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Synthesis of [Ni20(OH)24(MMT)12(SO 4, NO3)2·6H2O (1, A mixture of Ni(NO3)2·6H2O (0.290 g, 1 mmol, MMT (0.132 g, 1 mmol, triethylamine (0.102 g, 1.67 mmol, ethanolamine (0.072 g, 0.717 mmol, 4 mL of H2O, and 4 mL of C2H5OH was sealed in a 23 mL Teflon-lined stainless steel vessel and heated to 110 °C for 3 days and then cooled to room temperature at a rate of 0.1 °C/min. Green octahedral crystals were obtained. The product was washed with C2H5OH and dried in air 39% yield based on Ni II, Elem anal. Calcd for C36H72N 26Ni20O40S: C, 12.40; H, 2.07; N, 10.45; S, 23.87. Found: C, 12.36; H, 2.12; N, 10.50; S, 23.86
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40S: C, 12.40; H, 2.07; N, 10.45; S, 23.87. Found: C, 12.36; H, 2.12; N, 10.50; S, 23.86.
-
-
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41
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68949119082
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Crystal data of 1: C36H72N26Ni 20O40S26, MT, 3484.88, tetragonal, space group I 4, a= 13.7540(19) A, b= 13.7540(19) Å, c=28.029(6) Å, α=β= γ=90°, V=5302.3(15) Å3, Z=8, ρcalcd=2.183 g/cm3, Rint=0.0621, final R1, 0.0552 (wR2, 0.1318) for 2966 independent reflections [I > 2σ(I, Data were collected on a Bruker Smart-Apex CCD diffractometer with Mo Kα (λ, 0.71073 Å) at 298 K using the ω-scan technique. Multiscan absorption corrections were applied. The structure was solved by direct methods and refined by full matrix least squares on F2 using SHELXTL-97 software. The Flack parameter of 0.00(2) for 1 indicates that the absolute configuration is correct
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2 using SHELXTL-97 software. The Flack parameter of 0.00(2) for 1 indicates that the absolute configuration is correct.
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