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16
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85030822744
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note
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-1): ν(Cl-O), 1148, 1117, 1086 ; 1660 (broad), 1598, 1475, 1373, 779, 682, 630 (pao)
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17
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85030818439
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note
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2O (325 mg in 20 ml) are added 146 mg of Hpao and 48 mg of NaOH in 30 ml of MeOH. Sodium acetate (84 mg) is then added under stirring to the resulting dark brown solution. Stirring is continued for about 45 min and the solution is filtrated. The filtrate is then put under a saturated vapour of ether, resulting in the slow formation of dark crystals
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18
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85030825829
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note
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2) = 0.1125 for 5319 reflections with I > 2σ(I)
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19
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85030825682
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note
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2) = 0.3659 for 4621 reflections with I > 2σ(I)
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