AbstractThe coordination number of the gadolinium atom and bond distances in the crystal of monomeric porphyrinate, [Gd(TPP)acac·8H2O·3TCB] (TCB: 1,2,4‐trichlorobenzene, acac: anion of acetylacetone), were determined by EXAFS method. The Gd atom is eight‐coordinated to the four nitrogen atoms of a tetraphenylporphyrin ring, to the two oxygen atoms of one acetylacetonato anion and to two water molecules with Gd—N=0.232 nm, Gd—O=0.243 nm.