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Diffraction data for 1 and 2 were collected on a Bruker X8 Apex CCD diffractometer with MoKα radiation (λ, 0.71073 Å) by using φ and ω scans of narrow (0.5°) frames at 90.0(2, 1) and 100.0(2) K (2, The structures were solved by direct methods with the SIR2004 program[13] and refined by full-matrix least-squares treatment against, F |2 in anisotropic approximation using the SHELXTL program suite.[14] Absorption corrections were applied empirically using SADABS program [15] for 1 and numerically for 2 using Bruker X8Apex Software.[16] 1: H40AsCs6.50KMo 3N1.50O70S4W15, Mr, 5333.08; 0.09 x 0.05 x 0.02 mm3; triclinic, space group P1, a, 13.0784(2, b, 16.0985(3, c, 20.2299(4) Å, α, 97
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Further details of the crystal structure investigations may be obtained from the Fachinformationszentrum Karlsruhe, 76344 Eggenstein-Leopoldshafen, Germany (fax:, 49)7247-808-666; e-mail: crysdata@fiz-karlsruhe.de) on quoting the depository numbers CSD-418320 (1) and -418333 2
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Further details of the crystal structure investigations may be obtained from the Fachinformationszentrum Karlsruhe, 76344 Eggenstein-Leopoldshafen, Germany (fax: (+49)7247-808-666; e-mail: crysdata@fiz-karlsruhe.de) on quoting the depository numbers CSD-418320 (1) and -418333 (2).
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The 183WNMR spectra were obtained on a Bruker MSL300 spectrometer at 12.5 MHz. As external standard an aqueous solution of H 4[SiW12O40] was used to which some Cr 3+ was added, 103.7 ppm, taking the chemical shift of Na 2WO4 in aqueous solution as 0 ppm, Due to low solubility of 1 the NMR experiments were run with sodium salts, which were obtained in the same way by using Na9[AsW9O33] ·13H2O and cluster aqua complexes without introduction of other cations. The products were precipitated with ethanol and redissolved in 2.5 mL of 2M NaCl to give approximately 0.1M concentration of the POM
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