63018 20201113085627.0 doi 10.1107/S2053229617010841 sideral 101639 ART-2017-101639 eng (orcid)0000-0002-9687-4903 Castro, Miguel Universidad de Zaragoza A phase transition caught in mid-course: Independent and concomitant analyses of the monoclinic and triclinic structures of (nBu4N)[Co(orotate)2(bipy)]·3H2O 2017 Access copy available to the general public Unrestricted The preparation and characterization of the nBu4N+ salts of two bis-orotate(2-) complexes of cobalt, namely bis(tetra-n-butylammonium) diaquabis(2, 4-dioxo-1, 2, 3, 4-Tetrahydropyrimidin-1-ide-6-carboxylato-¿2N1, O6)cobalt(II) 1.8-hydrate, (C16H36N)2[Co(C5H2N2O4)2(H2O)2]·1.8H2O, (1), and tetra-n-butylammonium (2, 2'-bipyridine-¿2N, N')bis(2, 4-dioxo-1, 2, 3, 4-Tetrahydropyrimidin-1-ide-6-carboxylato-¿2N1, O6)cobalt(III) trihydrate, (C16H36N)[Co(C5H2N2O4)2(C10H8N2)]·3H2O, (2), are reported. The CoIII complex, (2), which is monoclinic at room temperature, presents a conservative single-crystal-To-single-crystal phase transition below 200bK, producing a triclinic twin. The transition, which involves a conformational change in one of the nBu groups of the cation, is reversible and can be cycled. Both end phases have been characterized structurally and the system was also characterized structurally in a two-phase intermediate state, using single-crystal diffraction techniques, with both the monoclinic and triclinic phases present. Thermal analysis allows a rough estimate of the small energy content, viz. 0.25bkJbmol-1, for both the monoclinic-To-Triclinic transformation and the reverse transition, in agreement with the nature of the structural changes involving only the nBu4N+ cation.Repeated cycling through a reversible order-disorder phase transition in a crystal of a cobalt orotate complex produces an arrested transformation, leaving the sample with both triclinic and monoclinic domains. Independent determinations of the two structures were carried out from single-phase samples and the partial transition permitted simultaneous structure determination of the two phases at a temperature at which one of them is not expected to exist independently. info:eu-repo/grantAgreement/ES/DGA/E16 info:eu-repo/grantAgreement/ES/MINECO/MAT2015-68200-C2-1-P info:eu-repo/semantics/openAccess by http://creativecommons.org/licenses/by/3.0/es/ 8.678 2017 CHEMISTRY, MULTIDISCIPLINARY 20 / 171 = 0.117 2017 Q1 T1 CRYSTALLOGRAPHY 1 / 26 = 0.038 2017 Q1 T1 0.834 2017 Condensed Matter Physics 2017 Q1 Inorganic Chemistry 2017 Q1 Materials Chemistry 2017 Q1 Medicine (miscellaneous) 2017 Q2 Physical and Theoretical Chemistry 2017 Q2 info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion (orcid)0000-0002-0444-996X Falvello, Larry R. Universidad de Zaragoza (orcid)0000-0001-8461-6846 Forcén-Vázquez, Elena Guerra, Pablo Al-Kenany, Nuha A. (orcid)0000-0001-7872-6301 Martínez, Gema Universidad de Zaragoza Tomás, Milagros 2010 760 Universidad de Zaragoza Dpto. Química Inorgánica Área Química Inorgánica 5005 555 Universidad de Zaragoza Dpto. Ing.Quím.Tecnol.Med.Amb. Área Ingeniería Química 5001 065 Universidad de Zaragoza Dpto. Ciencia Tecnol.Mater.Fl. Área Cienc.Mater. Ingen.Metal. 73, 9 (2017), 731-742 Acta crystallogr., C Struct. chem. Acta Crystallographica Section C-Structural Chemistry 2053-2296 2198018 http://zaguan.unizar.es/record/63018/files/texto_completo.pdf Versión publicada 86695 http://zaguan.unizar.es/record/63018/files/texto_completo.jpg?subformat=icon icon Versión publicada oai:zaguan.unizar.es:63018 articulos driver 2020-11-13-08:46:42 ARTICLE