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An improved synthesis using microwave heating affords (C 6 H 4 PO(OCH 3 ) 2 ) 2  in excellent isolated yield (95 %). The ligand properties of this bisphosphonateester were explored towards hard metal centers  M  2+  ( M  = Ca, UO 2 ) and  M  3+  ( M  = La, Ce, Sm, Eu) resulting in coordination polymers, for which the reduction of ionic size of the central metal atom resulted in lower‐dimensional structural motifs as opposed to higher dimensional networks obtained for the larger ions. All coordination polymers were characterized by single‐crystal X‐ray diffraction, IR spectroscopy, and combustion analysis. The ligand was furthermore characterized with multinuclear NMR spectroscopy.

Coordination Polymers based on the Neutral Ditopic Ligand (C 6 H 4 PO(OCH 3 ) 2 ) 2 Involving some f‐Block Elements