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The synthesis, structure, magnetic, and photophysical properties of two dinuclear, luminescent, mixed‐ligand [Cr III  2 L(O 2 CR)] 3+  complexes (R=CH 3  ( 1 ), Ph ( 2 )) of a 24‐membered binucleating hexa‐aza‐dithiophenolate macrocycle (L) 2−  are presented. X‐ray crystallographic analysis reveals an edge‐sharing bioctahedral N 3 Cr( μ ‐SR) 2 ( μ  1,3 ‐O 2 CR)CrN 3  core structure with  μ  1,3 ‐bridging carboxylate groups. A ferromagnetic superexchange interaction between the electron spins of the Cr 3+  ions leads to a high‐spin ( S =3) ground state. The coupling constants ( J =+24.2(1) cm −1  ( 1 ), +34.8(4) cm −1  ( 2 ), H=−2 J S 1 S 2 ) are significantly larger than in related  bis ‐ μ ‐alkoxido‐ μ ‐carboxylato structures. DFT calculations performed on both complexes reproduce both the sign and strength of the exchange interactions found experimentally. Frozen methanol‐dichloromethane 1 : 1 solutions of  1  and  2  luminesce at 750 nm when excited into the  4 LMCT state on the  4 A 2  →  2 T 1  (ν 2 ) bands (λ exc =405 nm). The absolute quantum yields ( Φ  L ) for  1  and  2  were found to be strongly temperature dependent. At 77 K in frozen MeOH/CH 2 Cl 2  glasses,  Φ  L =0.44±0.02  (for  1 ),  Φ  L =0.45±0.02  (for  2 ).

chemistry – a european journal

Synthesis and Characterisation of Luminescent [Cr III  2 L( μ ‐carboxylato)] 3+  Complexes with High‐Spin  S =3 Ground States (L=N 6 S 2  donor ligand)