Observation of a re-entrant phase transition in the molecular complex tris(μ2-3,5-diisopropyl-1,2,4-triazolato-κ2N1:N2)trigold(I) under high pressure

Woodall, Christopher H.; Christensen, Jeppe; Skelton, Jonathan M.; Hatcher, Lauren E.; Parlett, Andrew; Raithby, Paul R.; Walsh, Aron; Parker, Stephen C.; Beavers, Christine M.; Teat, Simon J.; Intissar, Mourad; Reber, Christian; Allan, David R.

doi:10.1107/S2052252516013129

Title: Observation of a re-entrant phase transition in the molecular complex tris(μ₂-3,5-diisopropyl-1,2,4-triazolato-κ²N¹:N²)trigold(I) under high pressure

Journal Article · Thu Aug 18 00:00:00 EDT 2016 · IUCrJ

DOI:https://doi.org/10.1107/S2052252516013129· OSTI ID:1378975

Woodall, Christopher H. ^[1]; Christensen, Jeppe ^[2]; Skelton, Jonathan M. ^[1]; Hatcher, Lauren E. ^[1]; Parlett, Andrew ^[1]; Raithby, Paul R. ^[3]; Walsh, Aron ^[1]; Parker, Stephen C. ^[1]; Beavers, Christine M. ^[4]; Teat, Simon J. ^[4]; Intissar, Mourad ^[5]; Reber, Christian ^[5]; Allan, David R. ^[6]

Univ. of Bath, Bath (United Kingdom)
Harwell Oxford, Oxfordshire (United Kingdom)
Univ. of Bath, Bath (United Kingdom); Harwell Oxford, Oxfordshire (United Kingdom)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Univ. de Montreal, Montreal, QC (Canada)
Diamond Light Source, Oxfordshire (United Kingdom)

We report a molecular crystal that exhibits four successive phase transitions under hydrostatic pressure, driven by aurophilic interactions, with the ground-state structure re-emerging at high pressure. The effect of pressure on two polytypes of tris(μ₂-3,5-diisopropyl-1,2,4-triazolato-κ²N¹:N²)trigold(I) (denoted Form-I and Form-II) has been analysed using luminescence spectroscopy, single-crystal X-ray diffraction and first-principles computation. A unique phase behaviour was observed in Form-I, with a complex sequence of phase transitions between 1 and 3.5 GPa. The ambient C2/c mother cell transforms to a P2₁/n phase above 1 GPa, followed by a P2₁/a phase above 2 GPa and a large-volume C2/c supercell at 2.70 GPa, with the previously observed P2₁/n phase then reappearing at higher pressure. The observation of crystallographically identical low- and high-pressure P2₁/n phases makes this a rare example of a re-entrant phase transformation. The phase behaviour has been characterized using detailed crystallographic theory and modelling, and rationalized in terms of molecular structural distortions. The dramatic changes in conformation are correlated with shifts of the luminescence maxima, from a band maximum at 14040 cm^–1 at 2.40 GPa, decreasing steeply to 13550 cm^–1 at 3 GPa. A similar study of Form-II displays more conventional crystallographic behaviour, indicating that the complex behaviour observed in Form-I is likely to be a direct consequence of the differences in crystal packing between the two polytypes.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1378975

Journal Information:: IUCrJ, Vol. 3, Issue 5; ISSN 2052-2525

Publisher:: International Union of CrystallographyCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 8 works

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
re-entrant phase transitions
high-pressure crystallography
gold(I)
luminescence spectroscopy
DFT calculations

CCDC 1405868: Experimental Crystal Structure Determination: HEMTID02 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xl6 The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405869: Experimental Crystal Structure Determination: HEMTID03 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xm7 The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405870: Experimental Crystal Structure Determination: HEMTID04 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xn8 The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405871: Experimental Crystal Structure Determination: HEMTID05 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xp9 The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405872: Experimental Crystal Structure Determination: HEMTID06 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xqb The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405873: Experimental Crystal Structure Determination: HEMTID07 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xrc The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405874: Experimental Crystal Structure Determination: HEMTID18 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xsd The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405875: Experimental Crystal Structure Determination: HEMTID08 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xtf The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405876: Experimental Crystal Structure Determination: HEMTID09 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xvg The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405877: Experimental Crystal Structure Determination: HEMTID10 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xwh The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405878: Experimental Crystal Structure Determination: HEMTID11 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5xxj The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405879: Experimental Crystal Structure Determination: HEMTID12 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xyk The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405880: Experimental Crystal Structure Determination: HEMTID13 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5xzl The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405881: Experimental Crystal Structure Determination: HEMTID14 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C.; Christensen, J.; Skelton, J. https://doi.org/10.5517/ccdc.csd.cc1j5y0n The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405882: Experimental Crystal Structure Determination: HEMTID15 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5y1p The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405883: Experimental Crystal Structure Determination: HEMTID16 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5y2q The current record is supplemented by this dataset	dataset	August 2016
CCDC 1405884: Experimental Crystal Structure Determination: HEMTID17 : tris(μ-3,5-diisopropyl-1,2,4-triazolato-N,N')-tri-gold(i) Woodall, C. H.; Christensen, J.; Skelton, J. M. https://doi.org/10.5517/ccdc.csd.cc1j5y3r The current record is supplemented by this dataset	dataset	August 2016

Title: Observation of a re-entrant phase transition in the molecular complex tris(μ2-3,5-diisopropyl-1,2,4-triazolato-κ2N1:N2)trigold(I) under high pressure

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Title: Observation of a re-entrant phase transition in the molecular complex tris(μ₂-3,5-diisopropyl-1,2,4-triazolato-κ²N¹:N²)trigold(I) under high pressure