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Th[C6H3(CO2)3F]·0. 3H2O was synthesized by combining N(CH3)4Cl (0.219 g, 2.00 × 10-3 mol, Th(NO3) 4·6H2O (0.588 g, 1.00 × 10-3 mol, 1,3,5-C6H3(CO2H)3 (0.078 g, 3.71 × 10-4 mol, HCON(CH3)2 (0.25 mL, water (5 mL, and HF(aq, 40, 0.14 g) in a Teflon lined stainless steel autoclave and heating to 140°C for 24 h, before being cooled to room temperature at a rate of 3°C h-1. The mother liquor was decanted from the products, which were then sonicated and washed with water. Light yellow needle crystals were recovered by filtration. A yield of 78, based on thorium) was observed. IR data cm-1, 3586, 2867, 1612, 1529, 1438, 1367, 1228, 1112, 936, 761, 624, 608, 544, 519. Elemental analysis. Calcd: C, 23.30; H, 0.78
-
-1): 3586, 2867, 1612, 1529, 1438, 1367, 1228, 1112, 936, 761, 624, 608, 544, 519. Elemental analysis. Calcd: C, 23.30; H, 0.78; Th, 50.07. Exptl: C, 23.66; H, 0.68; Th, 50.02.
-
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25
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84885423732
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2].
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2].
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13C MAS NMR gave four resonances at 172.9 ppm, 172.1 ppm, 135.0 ppm, and 133.7 ppm which are assigned to the carbon atoms on the benzene ring. The carbonyl carbons were not observed, presumably due to its slow relaxation time.
-
13C MAS NMR gave four resonances at 172.9 ppm, 172.1 ppm, 135.0 ppm, and 133.7 ppm which are assigned to the carbon atoms on the benzene ring. The carbonyl carbons were not observed, presumably due to its slow relaxation time.
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