High-pressure polymorphism in pyridine

Giordano, Nico; Beavers, Christine M.; Campbell, Branton J.; Eigner, Václav; Gregoryanz, Eugene; Marshall, Willliam G.; Peña-Álvarez, Miriam; Teat, Simon J.; Vennari, Cara E.; Parsons, Simon

doi:10.1107/S2052252519015616

Title: High-pressure polymorphism in pyridine

Journal Article · 01 January 2020 · IUCrJ

DOI: https://doi.org/10.1107/S2052252519015616 · OSTI ID:1577894

Giordano, Nico ^[1]; Beavers, Christine M. ^[2]; Campbell, Branton J. ^[3]; Eigner, Václav ^[4]; Gregoryanz, Eugene ^[5];

^[6]; Peña-Álvarez, Miriam ^[5]; Teat, Simon J. ^[7]; Vennari, Cara E. ^[8]; Parsons, Simon ^[5]

Univ. of Edinburgh (United Kingdom); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Deutsches Elektonen-Synchrotron (DESY), Hamberg (Germany)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Univ. of California, Santa Cruz, CA (United States); Rutherford Appleton Lab., Didcot (United Kingdom)
Brigham Young Univ., Provo, UT (United States)
Univ. of Edinburgh (United Kingdom); Inst. of Physics of the Academy of Sciences of the Czech Republic, Prague (Czech Republic)
Univ. of Edinburgh (United Kingdom)
Rutherford Appleton Lab., Didcot (United Kingdom)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Univ. of California, Santa Cruz, CA (United States)

Single crystals of the high-pressure phases II and III of pyridine have been obtained by in situ crystallization at 1.09 and 1.69 GPa, revealing the crystal structure of phase III for the first time using X-ray diffraction. Phase II crystallizes in P2₁2₁2₁ with Z' = 1 and phase III in P4₁2₁2 with Z' = ½. Neutron powder diffraction experiments using pyridine-d₅ establish approximate equations of state of both phases. The space group and unit-cell dimensions of phase III are similar to the structures of other simple compounds with C_2v molecular symmetry, and the phase becomes stable at high pressure because it is topologically close-packed, resulting in a lower molar volume than the topologically body-centred cubic phase II. Phases II and III have been observed previously by Raman spectroscopy, but have been mis-identified or inconsistently named. Raman spectra collected on the same samples as used in the X-ray experiments establish the vibrational characteristics of both phases unambiguously. The pyridine molecules interact in both phases through CH∙∙∙π and CH∙∙∙N interactions. The nature of individual contacts is preserved through the phase transition between phases III and II, which occurs on decompression. A combination of rigid-body symmetry mode analysis and density functional theory calculations enables the soft vibrational lattice mode which governs the transformation to be identified.

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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); USDOE

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1577894

Alternate ID(s):: OSTI ID: 1599833

Journal Information:: IUCrJ, Vol. 7, Issue 1; ISSN 2052-2525

Publisher:: International Union of CrystallographyCopyright Statement

Country of Publication:: United States

Language:: English

References (72)

Structural behaviour of OP-ROY at extreme conditions Funnell, Nicholas P.; Bull, Craig L.; Ridley, Christopher J. CrystEngComm, Vol. 21, Issue 30 https://doi.org/10.1039/C8CE01946K	journal	January 2019
Generalized Gradient Approximation Made Simple Perdew, John P.; Burke, Kieron; Ernzerhof, Matthias Physical Review Letters, Vol. 77, Issue 18, p. 3865-3868 https://doi.org/10.1103/PhysRevLett.77.3865	journal	October 1996
High-Pressure–High-Temperature Study of Benzene: Refined Crystal Structure and New Phase Diagram up to 8 GPa and 923 K Chanyshev, Artem D.; Litasov, Konstantin D.; Rashchenko, Sergey V. Crystal Growth & Design, Vol. 18, Issue 5 https://doi.org/10.1021/acs.cgd.8b00125	journal	March 2018
From dimers to the solid-state: Distributed intermolecular force-fields for pyridine Aina, Alexander A.; Misquitta, Alston J.; Price, Sarah L. The Journal of Chemical Physics, Vol. 147, Issue 16 https://doi.org/10.1063/1.4999789	journal	October 2017
Interatomic force constants from first principles: The case of α-quartz Gonze, X.; Charlier, J. -C.; Allan, D. C. Physical Review B, Vol. 50, Issue 17 https://doi.org/10.1103/PhysRevB.50.13035	journal	November 1994
FCC–HCP phase boundary in lead Kuznetsov, A.; Dmitriev, V.; Dubrovinsky, L. Solid State Communications, Vol. 122, Issue 3-4 https://doi.org/10.1016/S0038-1098(02)00112-6	journal	April 2002
Deuterium Perturbs the Molecular Arrangement in the Solid State Merz, Klaus; Kupka, Anna Crystal Growth & Design, Vol. 15, Issue 4 https://doi.org/10.1021/cg5014973	journal	March 2015
The Reticular Chemistry Structure Resource (RCSR) Database of, and Symbols for, Crystal Nets O’Keeffe, Michael; Peskov, Maxim A.; Ramsden, Stuart J. Accounts of Chemical Research, Vol. 41, Issue 12, p. 1782-1789 https://doi.org/10.1021/ar800124u	journal	December 2008
The Cambridge Structural Database Groom, Colin R.; Bruno, Ian J.; Lightfoot, Matthew P. Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials, Vol. 72, Issue 2, p. 171-179 https://doi.org/10.1107/S2052520616003954	journal	April 2016
Pressure Measurement Made by the Utilization of Ruby Sharp-Line Luminescence Forman, R. A.; Piermarini, G. J.; Barnett, J. D. Science, Vol. 176, Issue 4032 https://doi.org/10.1126/science.176.4032.284	journal	April 1972
Molecular Pair Analysis: CH⋅⋅⋅F Interactions in the Crystal Structure of Fluorobenzene? And Related Matters Dunitz, Jack. D.; Schweizer, W. Bernd Chemistry - A European Journal, Vol. 12, Issue 26 https://doi.org/10.1002/chem.200600092	journal	September 2006
High pressure solid phases of benzene. I. Raman and x‐ray studies of C ₆ H ₆ at 294 K up to 25 GPa Thiéry, M. M.; Léger, J. M. The Journal of Chemical Physics, Vol. 89, Issue 7 https://doi.org/10.1063/1.454809	journal	October 1988
Use of a CCD diffractometer in crystal structure determinations at high pressure Dawson, Alice; Allan, David R.; Parsons, Simon Journal of Applied Crystallography, Vol. 37, Issue 3 https://doi.org/10.1107/S0021889804007149	journal	May 2004
A first-principles study of the vibrational properties of crystalline tetracene under pressure Abdulla, Mayami; Refson, Keith; Friend, Richard H. Journal of Physics: Condensed Matter, Vol. 27, Issue 37 https://doi.org/10.1088/0953-8984/27/37/375402	journal	September 2015
Phase transitions and chemical transformations of benzene up to 550 °C and 30 GPa Cansell, François; Fabre, Denise; Petitet, Jean‐Pierre The Journal of Chemical Physics, Vol. 99, Issue 10 https://doi.org/10.1063/1.465711	journal	November 1993
Efficient evaluation of triple excitations in symmetry-adapted perturbation theory via second-order Møller–Plesset perturbation theory natural orbitals Hohenstein, Edward G.; Sherrill, C. David The Journal of Chemical Physics, Vol. 133, Issue 10 https://doi.org/10.1063/1.3479400	journal	September 2010
Crystal-structure prediction of pyridine with four independent molecules van de Streek, Jacco; Neumann, Marcus A. CrystEngComm, Vol. 13, Issue 23 https://doi.org/10.1039/c1ce05881a	journal	January 2011
Effect of pressure on the Raman spectra of solids. 2. Pyridine Heyns, A. M.; Venter, M. W. The Journal of Physical Chemistry, Vol. 89, Issue 21 https://doi.org/10.1021/j100267a026	journal	October 1985
Density fitting of intramonomer correlation effects in symmetry-adapted perturbation theory Hohenstein, Edward G.; Sherrill, C. David The Journal of Chemical Physics, Vol. 133, Issue 1 https://doi.org/10.1063/1.3451077	journal	July 2010
Structural Collapse of the Hydroquinone-Formic Acid Clathrate: A Pressure-Medium-Dependent Phase Transition Eikeland, Espen; Thomsen, Maja K.; Madsen, Solveig R. Chemistry - A European Journal, Vol. 22, Issue 12 https://doi.org/10.1002/chem.201504908	journal	February 2016
Accurate Molecular Van Der Waals Interactions from Ground-State Electron Density and Free-Atom Reference Data Tkatchenko, Alexandre; Scheffler, Matthias Physical Review Letters, Vol. 102, Issue 7 https://doi.org/10.1103/PhysRevLett.102.073005	journal	February 2009
High Pressure Study of Ru ₃ (CO) ₁₂ by X-ray Diffraction, Raman, and Infrared Spectroscopy Slebodnick, Carla; Zhao, Jing; Angel, Ross Inorganic Chemistry, Vol. 43, Issue 17 https://doi.org/10.1021/ic049617y	journal	August 2004
Retrieval of Crystallographically-Derived Molecular Geometry Information Bruno, Ian J.; Cole, Jason C.; Kessler, Magnus Journal of Chemical Information and Computer Sciences, Vol. 44, Issue 6 https://doi.org/10.1021/ci049780b	journal	November 2004
Isotopic Polymorphism in Pyridine Crawford, Stephen; Kirchner, Michael T.; Bläser, Dieter Angewandte Chemie International Edition, Vol. 48, Issue 4 https://doi.org/10.1002/anie.200803589	journal	January 2009
The effect of pressure on the crystal structure of l-alanine Funnell, Nicholas P.; Dawson, Alice; Francis, Duncan CrystEngComm, Vol. 12, Issue 9 https://doi.org/10.1039/c001296c	journal	January 2010
Miniature diamond anvil pressure cell for single crystal x‐ray diffraction studies Merrill, Leo; Bassett, William A. Review of Scientific Instruments, Vol. 45, Issue 2 https://doi.org/10.1063/1.1686607	journal	February 1974
OLEX2 : a complete structure solution, refinement and analysis program Dolomanov, Oleg V.; Bourhis, Luc J.; Gildea, Richard J. Journal of Applied Crystallography, Vol. 42, Issue 2 https://doi.org/10.1107/S0021889808042726	journal	January 2009
Raman and infrared spectroscopy of pyridine under high pressure Zhuravlev, Kirill K.; Traikov, Katrina; Dong, Zhaohui Physical Review B, Vol. 82, Issue 6 https://doi.org/10.1103/PhysRevB.82.064116	journal	August 2010
The high-pressure, high-temperature equation of state of calcium fluoride, CaF ₂ Angel, R. J. Journal of Physics: Condensed Matter, Vol. 5, Issue 11 https://doi.org/10.1088/0953-8984/5/11/001	journal	March 1993
Packing Problems: High Z ′ Crystal Structures and Their Relationship to Cocrystals, Inclusion Compounds, and Polymorphism Steed, Kirsty M.; Steed, Jonathan W. Chemical Reviews, Vol. 115, Issue 8 https://doi.org/10.1021/cr500564z	journal	February 2015
Low-temperature and high-pressure polymorphs of isopropyl alcohol Ridout, Joe; Probert, Michael R. CrystEngComm, Vol. 16, Issue 32 https://doi.org/10.1039/C4CE01012D	journal	January 2014
SHELXT – Integrated space-group and crystal-structure determination Sheldrick, George M. Acta Crystallographica Section A Foundations and Advances, Vol. 71, Issue 1, p. 3-8 https://doi.org/10.1107/S2053273314026370	journal	January 2015
ISODISPLACE : a web-based tool for exploring structural distortions Campbell, Branton J.; Stokes, Harold T.; Tanner, David E. Journal of Applied Crystallography, Vol. 39, Issue 4 https://doi.org/10.1107/S0021889806014075	journal	July 2006
Low-Temperature Elastic Moduli of Lead Waldorf, D. L.; Alers, G. A. Journal of Applied Physics, Vol. 33, Issue 11 https://doi.org/10.1063/1.1931149	journal	November 1962
Crystal structures of pyridine and pyridine trihydrate Mootz, D.; Wussow, H. ‐G. The Journal of Chemical Physics, Vol. 75, Issue 3 https://doi.org/10.1063/1.442204	journal	August 1981
Thermoelastic properties of deuterated melamine, C ₃ N ₆ D ₆ , between 4.2–320 K at 5 kPa and between 0.1–5.0 GPa at 295 K from neutron powder diffraction and DFT calculations Fortes, A. D.; Funnell, N. P.; Bull, C. L. High Pressure Research, Vol. 39, Issue 1 https://doi.org/10.1080/08957959.2019.1578879	journal	January 2019
Hypothetical Crystal Structures of Benzene at 0 and 30 kbar van Eijck, B. P.; Spek, A. L.; Mooij, W. T. M. Acta Crystallographica Section B Structural Science, Vol. 54, Issue 3 https://doi.org/10.1107/S0108768197013384	journal	June 1998
Alloxan: Is it really a problem structure? Dunitz, Jack D.; Schweizer, W. Bernd CrystEngComm, Vol. 9, Issue 4 https://doi.org/10.1039/b700475c	journal	January 2007
Mercury CSD 2.0 – new features for the visualization and investigation of crystal structures Macrae, Clare F.; Bruno, Ian J.; Chisholm, James A. Journal of Applied Crystallography, Vol. 41, Issue 2 https://doi.org/10.1107/S0021889807067908	journal	March 2008
Variational density-functional perturbation theory for dielectrics and lattice dynamics Refson, Keith; Tulip, Paul R.; Clark, Stewart J. Physical Review B, Vol. 73, Issue 15 https://doi.org/10.1103/PhysRevB.73.155114	journal	April 2006
Structure validation in chemical crystallography Spek, Anthony L. Acta Crystallographica Section D Biological Crystallography, Vol. 65, Issue 2, p. 148-155 https://doi.org/10.1107/S090744490804362X	journal	January 2009
Hirshfeld surface analysis Spackman, Mark A.; Jayatilaka, Dylan CrystEngComm, Vol. 11, Issue 1 https://doi.org/10.1039/B818330A	journal	January 2009
Topology of molecular packings in organic crystals Peresypkina, E. V.; Blatov, V. A. Acta Crystallographica Section B Structural Science, Vol. 56, Issue 6 https://doi.org/10.1107/S0108768100011824	journal	December 2000
Efficient computer modeling of organic materials. The atom–atom, Coulomb–London–Pauli (AA-CLP) model for intermolecular electrostatic-polarization, dispersion and repulsion energies Gavezzotti, Angelo New Journal of Chemistry, Vol. 35, Issue 7 https://doi.org/10.1039/c0nj00982b	journal	January 2011
Infrared Spectra of Crystalline and Matrix Isolated Pyridine and Pyridine‐D ₅ Castellucci, E.; Sbrana, G.; Verderame, F. D. The Journal of Chemical Physics, Vol. 51, Issue 9 https://doi.org/10.1063/1.1672590	journal	November 1969
Reversible piezochromism in a molecular wine-rack Harty, Elena L.; Ha, Alex R.; Warren, Mark R. Chemical Communications, Vol. 51, Issue 53 https://doi.org/10.1039/C5CC02916C	journal	January 2015
Pressure as a tool in crystal engineering: inducing a phase transition in a high-Z′ structure Johnstone, Russell D. L.; Ieva, Maria; Lennie, Alistair R. CrystEngComm, Vol. 12, Issue 9 https://doi.org/10.1039/b917290d	journal	January 2010
Special points for Brillouin-zone integrations Monkhorst, Hendrik J.; Pack, James D. Physical Review B, Vol. 13, Issue 12, p. 5188-5192 https://doi.org/10.1103/PhysRevB.13.5188	journal	June 1976
The high-pressure phase diagram of ammonia dihydrate Fortes, A. D.; Wood, I. G.; Alfredsson, M. High Pressure Research, Vol. 27, Issue 2 https://doi.org/10.1080/08957950701265029	journal	June 2007
PEARL: the high pressure neutron powder diffractometer at ISIS Bull, C. L.; Funnell, N. P.; Tucker, M. G. High Pressure Research, Vol. 36, Issue 4 https://doi.org/10.1080/08957959.2016.1214730	journal	August 2016
TOPAS and TOPAS-Academic : an optimization program integrating computer algebra and crystallographic objects written in C++ Coelho, Alan A. Journal of Applied Crystallography, Vol. 51, Issue 1 https://doi.org/10.1107/S1600576718000183	journal	February 2018
Thermal equation of state of solid naphthalene to 13 GPa and 773 K: In situ X-ray diffraction study and first principles calculations Likhacheva, Anna Y.; Rashchenko, Sergey V.; Chanyshev, Artem D. The Journal of Chemical Physics, Vol. 140, Issue 16 https://doi.org/10.1063/1.4871741	journal	April 2014
Applied Topological Analysis of Crystal Structures with the Program Package ToposPro Blatov, Vladislav A.; Shevchenko, Alexander P.; Proserpio, Davide M. Crystal Growth & Design, Vol. 14, Issue 7 https://doi.org/10.1021/cg500498k	journal	May 2014
Crystal structure refinement with SHELXL Sheldrick, George M. Acta Crystallographica Section C Structural Chemistry, Vol. 71, Issue 1, p. 3-8 https://doi.org/10.1107/S2053229614024218	journal	January 2015
Chemical Crystallography at the Advanced Light Source McCormick, Laura; Giordano, Nico; Teat, Simon Crystals, Vol. 7, Issue 12 https://doi.org/10.3390/cryst7120382	journal	December 2017
On enantiomorph-polarity estimation Flack, H. D. Acta Crystallographica Section A Foundations of Crystallography, Vol. 39, Issue 6 https://doi.org/10.1107/S0108767383001762	journal	November 1983
Structure and reactivity of pyridine crystal under pressure Fanetti, Samuele; Citroni, Margherita; Bini, Roberto The Journal of Chemical Physics, Vol. 134, Issue 20 https://doi.org/10.1063/1.3591973	journal	May 2011
Benzene under High Pressure: a Story of Molecular Crystals Transforming to Saturated Networks, with a Possible Intermediate Metallic Phase Wen, Xiao-Dong; Hoffmann, Roald; Ashcroft, N. W. Journal of the American Chemical Society, Vol. 133, Issue 23 https://doi.org/10.1021/ja201786y	journal	June 2011
Density, freezing and molecular aggregation in pyridazine, pyridine and benzene Podsiadło, Marcin; Jakóbek, Katarzyna; Katrusiak, Andrzej CrystEngComm, Vol. 12, Issue 9 https://doi.org/10.1039/c001153c	journal	January 2010
Incorporation of a new design of backing seat and anvil in a Merrill–Bassett diamond anvil cell Moggach, Stephen A.; Allan, David R.; Parsons, Simon Journal of Applied Crystallography, Vol. 41, Issue 2 https://doi.org/10.1107/S0021889808000514	journal	March 2008
EosFit7-GUI : a new graphical user interface for equation of state calculations, analyses and teaching Gonzalez-Platas, Javier; Alvaro, Matteo; Nestola, Fabrizio Journal of Applied Crystallography, Vol. 49, Issue 4 https://doi.org/10.1107/S1600576716008050	journal	June 2016
A beamline for high-pressure studies at the Advanced Light Source with a superconducting bending magnet as the source Kunz, Martin; MacDowell, Alastair A.; Caldwell, Wendel A. Journal of Synchrotron Radiation, Vol. 12, Issue 5 https://doi.org/10.1107/S0909049505020959	journal	August 2005
Size does matter—the contribution of molecular volume, shape and flexibility to the formation of co-crystals and structures with Z′ > 1 Anderson, Kirsty M.; Probert, Michael R.; Goeta, Andrés E. CrystEngComm, Vol. 13, Issue 1 https://doi.org/10.1039/C0CE00172D	journal	January 2011
A study of the known and hypothetical crystal structures of pyridine: why are there four molecules in the asymmetric unit cell? Anghel, A. T.; Day, G. M.; Price, S. L. CrystEngComm, Vol. 4, Issue 62 https://doi.org/10.1039/B202084J	journal	January 2002
Towards a realistic model for the quantitative evaluation of intermolecular potentials and for the rationalization of organic crystal structures. Part II. Crystal energy landscapesFor Part I, see ref. 4.Electronic Supplementary Information (ESI) is available: the crystallographic coordinates of all the crystal stuctures considered and the SCDS-Pixel input and output files have been deposited. See http://www.rsc.org/suppdata/ce/b3/b311836c/ Gavezzotti, A. CrystEngComm, Vol. 5, Issue 77 https://doi.org/10.1039/b311836c	journal	January 2003
The pressure derivatives of the elastic constants of lead Miller, R. A.; Schuele, D. E. Journal of Physics and Chemistry of Solids, Vol. 30, Issue 3 https://doi.org/10.1016/0022-3697(69)90014-6	journal	March 1969
Putting pressure on aromaticity along with in situ experimental electron density of a molecular crystal Casati, Nicola; Kleppe, Annette; Jephcoat, Andrew P. Nature Communications, Vol. 7, Issue 1 https://doi.org/10.1038/ncomms10901	journal	March 2016
Destabilisation of hydrogen bonding and the phase stability of aniline at high pressure Funnell, Nicholas P.; Dawson, Alice; Marshall, William G. CrystEngComm, Vol. 15, Issue 6 https://doi.org/10.1039/C2CE26403J	journal	January 2013
Isotopic Polymorphism in Pyridine Crawford, Stephen; Kirchner, Michael T.; Bläser, Dieter Angewandte Chemie, Vol. 121, Issue 4 https://doi.org/10.1002/ange.200803589	journal	January 2009
The pressure derivatives of the elastic constants of lead Miller, R. A.; Schuele, D. E. Solid State Communications, Vol. 6, Issue 10 https://doi.org/10.1016/0038-1098(68)90611-x	journal	October 1968
Quantum dissipation driven by electron transfer within a single molecule investigated with atomic force microscopy Berger, Jan; Ondráček, Martin; Stetsovych, Oleksandr Nature Communications, Vol. 11, Issue 1 https://doi.org/10.1038/s41467-020-15054-w	journal	March 2020
Putting pressure on aromaticity along with in situ experimental electron density of a molecular crystal Kleppe, Annette; Jephcoat, Andrew P.; Casati, Nicola Nature Publishing Group https://doi.org/10.7892/boris.80165	text	January 2016

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A Short Review of Current Computational Concepts for High-Pressure Phase Transition Studies in Molecular Crystals Rychkov, Denis A. Crystals, Vol. 10, Issue 2 https://doi.org/10.3390/cryst10020081	journal	January 2020

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36 MATERIALS SCIENCE
polymorphism
pressure
in situ crystallization
phase transitions

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