By Mellor J.W.
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Additional info for A Comprehensive Treatise Inorganic and Theoretical Chemistry
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 .
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) .