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High‐pressure studies of three polymorphs of a palladium(II) oxathioether macrocyclic complex
Author(s) -
Tidey Jeremiah P.,
Wong Henry L. S.,
McMaster Jonathan,
Schröder Martin,
Blake Alexander J.
Publication year - 2016
Publication title -
acta crystallographica section b
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.604
H-Index - 33
ISSN - 2052-5206
DOI - 10.1107/s2052520616007435
Subject(s) - palladium , crystallography , chemistry , crystal structure , diffraction , phase transition , phase (matter) , x ray crystallography , stereochemistry , thermodynamics , organic chemistry , catalysis , physics , optics
The three reported phases of the mononuclear macrocyclic Pd II complex [PdCl 2 ([9]aneS 2 O)] [(1); [9]aneS 2 O = 1‐oxa‐4,7‐dithiacyclononane] were each studied up to pressures exceeding 9 GPa using high‐pressure single‐crystal X‐ray diffraction. The α‐ and γ‐phases both exhibit smooth compression of the unit‐cell parameters with third‐order Birch–Murnaghan bulk moduli of 14.4 (8) and 7.6 (6) GPa, respectively. Between 6.81 and 6.87 GPa β‐[PdCl 2 ([9]aneS 2 O)] was found to undergo a reversible transition to a phase denoted as β′ and characterized by a tripling of the unit‐cell volume. Across the phase transition, rearrangement of the conformation of the bound macrocycle at two of the resulting three unique sites gives rise to an extensively disordered structure.