aquated organic solvents (50 : 50) like methanol, dioxane, acetonitrile and dimethylformamide. Variations in the spectral energy parameters — Slater-Condon (F _k ) factor, Lande spin-orbit coupling constant (ξ4f), nephelauxetic ratio (β), bonding parameter (b ^1/2 ) and percent covalency (δ) — are calculated and correlated with binding of Nd(III) with GSH in presence and absence of Zn(II).     

Partitioning of para-phenylenediamines in oil-in-water emulsions

A method to measure distribution coefficients (P) of electroactive species in situ in turbid oil-in-water emulsions is demonstrated using four p-phenylenediamines (PPD) in oil-in-aqueous-gelatin emulsions of six oils at 40°C. The PPD examined represent a series in β-X-ethyl substitution (4-amino-3-methyl-N-ethyl-N-(β-X-ethyl)aniline) where X = H (2), OH (3), methylsulfonamide (4), and methoxyethyl (5), respectively, for PPD 2–5. The oils examined include di-n-butyl phthalate (DBP), N,N-diethyldodecanamide (DEDA), 1-octanol (OCA), 1-undecanol (UNA), tri-n-hexyl phosphate (THP), and dodecane (DOD). The rotating platinum disk electrode (RPDE) is used as a voltammetric probe of PPD concentration in the aqueous-gelatin phase of the emulsions. Distribution coefficients in macroscopic aqueous/oil systems are also reported, and are illustrated to correlate linearly with values determined in emulsions. The distribution coefficients (P = C_oilC_aqueus) for the different PPD decrease in the order 2 > 5 > 3 ≈ 4 for each of the six oils. The largest distribution coefficients are obtained with THP, and the smallest are obtained with DOD. The interface appears to play a significant role in modifying solute distribution in emulsions.     

Synthesis and structural features of tris(5-bromo-2-methoxyphenyl)antimony dicarboxylates

Tris(5-bromo-2-methoxyphenyl)antimony bis(4-nitrophenylacetate) (I), tris(5-bromo-2-methoxyphenyl)antimony bis(2-methoxybenzoate) (II), and tris(5-bromo-2-methoxyphenyl)antimony bis(phenylpropiolate) (III) have been synthesized via the reaction between tris(5-bromo-2-methoxyphenyl) antimony and 4-nitrophenylacetic acid, 2-methoxybenzoic acid, and phenylpropiolic acid, respectively, in the presence of hydrogen peroxide (molar ratio: 1: 2: 1). According to X-ray diffraction data, the antimony atom in molecules of complexes I–III has a distorted trigonal bipyramidal coordination. The OSbO axial angles and the CSbC bond angles in the equatorial plane are 173.27(15)°, 172.96(11)°, 172.99(10)°, and 115.5(2)°–123.3(2)°, 108.81(16)°–129.32(17)°, and 110.66(17)°–127.91(17)°, respectively. The Sb-O bond lengths are 2.092(4) and 2.115(4)Å in I, 2.088(3) and 2.097(2) Å in II, and 2.096(3) and 2.120(3) Å in III. The Sb-C bonds range within 2.095(6)–2.123(6) Å in I, 2.107(4)–2.117(4) Å in II, and 2.097(4)–2.116(4) Å in III. Complexes I, II, and III are observed to have intramolecular Sb…OCH₃ contacts (3.169–3.226, 3.134–3.174, and 3.147–3.196 Å, respectively) in addition to Sb…O=C interactions (3.121, 3.139Å; 2.944, 3.038 A0; 3.111, 3.120 Å).     

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.     

Determination of As(III) and As(V) in soils using sequential extraction combined with flow injection hydride generation atomic fluorescence detection

An analytical procedure for determination of As(III) and As(V) in soils using sequential extraction combined with flow injection (FI) hydride generation atomic fluorescence spectrometry (HG-AFS) was presented. The soils were sequentially extracted by water, 0.6 mol l⁻¹ KH₂PO₄ solution, 1% (v/v) HCl solution and 1% (w/v) NaOH solution. The arsenite (As(III)) in extract was analyzed by HG-AFS in the medium of 0.1 mol l⁻¹ citric acid solution, then the total arsenic in extract was determined by HG-AFS using on-line reduction of arsenate with l-cysteine. The concentration of arsenate (As(V)) was calculated by the difference. The optimum conditions of extraction and determination were studied in detail. The detection limit (3σ) for As(III) and As(V) were 0.11 and 0.07 μg l⁻¹, respectively. The relative standard deviation (R.S.D.) was 1.43% (n=11) at the 10 μg l⁻¹ As level. The method was applied in the determination of As(III) and As(V) of real soils and the recoveries of As(III) and As(V) were in the range of 89.3-118 and 80.4-111%, respectively.     

Headspace gas chromatographic separation of toxic organic impurities from air

Summary To determine toxic organic compounds (methanol, ethanol, n-propanol, acetone, methyl ethyl ketone, methyl isobutyl ketone) in air a method was developed for their headspace gas chromatographic analysis with preconcentration in n-butanol (alcohols) and in n-pentanol (ketones). The distribution coefficients of analytes in the air-absorbent system have been measured: 1051 (MeOH), 5630 (EtOH), 6773 (n-PrOH), 307 (Me₂CO), 580 (MeCOEt), 1035 (MeCOBu-i). The minimum detectable level (mg m⁻³) was determined as low as 0.9 (MeOH), 4.0 (EtOH), 0.9 (n-PrOH), 0.2 (Me₂CO), 0.1 (MeCOEt), 0.4 (MeCOBu-i). The method was effectively used for gas effluent air control in the workplace and in the atmosphere. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996     

X-ray photoelectron spectroscopy study of neodymium niobate and tantalate precursors and thin films

Neodymium niobate NdNbO₄ (NNO) and tantalate NdTaO₄ (NTO) thin films (~100 nm) were prepared by sol-gel/spin-coating process on Al₂O₃ substrate with LaNbO₄/PbZrO₃ interlayer and annealing at 1000°C. Surface chemistry was investigated by X-ray photoelectron spectroscopy (XPS). The core-level XPS studies of sol-gel NNO and NTO were performed for the first time. The binding energy differences Δ(O―Nb) and Δ(O―Ta) were used to characterize average energies of Nb―O bonding in NNO (322.9 eV) and Ta―O bonding in NTO (504.2 eV). The XPS demonstrated single valence state of Nd (Nd³⁺) in precursors. Nd concentration (at. %) decreases from 22% in precursors to 7% in films considering the substrate contains C, Al, Si, Pb, and Zr elements (37%) at Nb or Ta (5%) and O (51%). The X-ray diffraction analyses verified formation of the monoclinic (M-NdNbO₄ or M′-NdTaO₄), orthorhombic (O-NdNbO₄) and tetragonal (T-NdTaO₄) phases in precursors and films. Single valence state of Nd³⁺ was confirmed in these films designed for the application in environmental electrolytic thin film devices.     

Alkaline metal oxoantimonates(III), A3[SbO3] (A = K or Cs)

The two title trialkaline trioxoantimonates(III), tripotassium trioxoantimonate(III), K₃[SbO₃], (I), and tricaesium trioxo­antimonate(III), Cs₃[SbO₃], (II), crystallize in the cubic Na₃[AsS₃] structure type in space group P2₁3. The structures show discrete Ψ-tetrahedral [SbO₃]³⁻ anions with C_3v point-group symmetry. The Sb—O distances are 1.923 (4) Å in (I) and 1.928 (2) Å in (II), and the O—Sb—O bond angles are 99.5 (2)° in (I) and 100.4 (1)° in (II).     

Polarographische Bestimmung von Molybd?n neben anderen Metallen

Zusammenfassung Es wird eine polarographische Bestimmungsmethode für Molybdän in Gegenwart anderer Metalle beschrieben. Molybdän(VI) gibt in Anwesenheit einer 0,25 M Ammoniumtartratlösung eine gut reproduzierbare Reduktionsstufe bei E _1/2= – 1,27 V (GKE). Die Methode wurde mit guten Ergebnissen bei der Molybdänbestimmung in Legierungen (Fehler ±1%) und mineralischem Gestein (Fehler –2%) angewandt. Der störende Einfluß von größeren Mengen Chrom(VI) wird durch ein beschriebenes säulen-chromatographisches Trennverfahren mit Hilfe des Anionenaustauschers Wofatit SBW beseitigt. Ein zehnfacher Überschuß an W(VI), Mn(II), Ni(II), Cu(II) und Tl(I) sowie gleiche Mengen an Fe(II), Fe(III), Cd(II), Co(II), V(V) und Bi(III) stören nicht.

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Summary A polarographic method for the determination of molybdenum in presence of other metals is described. Molybdenum (VI) yields a well-defined cathodic wave in ammonium tartrate medium (0.25 M) at E _1/2= –1.27 V vs. S.C.E. The results obtained have been applied to the determination of molybdenum in ores (error ±1%) and alloys (error –2%). The interfering influence of greater amounts of chromium(VI) is eliminated by ion-exchange with the strongly basic anion-exchanger Wofatit SBW. A ten-fold excess of W(VI), Mn(II), Ni(II), Cu(II) and Tl(I) as well as equal amounts of Fe(II), Fe(III), Cd(II), Co(II), V(V) and Bi(III) do not interfere.

     

Fluorenylsilane : III. Über die umsetzung von 9-fluorenyl-tris(trimethylsilyl)silan mit chlor

9-Fluorenyltris(trimethylsilyl)silane (A) reacts with chlorine in CCl₄ to give dichloro-9-fluorenyltrimethylsilylsilane (B) in good yield. B is characterized spectroscopically and by X-ray structure analysis; it crystallizes in the triclinic space group P$\text{1}$ with a 950(2), b 1367(3), c 1138(2) pm, α 137.5(1), β 109.9(2), γ 89.8(2)°. The conformation of B is staggered with approximate C_s-symmetry; C(9)Si 187.6(5), SiSi 233.2(4), SiCl 207.1(3) and 205.3(3) pm.     

Hydrido-Silyl-Komplexe. V. Strukturelle Änderungen in Hydrido-Silyl-Komplexen infolge Si?H-Wechselwirkung; Strukturvergleich zwischen (π-CH3C5H4)(CO)2Mn(H)SiR3- und analogen (π-C5H5)(CO)2FeSiR3-Komplexen

Hydrido Silyl Complexes. V. Structural Changes in Hydrido Silyl Complexes Due to Si? H Interaction; Comparison between the Structures of (π-CH₃C₅H₄)(CO)₂Mn(H)SiR₃ and Analogous (π-C₅H₅)(CO)₂FeSiR₃ Complexes The structures of the complexes Cp(CO)₂FeSiFPh₂ ( 2a ) and Cp(CO)₂FeSiCl₃ ( 2b ), containing ?normal”? metal-silicon bonds, are compared with the known structures of the complexes MeCp(CO)₂Mn(H)SiFPh₂ ( 1a ) and MeCp(CO)₂Mn(H)SiCl₃ ( 1b ), containing Mn? H? Si three-center bonds. 2a crystallizes in space group P2₁/c, a = 805.8(3), b = 1417.5(6), c = 1498.2(4) pm, β = 90.99(3)°, 2b in space group P2₁/n, a = 817(1), b = 1244(1), c = 1142(1)pm, β = 99.9(1)°. In 2a gauche conformation in respect to the Fe? Si bond is found; in 2b the silylligand is rotated 12° around the Fe? Si axis out of a staggered conformation. Possible reasons for the unsymmetrical conformations are discussed. Lengthening of the Fe? Si distance from 221.6(1)pm in 2b to 227.8(1) pm in 2a corresponds to the expected increase in the bond radius of silicon due to exchange of the substituents at silicon. Additional lengthening of the Mn? Si distance by about 3.5 pm in 1a compared with 1b is attributed to the increased delocalization of the Mn? H? Si bond in 1a .     

Synthesis and Structure of Triphenylantimony Dipropionate

Triphenylantimony dipropionate Ph₃Sb[OC(O)C₂H₅]₂was prepared by reacting triphenylantimony dibromide with sodium salt of propionic acid in toluene at 90°C. The structure of the compound was determined by X-ray diffraction. The coordination of the Sb atom in the compound is a trigonal bipyramid with the carboxylic groups in the axial positions. The Sb(1)–C(Ph)_eqdistances vary in the 2.099(7)–2.135(6) Å range; the Sb(1)–O(1,3) distances are 2.113(5) and 2.109(5) Å, respectively. The value of the O(1)Sb(1)O(3) axial angle is 175.0(2)°.