Solution and solid-state preparation of 18-crown-6 and 15-crown-5 adducts of hydrogen sulfate salts and an investigation of the reversible dehydration processes

Dario Braga; Massimo Gandolfi; Matteo Lusi; Marco Polito; Katia Rubini; Fabrizia Grepioni

doi:10.1021/cg0607598

Solution and solid-state preparation of 18-crown-6 and 15-crown-5 adducts of hydrogen sulfate salts and an investigation of the reversible dehydration processes

Dario Braga
, Massimo Gandolfi
, Matteo Lusi
, Marco Polito
, Katia Rubini
, Fabrizia Grepioni

University of Bologna

Research output: Contribution to journal › Article › peer-review

Abstract

A new class of organic-inorganic complexes has been prepared by reaction in solution or by mechanical mixing of 15-Crown-5 or 18-Crown-6 ethers with MSO₄ (M = Mn²⁺, Cd²⁺, Pb^2-) and/or H₂SO₄ in stoichiometric amount. The complexes (15-Crown-5)[Mn(H₂O)₂(HSO₄)₂] (1), (15-Crown-5)[Cd(H₂O)₂(HSO₄)₂] (2), (15-Crown-5)[H₇O₃(HSO₄)₂· H₂O (3), (18-Crown-6)[Pb(HSO₄)₂] (4), and (18-Crown-6)[(H₅O₂)(HSO₄)] (5) have been characterized by single-crystal X-ray diffraction. Compounds 1 and 2 undergo reversible water release-uptake processes, accompanied by a change in coordination at the metal centers; the dehydration and phase-transition processes have been investigated by DSC, TGA, and variable-temperature X-ray powder diffraction.

Original language	English
Pages (from-to)	919-924
Number of pages	6
Journal	Crystal Growth and Design
Volume	7
Issue number	5
DOIs	https://doi.org/10.1021/cg0607598
Publication status	Published - May 2007
Externally published	Yes

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title = "Solution and solid-state preparation of 18-crown-6 and 15-crown-5 adducts of hydrogen sulfate salts and an investigation of the reversible dehydration processes",

abstract = "A new class of organic-inorganic complexes has been prepared by reaction in solution or by mechanical mixing of 15-Crown-5 or 18-Crown-6 ethers with MSO4 (M = Mn2+, Cd2+, Pb2-) and/or H2SO4 in stoichiometric amount. The complexes (15-Crown-5)[Mn(H2O)2(HSO4)2] (1), (15-Crown-5)[Cd(H2O)2(HSO4)2] (2), (15-Crown-5)[H7O3(HSO4)2· H2O (3), (18-Crown-6)[Pb(HSO4)2] (4), and (18-Crown-6)[(H5O2)(HSO4)] (5) have been characterized by single-crystal X-ray diffraction. Compounds 1 and 2 undergo reversible water release-uptake processes, accompanied by a change in coordination at the metal centers; the dehydration and phase-transition processes have been investigated by DSC, TGA, and variable-temperature X-ray powder diffraction.",

author = "Dario Braga and Massimo Gandolfi and Matteo Lusi and Marco Polito and Katia Rubini and Fabrizia Grepioni",

year = "2007",

month = may,

doi = "10.1021/cg0607598",

language = "English",

volume = "7",

pages = "919--924",

journal = "Crystal Growth and Design",

issn = "1528-7483",

number = "5",

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TY - JOUR

T1 - Solution and solid-state preparation of 18-crown-6 and 15-crown-5 adducts of hydrogen sulfate salts and an investigation of the reversible dehydration processes

AU - Braga, Dario

AU - Gandolfi, Massimo

AU - Lusi, Matteo

AU - Polito, Marco

AU - Rubini, Katia

AU - Grepioni, Fabrizia

PY - 2007/5

Y1 - 2007/5

N2 - A new class of organic-inorganic complexes has been prepared by reaction in solution or by mechanical mixing of 15-Crown-5 or 18-Crown-6 ethers with MSO4 (M = Mn2+, Cd2+, Pb2-) and/or H2SO4 in stoichiometric amount. The complexes (15-Crown-5)[Mn(H2O)2(HSO4)2] (1), (15-Crown-5)[Cd(H2O)2(HSO4)2] (2), (15-Crown-5)[H7O3(HSO4)2· H2O (3), (18-Crown-6)[Pb(HSO4)2] (4), and (18-Crown-6)[(H5O2)(HSO4)] (5) have been characterized by single-crystal X-ray diffraction. Compounds 1 and 2 undergo reversible water release-uptake processes, accompanied by a change in coordination at the metal centers; the dehydration and phase-transition processes have been investigated by DSC, TGA, and variable-temperature X-ray powder diffraction.

AB - A new class of organic-inorganic complexes has been prepared by reaction in solution or by mechanical mixing of 15-Crown-5 or 18-Crown-6 ethers with MSO4 (M = Mn2+, Cd2+, Pb2-) and/or H2SO4 in stoichiometric amount. The complexes (15-Crown-5)[Mn(H2O)2(HSO4)2] (1), (15-Crown-5)[Cd(H2O)2(HSO4)2] (2), (15-Crown-5)[H7O3(HSO4)2· H2O (3), (18-Crown-6)[Pb(HSO4)2] (4), and (18-Crown-6)[(H5O2)(HSO4)] (5) have been characterized by single-crystal X-ray diffraction. Compounds 1 and 2 undergo reversible water release-uptake processes, accompanied by a change in coordination at the metal centers; the dehydration and phase-transition processes have been investigated by DSC, TGA, and variable-temperature X-ray powder diffraction.

UR - https://www.scopus.com/pages/publications/34249106671

U2 - 10.1021/cg0607598

DO - 10.1021/cg0607598

M3 - Article

AN - SCOPUS:34249106671

SN - 1528-7483

VL - 7

SP - 919

EP - 924

JO - Crystal Growth and Design

JF - Crystal Growth and Design

IS - 5

ER -

Solution and solid-state preparation of 18-crown-6 and 15-crown-5 adducts of hydrogen sulfate salts and an investigation of the reversible dehydration processes

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