Taguchi Method for the General, Gentle, and Efficient Synthesis of Hexamethylphosphotriamide Nickel(II) Complexes with Weakly Coordinated Anions: Crystal Structure of the Tetravalent [Ni(HMPA)4][BArF24]2

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Abstract

The synthesis of novel dicationic nickel (II) complexes, designated [Ni(HMPA) 4 ][Y] 2 , was achieved by reaction of the organometallic compound [Ni(cod) 2 ] with the allylic salt (C 4 H 7 (OP(NMe 2 ) 3 /NaY), (Y = BF 4 , PF 6 , BArF 24 ). Crystal structure analysis, NMR, and infrared studies provided conclusive evidence for the identification of a homoleptic nickel (II) Oxo-phosphoryl complex. The synthetic procedure involves the oxidative addition of methallyloxyphosphonium salts with non-coordinating anions, resulting in a tetrakis(hexamethylphosphotriamide) nickel (II) complex. Using an orthogonal Taguchi design, key factors such as reaction time, temperature, and stirring rate were considered. The optimized conditions were determined.

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