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Ni-norcorrole Derivatives 3 was obtained in moderate yield by the reaction of Ni-norcorrole 1 and dimethyl acetylenedicarboxylate or diethyl acetylenedicarboxylate in toluene at 110℃ for 24 Hr.Ninorcorrole Derivatives 2 was obtained by the reaction of Ni-norcorrole 1,triphenylphosphine and dimethyl acetylenedicarboxylateor diethyl acetylenedicarboxylate at 110℃ for 40 min.