Two novel polyoxotantalates formed by Lindqvist-type hexatantalate and Copper-amine complexes

Inorganic Chemistry Communications

Volumn 14, Issue 9, 2011, Pages 1448-1451

  Guo, Gui Ling ^a   Xu, Yan Qing ^a   Chen, Bao Kuan ^a   Lin, Zheng Guo ^a   Hu, Chang Wen ^a  

^a BEIJING UNIVERSITY OF POSTS AND TELECOMMUNICATIONS   (China)

Author keywords

Lindqvist type; Polyoxometalates; Polyoxotantalate; Supramolecular; Water tetramer; Water trimer

Indexed keywords

EID: 79960748348     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2011.05.044     Document Type: Article

References (24)

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14. Synthesis of 1: 0.15 mmol CuI, 0.4 mmol pyrazine and 0.3 mL 1,3-dap was placed in 4 mL DMSO and 1 mL H2O mixed-solution, the resulting solution was stirred for 2 h in air, then the mixture was transferred into a 20 ml test tube. Subsequently, 4 mL 3: 1 DMSO: H2O mixed-solution and 4 mL H2O solution containing 0.05 mmol K8Ta6O19•17H2O were dropped slowly into the test tube in sequence. The test tube was sealed with film and left at room temperature. After a few weeks, blue crystals of 1 were obtained (yield: 12% base on Ta). Elemental analysis for C18H80Cu4N12Ta6O29 (%).Calcd: C, 9.52; H, 3.52; N, 7.40. Found: C, 9.38; H, 3.41; N, 7.49. Synthesis of 2: 5 mL H2O solution containing K8Ta6O19•17H2O (0.05mmmol), 5 mL 1: 4 en: H2O mixed-solution and 5 mL en solution containing 0.5 mmol Cu(CH3COOH)2•H2O were dropped slowly in a 20 mL test tube in sequence. The test tube was sealed with film and left at room temperature. After a few weeks, blue crystals of 2 were obtained (yield: 42% base on Ta). Elemental analysis for C16H92Cu4N16Ta6O33 (%). Calcd: C, 8.07; H, 3.87; N, 9.42. Found: C, 8.33; H, 4.02; N, 9.15.
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19. 2 (all data) = 0.0492. Crystal data for compound 1 was collected at 296(2) K on Bruker APEX-II CCD detector with graphite monochromatic Mo Kα radiation (λ = 0.71073 Å). Crystal data for compound 2 was collected at 93(2)K on Rigaku RAXIS-RAPID CCD diffractometer with Mo Kα radiation (λ = 0.71073 Å). The structures were solved by direct methods and refined using full-matrix least-squares calculations with anistropic thermal parameters for all non-hydrogen atoms. Thehydrogen atoms were geometrically fixed to allow riding on the parent atoms to which they are attached. All calculations were performed using the SHELXL-97 program package. CCDC reference numbers 801642 (1) and 776870 (2).
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