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note
-
The number of crystallized water molecules in the formula of 1 was established by elemental analysis and TG analysis. The elemental analysis found: C, 8.48; H, 1.94; N, 1.57% (calcd: C, 8.25; H, 1.81; N, 1.48%). The ICP analysis showed that 1 contained 58.95% W, 3.22% Ni and 1.18% P (calcd: W, 58.31; Ni, 3.10; P, 1.09%). The TG curve of 1 (Figure S8, Supporting Information) shows a total weight loss of 20.22% in the range of 46-685 °C, which agrees with the calculated value of 19.99%. The weight loss of 9.64% at 46-320 °C corresponds to the loss of all crystallized water molecules and coordinated water molecules (calc. 9.52%). The weight loss of 10.58% at 340-685 °C arises from the loss of bpp ligands (calc. 10.47%).
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-1): 3394 (br), 1614 (s), 1558 (w), 1504 (w), 1425 (m), 1224 (w), 1081 (vs), 1025 (w), 948 (s), 881 (w), 784 (vs) and 520 (m) (Figure S9, Supporting Information).
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note
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