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67650356726
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Preparation of [Mo2(DAniF)3](S2CC 6H4CS2)[Mo2(DAniF)3, 1, A yellow solution Of Mo2(DAniF)3(O2CCH 3, 0.102 g, 0.10 mmol) in 10 mL of THF was mixed with dipiperidinium tetrathioterephthalate (0.020 g, 0.05 mmol) in 10 mL of ethanol. After stirring for 2 h, a green microcrystalline product formed, which was filtered and washed with ethanol (2x5 mL, Yield: 0.0714 g (67, Diffusion of ethanol into a dichloromethane solution of the product affords green needle-shaped crystals. 1H NMR (CDCl3, ppm, 8.50 (s, 2H, NCHN, 8.33 (s, 4H, NCHN, 8.30 (s, 4H, aromatic H, 6.67 (d, 16H, aromatic H, 6.64 (d, 16H, aromatic H, 6.57 (d, 8H, aromatic H, 6.56 (d, 8H, aromatic H, 3.73 (s, 24H, OCH3, 3.67 s, 12H, OCH3, Anal. Calcd for C 98H94Mo4N12O12S 4
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4 (1): C, 53.81; H, 4.42; N, 7.84. Found: C, 53.98; H, 4.80; N, 7.52.
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27
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67650366059
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2 and converged for 11541 unique reflections and 648 parameters to give R1 = 0.1082 and wR2 = 0.1388 and a GOF of 0.963.
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2 and converged for 11541 unique reflections and 648 parameters to give R1 = 0.1082 and wR2 = 0.1388 and a GOF of 0.963.
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28
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37049093235
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