The Preparation and Crystal Structure of Ammonium Bis (glycolato) antimony (III), the First Structurally Characterised Discrete Monomeric Four-Coordinate Complex of Antimony (III) with a Dianionic α-Hydroxy Acid

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• Preparation: The complex was prepared by refluxing 1:2 stoichiometric quantities of antimony(III) chloride (0.46 g, 2 mmol) and glycolic acid (hydroxyacetic acid) (0.30 g, 4 mmol) in dilute aqueous ammonia solution (40 cm3, 10% solution) for 30 mins. then reducing the volume to ca. 20 cm3. Large colourless crystals (m.pt. 218–220°) formed after several weeks standing at room temperature. The infrared spectrum and elemental analysis (C, H, N) indicated the formula NH4[Sb(C2H2O3)2] [Found:C, 16.4; N,2.8;N, 4.9%. Calc. for C4H8NO6Sb:C, 16.7;H, 2.8;N,4.9%]
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• a Crystal data: C4H8NO6Sb, Mr = 287.9, monoclinic, space group Ia (variant of Cc) a = 6.210(1), b = 16.108(1), c = 8.427(1)Å, β = 110.404(7)°, V = 790.1(2)Å3; Z = 4,D, = 2.420gcm−3, Dm, = 2.40 gcm−3; F(000) 552, μ(Mo-Kα) = 34.9 cm−1; T = 298(2) K. b Data collection, structure solution and refinement: Data were collected on an Enraf-Nonius CAD-4 diffractometer (monochromatic Mo Kα radiation, λ = 0.71073 Å) from a cleaved specimen (0.20 × 0.18 × 0.15mm). 762 reflections, collected up to 20max = 50°, were corrected for absorption using semi-empirical (psi scan) methods.17 The structure was solved by Patterson methods (SHELXS-8618) and refined (on F 2), with all non-hydrogen atoms anisotropic (SHELXL-9319). Hydrogens were included at calculated positions and their positional and thermal parameters refined. Final residuals R[= Σ{| F0| –| Fc‖/‖F0‖}], wR [ = {Σw(F2 0 – F2 0)2/Σw(F2 0)}1/2] {with w = 1/ [σ2F2 0 + (0.0302P)2], where P = [max (F2 0, 0) + 2F2 0]/3}, and S were 0.017, 0.043 and 1.06, respectively, for 747 reflections with I > 2.0σ(I). The maximum peak in the final difference map was 0.28eÅ−3. The absolute configuration was confirmed using the method of Flack20 [absolute structure parameter, - 0.02(4)]
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