Structure and NMR Spectroscopy in Solid State and Solution of {Na 2 [μ 2 ‐(C 6 H 4 O 2 ) 2 ](C 6 H 4 OOH) 2 } 4−

The new compound (NH 3 CH 2 CH 2 NH 3 ) 2 {Na 2 [μ 2 ‐(C 6 H 4 O 2 ) 2 ](C 6 H 4 OOH) 2 } has been synthesized and characterized by elemental analysis, IR, UV, NMR and single crystal X‐ray diffraction. The yellow crystals crystallized in the triclinic system with space group P ‐1 and a =0.6091(2) nm, b =1.0274(3) nm, c =1.2466(4) nm, α =89.073(6)°, β =89.376(6)°, γ =78.873(5)°, V =0.7653(4) nm 3 , Z =1, R 1 =0.0568, wR 2 =0.1198. Every sodium ion coordinates in trigonal prismatic fashion with two O atoms from a terminal chelating catecholato ligand and four O atoms from bridging µ 2 catecholato ligands. Two neighboring NaO 6 trigonal prisms are face‐shared and centrosymmetric with regard to the inversion center consisting of four tri‐bridging O atoms to form a binuclear cluster {Na 2 [μ 2 ‐(C 6 H 4 O 2 ) 2 ]} 2− anion. The comparison of 13 C NMR spectrum of the complex in solid state with that in solution indicated that the rapid exchange between the bridging [μ 2 ‐(C 6 H 4 O 2 )] 2− and terminal [C 6 H 4 OOH] − ligands was present in solution.