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This study details the structural characterization of glycolide-h4 as a function of pressure to 6 GPa using neutron powder diffraction on the PEARL instrument at ISIS Neutron and Muon source. Glycolide-h4, rather than its deuterated isotopologue, was used in this study due to the difficulty of deuteration. The low background afforded by zirconia-toughened alumina anvils nevertheless enabled the collection of data suitable for structural analysis to be obtained to a pressure of 5 GPa. Glycolide-h4 undergoes a reconstructive phase transition at 0.15 GPa to a previously identified form (II), which is stable to 6 GPa.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617015657/xk5043sup1.cif
Contains datablocks 12tns, 26tns, 35tns, 50tns, 59tns

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520617015657/xk504312tnssup2.rtv
Contains datablock 12tprofile

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520617015657/xk504326tnssup3.rtv
Contains datablock 26tprofile

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520617015657/xk504335tnssup4.rtv
Contains datablock 35tprofile

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520617015657/xk504350tnssup5.rtv
Contains datablock 50tprofile

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520617015657/xk504359tnssup6.rtv
Contains datablock 59tprofile

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617015657/xk5043sup7.pdf
Supplementary material

html

Hyper-Text Markup Language (HTML) file
Electronic data for glycolide-h4

CCDC references: 1582353; 1582354; 1582355; 1582356; 1582357

Computing details top

For all structures, data collection: ISIS data collection; cell refinement: TOPAS Academic; data reduction: Mantid; program(s) used to solve structure: CSD; program(s) used to refine structure: TOPAS Academic.

Glycolide (12tns) top
Crystal data top
C4H4O4V = 441.71 (6) Å3
Mr = 116.07Z = 4
Orthorhombic, PbcaF(000) = 240
a = 5.1174 (4) ÅDx = 1.745 Mg m3
b = 7.3666 (4) ÅT = 298 K
c = 11.7174 (10) Å
Data collection top
ZnS scintillator
diffractometer
Scan method: time of flight
Radiation source: Spallation source, spallation
Refinement top
Rp = 1.739Profile function: pseudo-Voigt
Rwp = 1.737Background function: Chebyshev polynomial
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/BeqOcc. (<1)
O10.3213 (15)0.7188 (8)0.3381 (3)1.58 (7)0.5
C10.4015 (8)0.6178 (5)0.41281 (19)1.58 (7)0.5
O20.2734 (6)0.6107 (6)0.5126 (3)1.58 (7)0.5
C30.3658 (6)0.5015 (4)0.60739 (13)1.58 (7)0.5
H310.4151 (10)0.5952 (5)0.67657 (15)1.90 (9)0.5
H320.2016 (9)0.4172 (7)0.6350 (3)1.90 (9)0.5
C40.5986 (8)0.3822 (5)0.58716 (19)1.58 (7)0.5
O40.6789 (15)0.2812 (8)0.6618 (3)1.58 (7)0.5
O50.7266 (6)0.3894 (6)0.4873 (3)1.58 (7)0.5
C60.6342 (6)0.4984 (4)0.39266 (13)1.58 (7)0.5
H610.5848 (10)0.4048 (5)0.32347 (15)1.90 (9)0.5
H620.7984 (9)0.5828 (7)0.3650 (3)1.90 (9)0.5
Glycolide (26tns) top
Crystal data top
C4H4O4V = 407.28 (5) Å3
Mr = 116.07Z = 4
Orthorhombic, PbcaF(000) = 240
a = 4.9209 (4) ÅDx = 1.893 Mg m3
b = 7.1818 (5) ÅT = 298 K
c = 11.5243 (10) Å
Data collection top
ZnS scintillator
diffractometer
Scan method: time of flight
Radiation source: Spallation source, spallation
Refinement top
Rp = 1.525Profile function: pseudo-Voigt
Rwp = 1.607Background function: Chebyshev polynomial
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/BeqOcc. (<1)
O10.305 (10)0.706 (9)0.328 (2)0.14 (6)0.5
C10.395 (4)0.613 (3)0.4078 (10)0.14 (6)0.5
O20.246 (2)0.593 (3)0.5047 (10)0.14 (6)0.5
C30.350 (3)0.500 (4)0.6070 (10)0.14 (6)0.5
H310.415 (9)0.609 (7)0.6676 (19)0.17 (8)0.5
H320.186 (5)0.414 (8)0.641 (4)0.17 (8)0.5
C40.593 (5)0.372 (4)0.5866 (15)0.14 (6)0.5
O40.661 (9)0.258 (7)0.660 (3)0.14 (6)0.5
O50.719 (9)0.371 (7)0.483 (3)0.14 (6)0.5
C60.649 (3)0.500 (3)0.3932 (7)0.14 (6)0.5
H610.623 (9)0.420 (8)0.313 (3)0.17 (8)0.5
H620.815 (5)0.602 (5)0.388 (6)0.17 (8)0.5
Glycolide (35tns) top
Crystal data top
C4H4O4V = 394.91 (5) Å3
Mr = 116.07Z = 4
Orthorhombic, PbcaF(000) = 240
a = 4.8571 (4) ÅDx = 1.952 Mg m3
b = 7.1033 (5) ÅT = 298 K
c = 11.4462 (10) Å
Data collection top
ZnS scintillator
diffractometer
Scan method: time of flight
Radiation source: Spallation source, spallation
Refinement top
Rp = 1.653Profile function: pseudo-Voigt
Rwp = 1.621Background function: Chebyshev polynomial
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/BeqOcc. (<1)
O10.336 (12)0.744 (9)0.343 (5)0.224970.5
C10.394 (5)0.613 (4)0.4077 (12)0.224970.5
O20.248 (4)0.600 (4)0.5065 (12)0.224970.5
C30.351 (4)0.503 (5)0.6086 (11)0.224970.5
H310.417 (11)0.610 (8)0.671 (2)0.2699640.5
H320.177 (6)0.426 (10)0.647 (5)0.2699640.5
C40.598 (6)0.377 (5)0.5892 (16)0.224970.5
O40.701 (11)0.290 (9)0.670 (3)0.224970.5
O50.730 (10)0.378 (9)0.487 (3)0.224970.5
C60.656 (4)0.507 (4)0.3938 (10)0.224970.5
H610.630 (11)0.423 (9)0.314 (3)0.2699640.5
H620.832 (6)0.601 (7)0.381 (7)0.2699640.5
Glycolide (50tns) top
Crystal data top
C4H4O4V = 378.66 (5) Å3
Mr = 116.07Z = 4
Orthorhombic, PbcaF(000) = 240
a = 4.7757 (4) ÅDx = 2.036 Mg m3
b = 6.9930 (5) ÅT = 298 K
c = 11.3384 (10) Å
Data collection top
ZnS scintillator
diffractometer
Scan method: time of flight
Radiation source: Spallation source, spallation
Refinement top
Rp = 1.649Profile function: pseudo-Voigt
Rwp = 1.660Background function: Chebyshev polynomial
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/BeqOcc. (<1)
O10.333 (13)0.747 (11)0.339 (5)0.205690.5
C10.402 (5)0.624 (4)0.4100 (14)0.205690.5
O20.245 (3)0.601 (4)0.5063 (13)0.205690.5
C30.349 (4)0.504 (5)0.6097 (13)0.205690.5
H310.415 (11)0.614 (8)0.672 (2)0.2468280.5
H320.176 (5)0.420 (10)0.646 (5)0.2468280.5
C40.602 (6)0.380 (5)0.5915 (17)0.205690.5
O40.705 (11)0.287 (10)0.672 (3)0.205690.5
O50.733 (11)0.377 (10)0.487 (3)0.205690.5
C60.663 (3)0.512 (4)0.3941 (10)0.205690.5
H610.630 (11)0.429 (10)0.314 (3)0.2468280.5
H620.843 (6)0.608 (6)0.384 (7)0.2468280.5
Glycolide (59tns) top
Crystal data top
C4H4O4V = 369.89 (6) Å3
Mr = 116.07Z = 4
Orthorhombic, PbcaF(000) = 240
a = 4.7321 (4) ÅDx = 2.084 Mg m3
b = 6.9298 (5) ÅT = 298 K
c = 11.2798 (11) Å
Data collection top
ZnS scintillator
diffractometer
Scan method: time of flight
Radiation source: Spallation source, spallation
Refinement top
Rp = 1.781Profile function: pseudo-Voigt
Rwp = 1.795Background function: Chebyshev polynomial
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/BeqOcc. (<1)
O10.33 (2)0.751 (16)0.340 (8)0.299330.5
C10.398 (8)0.622 (6)0.409 (2)0.299330.5
O20.244 (5)0.602 (6)0.507 (2)0.299330.5
C30.343 (6)0.499 (8)0.610 (2)0.299330.5
H310.399 (18)0.606 (14)0.677 (3)0.3591960.5
H320.167 (9)0.411 (16)0.642 (8)0.3591960.5
C40.603 (10)0.379 (8)0.592 (3)0.299330.5
O40.706 (17)0.285 (16)0.673 (4)0.299330.5
O50.740 (17)0.383 (16)0.488 (5)0.299330.5
C60.662 (6)0.509 (6)0.3927 (16)0.299330.5
H610.625 (16)0.419 (16)0.315 (6)0.3591960.5
H620.842 (10)0.605 (10)0.377 (11)0.3591960.5
 

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