Two‐step Hydrothermal Syntheses and Structures of Three Tantalum Oxyfluoride Compounds with [ M (phen) 3 ] 2+ ( M = Ru, Fe) Counter Ions

Three tantalum oxyfluoride compounds, [Fe(phen) 3 ][Ta 2 OF 10 ] ( 1 ), [Fe(phen) 3 ][Ta 2 OF 10 ] · 2H 2 O ( 2 ), and [Ru(phen) 3 ] 2 [Ta 2 OF 10 ][TaF 6 ] 2 ( 3 ), were synthesized by a two‐step hydrothermal method and their crystal structures were characterized by single‐crystal X‐ray diffraction. The unique characters of these compounds are the [ M (phen) 3 ] 2+ cations. C–H ··· F interactions exist between cations and anions and O–H ··· F hydrogen bonds exist between the water molecules and anions. Photocurrent measurements reveal that compound 3 is the photoelectric responsive with the moderate current intensity.