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The vagaries of recrystallisation are highlighted in this contribution which describes the full characterisation of crystals isolated from the recrystallisation of [Cu 2 L 4 (EtOH) 2 ] from a 1 : 2 mixture of DMSO and CHCl 3  (v/v); L is 4-nitrobenzoate. Slow evaporation over four weeks yielded blue-green crystals of  1  that were shown to be a rare example of a three-component co-crystal comprising [CuL 2 (OH 2 )(DMSO)] 2 , [CuL 2 (OH 2 ) 2 (DMSO)] and [CuL 2 (OH 2 )(DMSO) 2 ] in the ratio 1 : 2 : 2. After crystals of  1  were removed from the solution, blue crystals of  2  were isolated after another week had elapsed. These proved to be [CuL 2 (OH 2 )(DMSO) 2 ] and to be the  trans -DMSO isomer of one of the components of  1 . The supramolecular aggregation in each crystal structure features ten-membered {…HOH…OCOCuOCO} synthons whereby the hydrogen atoms of a water molecule link two carbonyl-O atoms of another complex molecule. In  1 , these synthons lead to an isolated six-copper aggregate, and in  2 , these lead to supramolecular chains. IR and thermal analysis (TGA and DSC) data are also presented. Crystal data for ( 1 ): triclinic,  P -1,  a  = 13.9035(4),  b  = 15.5305(4),  c  = 15.7069(4) Å,  α  = 80.062(2),  β  = 83.174(2),  γ  = 70.109(2)°,  V  = 3134.75(15)Å 3 ,  Z  = 2,  R  = 0.036. Crystal data for ( 2 ): monoclinic,  C 2/  c,  a  = 30.0180(16),  b  = 5.8440(3),  c  = 14.2639(8) Å,  β  = 114.669(7)°,  V  = 2273.9(2) Å 3 ,  Z  = 4,  R  = 0.027.

A three-component co-crystal and a mono crystal isolated from the same crystallisation of a copper(II) carboxylate