X-ray structure and investigation of molecular motions by dielectric, vibrational and 1H NMR methods for two organic-inorganic hybrid piperazinium compounds: (C4H12N2)2[Sb2Cl10]·2H2O and (C4H12N2)2[Sb2Br10]·2H2O

• Published in: Materials research bulletin Vol. 104; pp. 202 - 211
• Main Authors: Moskwa, Marcin, Bator, Grażyna, Piecha-Bisiorek, Anna, Jakubas, Ryszard, Medycki, Wojciech, Ciżman, Agnieszka, Baran, Jan
• Format: Journal Article
• Language: English
• Published: United States Elsevier Ltd 01.08.2018
• Subjects: 1H NMR; CATIONS; CHLORIDES; CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; Dielectric; DIELECTRIC MATERIALS; HYDRATES; HYDROGEN 1; MONOCLINIC LATTICES; MONOCRYSTALS; NUCLEAR MAGNETIC RESONANCE; PHASE TRANSFORMATIONS; Phase transition; Piperazine-1,4-diium; PIPERAZINES; STOICHIOMETRY; SYMMETRY; WATER; X-RAY DIFFRACTION; 1H NMR; IR; Piperazine-1,4-diium; Dielectric; Phase transition
• ISSN: 0025-5408; 1873-4227
• DOI: 10.1016/j.materresbull.2018.03.048

[Display omitted] •Bis(piperazine-1,4-diium) decabromodiantimonate(III) (PSB) dihydrate has been synthesized and characterized.•The structural phase transition for PSB at ca. 50 K has been confirmed by the dielectric and 1H NMR spectroscopy results.•The molecular motion parameters of the organic cations and water molecules have been evaluated and compared for PSB and PSC. Bis(piperazine-1,4-diium) decabromodiantimonate(III) dihydrate, (C4H12N2)2[Sb2Br10]·2H2O, (abbreviated as PSB) has been synthesized and characterized by single-crystal X-ray diffraction studies. The obtained results indicate that PSB is isostructural with a recently described chloride analogue, (C4H12N2)2[Sb2Cl10]⋅2H2O (PSC), crystallizing with R2MX5·nH2O stoichiometry and characterized by the discrete zero-dimensional anionic species. The crystal structure of PSB is described by monoclinic symmetry in a P21/n space group. Dielectric measurements (down to 25 K) and IR spectral analyses (measured over a broad temperature range) suggested a much more complicated phase situation below 80 K than for that of PSC. To verify and compare the molecular motions of the organic cations in both analogues, a proton magnetic resonance (1H NMR) technique was also applied.