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Inorganic Chemistry

Volumn 46, Issue 11, 2007, Pages 4383-4385

13-Tungstoborate stabilized by an organostannoxane hexamer

(4) Reinoso, Santiago a Dickman, Michael H a Matei, Marius F a Kortz, Ulrich a

a JACOBS UNIVERSITY BREMEN (Germany)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 34250705817 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic7004437 Document Type: Article

Times cited : (36)

References (42)

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- 2O was synthesized according to ref 4e.
- 2O was synthesized according to ref 4e.

37
- 34250747658
- 2O (0.642 g, 0.2 mmol) was added. The reaction mixture (pH 4.0) was heated at ∼70°C for 30 min. After cooling down to room temperature, aqueous 1 M NaCl solution (2.5 mL) was added to the resulting clear solution. Plate-like colorless crystals suitable for X-ray diffraction were formed in a few days by slow evaporation of the solvent at room temperature.
- 2O (0.642 g, 0.2 mmol) was added. The reaction mixture (pH 4.0) was heated at ∼70°C for 30 min. After cooling down to room temperature, aqueous 1 M NaCl solution (2.5 mL) was added to the resulting clear solution. Plate-like colorless crystals suitable for X-ray diffraction were formed in a few days by slow evaporation of the solvent at room temperature.

38
- 34250753032
- Synthesis of 1a: To a solution of Na2WO 4·2H2O (0.132 g, 0.4 mmol) and (CH 3)2SnCl2 (0.132 g, 0.6 mmol) in aqueous 1 M KCl (30 mL) solid K8[HBW11O39]·13H 2O (0.642 g, 0.2 mmol) was added. The reaction mixture (pH 4.7) was heated at ∼70°C for 30 min, leading to a cloudy solution which was filtered while hot and then left for evaporation of the solvent in an open beaker. Compound 1a was obtained overnight as a crystalline powder (yield: 0.322 g, 39% based on Sn, Anal. Calcd (found) for C12H 106B2K12O128Sn6W 26: C, 1.74 (1.62, H, 1.29 (1.27, B, 0.26 (0.20, K, 5.67 (5.50, Sn, 8.60 (8.74, W, 57.7 (58.1, IR, KBr pellets, cm-1, 1229(w, 1203(sh, 1065(sh, 968(m, 952(s, 902(s, 835(vs, 780(vs, 769(sh, 742(sh, 636(m, 549(sh, 517(m, 451w, TGA/DS
- 26: 91.37 (91.40)].

39
- 34250729330
- Crystal data for 1a: C12H106B 2K12O128Sn6W26, fw, 8282.0 g·mol-1, triclinic, P1 space group; a, 12.2644(8) Å, b, 13.0387(12) Å, c, 23.392(2) Å, α, 91.952(5)°, β, 96.536(5)°, γ, 111.559(4)°, V, 3444.7(5) Å3, Z, 1, ρcalcd, 4.015 g·cm-3, μ, 23.144 mm -1; 93 894 collected reflns, 14 054 unique (Rint, 0.191, 7770 observed [I > 2σ(I, 490 params, R(F, 0.065 [I > 2σ(I, wR(F)2, 0.180 (all data, GOF, 1.008; Bruker X8 APEX II CCD diffractometer, T, 173(2) K, λMo Kα, 0.71073 Å
- 2 = 0.180 (all data), GOF = 1.008; Bruker X8 APEX II CCD diffractometer, T = 173(2) K, λ(Mo Kα) = 0.71073 Å.

40
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