A Comprehensive Treatise Inorganic and Theoretical Chemistry by Mellor J.W.

By Mellor J.W.

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Route II has been regarded as the most promising procedure since modern methods for the synthesis of the initial glyoximate clathrochelates with yields of 70 to 80% are 30 developed. However, attempts to implement a complete halogenation of dioximate fragments of such complexes and to isolate hexahalogenide precursors of triribbed-functionalized clathrochelates has met with failure. A mixture of partial substitution products, largely containing trihalogen-substituted compounds, was obtained. In addition, in the case of a phenylboronic FeGm3(BC6H5)2 glyoximate the halogenation side reactions of the aromatic substituents at apical boron atoms were observed [65].

The nioximate dianion was also isolated as a salt with a HPy cation. , the formation of a protonated tris-complex. Although the product yield of Reaction 17 is higher, Reaction 16 is preferred because of the difficulties encountered in the isolation of nonmacrocyclic iron(II) trisdioximates. Tin-capped complexes also arise from the interaction of the Tchugaev type Fe(HD)2Am2 bis-dioximates with tin(IV) tetrachloride, and from the labile boron-capped FeD3(BOR)2 complexes with a great excess of SnCU.

However, this is not a general method; attempts to prepare the FeDm3(BC6H5)(BF) complex by an analogous scheme have not been 25 R HO—N-fe-"N-OH HO-N. + Y HO-W-Fe^-'N. ^'N—OH R R HO-N. J—0+ / ri^ 0 - N ; R \ ^ N - 0 R P-N R R I—Q ((C2H5)30')(C6H5BF3-) R Scheme 10 R 26 R R R R 4-O-ISN_-JN--OH HO—N-;Fe^-'N-OH HO-N^ ^'N—OH R 4-0—N"Fe^"N-OH ^ O - N ^ N - O H R R 1 ho—N"Fe •••'N-a\. N—O M R 2 R /' Ah-O-N, A R R R R ^ R / -0-N-Fe^-'N-a\. -O-N^N^O Y,Z = Lewis acids /' \ / / \ 0 - N ^ N - O R R R R S c h e m e 11 successful (only a symmetric FeDm3(BF)2 complex h a s been formed) [64].

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