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

作者：Abdullah Norbani^*; Mohamadin Mohammad Isa; Seik Weng Ng; Tiekink Edward R T

来源：Zeitschrift fur Kristallographie-Crystalline Materials, 2012, 227(2): 122-128.

DOI：10.1524/zkri.2012.1439

• Carboxylate
• Co-crystal
• Recrystallisation
• Crystal structure analysis
• X-ray diffraction

The vagaries of recrystallisation are highlighted in this contribution which describes the full characterisation of crystals isolated from the recrystallisation of [Cu2L4(EtOH)(2)] from a 1 : 2 mixture of DMSO and CHCl3 (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 [CuL2(OH2)(DMSO)](2), [CuL2(OH2)(2)(DMSO)] and [CuL2(OH2)(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 [CuL2(OH2)(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 {center dot center dot center dot HOH center dot center dot center dot OCOCuOCO} synthons whereby the hydrogen atoms of a water molecule link two carbonyl-0 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) over bar, a = 13.9035(4), b = 15.5305(4), c = 15.7069(4) angstrom, alpha = 80.062(2), beta = 83.174(2), gamma = 70.109(2)degrees, V = 3134.75(15)angstrom(3), Z = 2, R = 0.036. Crystal data for (2): monoclinic, C2/c, a = 30.0180(16), b = 5.8440(3), c = 14.2639(8) angstrom, beta = 114.669(7)degrees, V = 2273.9(2) angstrom(3), Z = 4, R = 0.027.

• 出版日期2012