Synthesis and Structural Characterization of Three New Inorganic “Host-guest”Polyoxomolybdates

来源 :Chinese Journal of Chemistry | 被引量 : 0次 | 上传用户:luoxueyan191
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Since two interesting inorganic “host guest” polyoxomolybdates 1 and 2 have been reported previously, we have now succeeded in selectively isolating three new acetated “host guest” polyoxomolybdates 3—5, which considerably extend the range of structures in the cyclic polyoxomolybdate catalogue. 3 crystallizes in the triclinic space group P 1 with a =1 22235(1) nm, b =1 52977(2) nm, c =1 54022(1) nm, α =113 746(1)°, β =96 742(1)°, γ = 101 564(1)°, V =2 51892(4) nm 3, Z =1, D c=2 568 g·cm -3 . 4 and 5 crystallize in the monoclinic system: P 2(1)/ n , a =1 08298(2) nm, b =1 54029(1) nm, c = 2 78893(5) nm, β =94 2730(10)°, V =4 63929(12) nm 3, Z =2 and D c=2 671 g·cm -3 for 4, and C 2/ c , a =2 59907(8) nm, b =1 65992(3) nm, c =2 28473(7) nm, β = 93 4370(10)° , V =9 8392(5) nm 3, Z =4 and D c=2 556 g·cm -3 for 5. The structures of 3, 4 and 5 consist of 18 membered “host guest” polyoxoanions [{Na(X) 2}{( μ 3 OH) 4Mo V 8Mo VI 10 O 52 ( μ 2 CH 3COO) 2}] -( n +9) (X=CH 3COO - for 3, DMF for 4 and H 2O for 5), which are connected via Na + ions or hydrogen bonds into infinite extended frameworks. Since two interesting inorganic “host guest” polyoxomolybdates 1 and 2 have been reported previously, we have now succeeded in selectively isolating three new acetated “host guest” polyoxomolybdates 3-5, which determines the structure of the cyclic polyoxomolybdate catalog. 3 crystallizes in the triclinic space group P 1 with a = 1 22235 nm, b = 1 52977 nm, c = 1 54022 nm, α = 113 746 °, β = 96 742 (1) 1) °, γ = 101 564 (1) °, V = 2 51892 (4) nm 3, Z = 1, D c = 2 568 g · cm -3. 4 and 5 crystallize in the monoclinic system: B = 1 54029 (1) nm, c = 2 78893 (5) nm, β = 94 2730 (10) °, V = 4 63929 (12) nm 3 , Z = 2 and D c ​​= 2 671 g · cm -3 for 4 and C 2 / c, a = 2 59907 (8) nm, b = 1 65992 (3) nm and c = 2 28473 (7) nm , β = 93 4370 (10) °, V = 9 8392 (5) nm 3, Z = 4 and D c ​​= 2 556 g · cm -3 for 5. The structures of 3, 4 and 5 of 18 membered “host guest” polyoxoanions [{Na (X) 2}  {(μ 3 OH) 4Mo V 8Mo VI 10 O 52 (μ 2 CH 3COO) 2}] - (n + 9) (X = CH 3 COO - for 3, DMF for 4 and H 2 O for 5), which are connected via Na + ions or hydrogen bonds into infinite extended frameworks.
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