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65249123391
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For the preparation of compound 1. homophthalic acid (0.077 g, 0.43 mmol) and 2 equiv of potassium hydroxide (0.048 g, 0.85 mmol) were dissolved in a 9:1 mixture of methanol and water (15 mL, whereupon 1 equiv of dimethyltin dichloride (0.094 g, 0.43 mmol) dissolved in methanol (5 mL) was added. A white microcrystalline precipitate formed that was insoluble in common organic solvents. Yield: 0.039 g (34, Mp >220 °C (dec, 1R (KBr, ṽ, 3436 (m, 3072 (w, 3004 (w, 2919 (w, 1590 v as(OCO, s, 1551 vas(OCO, s, 1395 vs(OCO, s, 1365 vs(OCO, s, 1195 (w, 1163 (w, 1090 (w, 1047 (w, 937 (w, 802 (m, 730 (m, 641 (s, 581 (m, 497 (m, 447 (w) cm-1. C13H18O5Sn2•2.17H2O 530.69, calcd. C 29.42, H 4.24; found C 29.54, H 4.13
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2O (530.69): calcd. C 29.42, H 4.24; found C 29.54, H 4.13.
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36
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65249156991
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Crystal data: C13H18O5Sn 2-2.17H2O, Mr, 530.69 g mol-1, 0.23 × 0.27 × 0.33 mm3, trigonal, space group R3, T, 100(2) K, a= 32.1550(14, c, 9.3233(6) Å, V, 8348.3(7) Å3, Z, 18, pcalcd, 1.900, μ, 2.720 mm-1, 2θmax, 25.00, 22 241 measured and 3264 independent reflections (Rint= 0.029, R1, 0.023 for 3227 reflections with, > 2σ(I) and wR 2, 0.059 for all data, 202 parameters, GOF, 1.17. CCDC 710846
-
2 = 0.059 for all data, 202 parameters, GOF = 1.17. CCDC 710846.
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37
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84990507521
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It should be noticed that different isomers of bis(tetraorganodistan- noxanes) are known, which differ from each other by the number of carboxylate groups acting as syn-syn bidentate bridges between the tetranuclear Sn 4O2 core. For reviews see: (a) Tiekink, E. R. T. Appl. Organomet. Chem. 1991, 5, 1-23
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