
Crystal Growth and Design p. 2035 - 2038 (2011)
Update date:2022-08-04
Topics:
Lue, Jian
Han, Li-Wei
Lin, Jing-Xiang
Cao, Rong
Reactions of two halogenated derivatives of bis(4-hydroxyphenyl)sulphone (BPS, 1), tetrabromobisphenol-S (TBBPS, 2), and tetrachlorobisphenol-S (TCBPS, 3), with piperazine (PZ, 4), were investigated by means of the combinational usage of solvothermal and mechanochemical methods. The resultant organic complexes, [(C6H2OBr2)2SO 2]?[(C4H10N2) 2CH2] (5), [(C6H2OBr 2)2SO2]2?(C4H 12N2)2?3(CH3OH) (6), [(C 6H2OCl2)2SO2] ?[(C4H10N2)2CH2] (7), and [(C6H2OCl2)2SO 2]2?(C4H12N2) 2?3(CH3OH) (8), were fully characterized by single crystal and powder X-ray diffractions. In the cases of complexes 5 and 7 that were prepared from solvothermal conditions, a rare metal-free in situ ligand formation has been observed, in which the new organic molecule 1,2-bispiperazinylmethane was presumably originated from the double C-N coupling of two piperazines on a carbon atom coming from methanol. In addition, the relevant concomitants 6 and 8 were also isolated from the solutions of 5 and 7, respectively. Complexes 6 and 8 contain 1:1 starting molecules of 2/3 with 4 assembled into helical structures.
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