Pressure Induced Phase Transitions and Metallization of a Neutral Radical Conductor

The crystal structure and charge transport properties of the prototypal oxobenzene-bridged 1,2,3-bisdithiazolyl radical conductor 3a are strongly dependent on pressure. Compression of the as-crystallized α-phase, space group Fdd2, to 3–4 GPa leads to its conversion into a second or β-phase, in which...

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Published inJournal of the American Chemical Society Vol. 136; no. 3; pp. 1070 - 1081
Main Authors Wong, Joanne W. L, Mailman, Aaron, Lekin, Kristina, Winter, Stephen M, Yong, Wenjun, Zhao, Jianbao, Garimella, Subrahmanyam V, Tse, John S, Secco, Richard A, Desgreniers, Serge, Ohishi, Yasuo, Borondics, Ferenc, Oakley, Richard T
Format Journal Article
LanguageEnglish
Published United States American Chemical Society 22.01.2014
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Abstract The crystal structure and charge transport properties of the prototypal oxobenzene-bridged 1,2,3-bisdithiazolyl radical conductor 3a are strongly dependent on pressure. Compression of the as-crystallized α-phase, space group Fdd2, to 3–4 GPa leads to its conversion into a second or β-phase, in which F-centering is lost. The space group symmetry is lowered to Pbn21, and there is concomitant halving of the a and b axes. A third or γ-phase, also space group Pbn21, is generated by further compression to 8 GPa. The changes in packing that accompany both phase transitions are associated with an “ironing out” of the ruffled ribbon-like architecture of the α-phase, so that consecutive radicals along the ribbons are rendered more nearly coplanar. In the β-phase the planar ribbons are propagated along the b-glides, while in the γ-phase they follow the n-glides. At ambient pressure 3a is a Mott insulator, displaying high but activated conductivity, with σ(300 K) = 6 × 10–3 S cm–1 and E act = 0.16 eV. With compression beyond 4 GPa, its conductivity is increased by 3 orders of magnitude, and the thermal activation energy is reduced to zero, heralding the formation of a metallic state. High pressure infrared absorption and reflectivity measurements are consistent with closure of the Mott–Hubbard gap near 4–5 GPa. The results are discussed in the light of DFT calculations on the molecular and band electronic structure of 3a. The presence of a low-lying LUMO in 3a gives rise to high electron affinity which, in turn, creates an electronically much softer radical with a low onsite Coulomb potential U. In addition, considerable crystal orbital (SOMO/LUMO) mixing occurs upon pressurization, so that a metallic state is readily achieved at relatively low applied pressure.
AbstractList The crystal structure and charge transport properties of the prototypal oxobenzene-bridged 1,2,3-bisdithiazolyl radical conductor 3a are strongly dependent on pressure. Compression of the as-crystallized α-phase, space group Fdd2, to 3–4 GPa leads to its conversion into a second or β-phase, in which F-centering is lost. The space group symmetry is lowered to Pbn21, and there is concomitant halving of the a and b axes. A third or γ-phase, also space group Pbn21, is generated by further compression to 8 GPa. The changes in packing that accompany both phase transitions are associated with an “ironing out” of the ruffled ribbon-like architecture of the α-phase, so that consecutive radicals along the ribbons are rendered more nearly coplanar. In the β-phase the planar ribbons are propagated along the b-glides, while in the γ-phase they follow the n-glides. At ambient pressure 3a is a Mott insulator, displaying high but activated conductivity, with σ(300 K) = 6 × 10–3 S cm–1 and E act = 0.16 eV. With compression beyond 4 GPa, its conductivity is increased by 3 orders of magnitude, and the thermal activation energy is reduced to zero, heralding the formation of a metallic state. High pressure infrared absorption and reflectivity measurements are consistent with closure of the Mott–Hubbard gap near 4–5 GPa. The results are discussed in the light of DFT calculations on the molecular and band electronic structure of 3a. The presence of a low-lying LUMO in 3a gives rise to high electron affinity which, in turn, creates an electronically much softer radical with a low onsite Coulomb potential U. In addition, considerable crystal orbital (SOMO/LUMO) mixing occurs upon pressurization, so that a metallic state is readily achieved at relatively low applied pressure.
The crystal structure and charge transport properties of the prototypal oxobenzene-bridged 1,2,3-bisdithiazolyl radical conductor 3a are strongly dependent on pressure. Compression of the as-crystallized α-phase, space group Fdd2, to 3-4 GPa leads to its conversion into a second or β-phase, in which F-centering is lost. The space group symmetry is lowered to Pbn2₁, and there is concomitant halving of the a and b axes. A third or γ-phase, also space group Pbn2₁, is generated by further compression to 8 GPa. The changes in packing that accompany both phase transitions are associated with an "ironing out" of the ruffled ribbon-like architecture of the α-phase, so that consecutive radicals along the ribbons are rendered more nearly coplanar. In the β-phase the planar ribbons are propagated along the b-glides, while in the γ-phase they follow the n-glides. At ambient pressure 3a is a Mott insulator, displaying high but activated conductivity, with σ(300 K) = 6 × 10(-3) S cm(-1) and E(act) = 0.16 eV. With compression beyond 4 GPa, its conductivity is increased by 3 orders of magnitude, and the thermal activation energy is reduced to zero, heralding the formation of a metallic state. High pressure infrared absorption and reflectivity measurements are consistent with closure of the Mott-Hubbard gap near 4-5 GPa. The results are discussed in the light of DFT calculations on the molecular and band electronic structure of 3a. The presence of a low-lying LUMO in 3a gives rise to high electron affinity which, in turn, creates an electronically much softer radical with a low onsite Coulomb potential U. In addition, considerable crystal orbital (SOMO/LUMO) mixing occurs upon pressurization, so that a metallic state is readily achieved at relatively low applied pressure.
Author Oakley, Richard T
Ohishi, Yasuo
Secco, Richard A
Lekin, Kristina
Mailman, Aaron
Winter, Stephen M
Tse, John S
Yong, Wenjun
Desgreniers, Serge
Borondics, Ferenc
Wong, Joanne W. L
Garimella, Subrahmanyam V
Zhao, Jianbao
AuthorAffiliation Department of Chemistry
University of Western Ontario
Department of Physics and Engineering Physics
University of Waterloo
Japan Synchrotron Radiation Research Institute (JASRI)
Materials Science Division
Department of Earth Sciences
University of Saskatchewan
University of Ottawa
Department of Physics
AuthorAffiliation_xml – name: Materials Science Division
– name: Department of Chemistry
– name: University of Ottawa
– name: Department of Earth Sciences
– name: Department of Physics
– name: Department of Physics and Engineering Physics
– name: University of Western Ontario
– name: University of Saskatchewan
– name: University of Waterloo
– name: Japan Synchrotron Radiation Research Institute (JASRI)
Author_xml – sequence: 1
  givenname: Joanne W. L
  surname: Wong
  fullname: Wong, Joanne W. L
– sequence: 2
  givenname: Aaron
  surname: Mailman
  fullname: Mailman, Aaron
– sequence: 3
  givenname: Kristina
  surname: Lekin
  fullname: Lekin, Kristina
– sequence: 4
  givenname: Stephen M
  surname: Winter
  fullname: Winter, Stephen M
– sequence: 5
  givenname: Wenjun
  surname: Yong
  fullname: Yong, Wenjun
– sequence: 6
  givenname: Jianbao
  surname: Zhao
  fullname: Zhao, Jianbao
– sequence: 7
  givenname: Subrahmanyam V
  surname: Garimella
  fullname: Garimella, Subrahmanyam V
– sequence: 8
  givenname: John S
  surname: Tse
  fullname: Tse, John S
– sequence: 9
  givenname: Richard A
  surname: Secco
  fullname: Secco, Richard A
– sequence: 10
  givenname: Serge
  surname: Desgreniers
  fullname: Desgreniers, Serge
– sequence: 11
  givenname: Yasuo
  surname: Ohishi
  fullname: Ohishi, Yasuo
– sequence: 12
  givenname: Ferenc
  surname: Borondics
  fullname: Borondics, Ferenc
– sequence: 13
  givenname: Richard T
  surname: Oakley
  fullname: Oakley, Richard T
  email: oakley@uwaterloo.ca
BackLink https://www.ncbi.nlm.nih.gov/pubmed/24400662$$D View this record in MEDLINE/PubMed
https://www.osti.gov/biblio/1162812$$D View this record in Osti.gov
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Snippet The crystal structure and charge transport properties of the prototypal oxobenzene-bridged 1,2,3-bisdithiazolyl radical conductor 3a are strongly dependent on...
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Title Pressure Induced Phase Transitions and Metallization of a Neutral Radical Conductor
URI http://dx.doi.org/10.1021/ja411057x
https://www.ncbi.nlm.nih.gov/pubmed/24400662
https://search.proquest.com/docview/1492679076
https://www.osti.gov/biblio/1162812
Volume 136
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