The structure of methanol at 5.09 GPa: the fortuitous formation of a new high-pressure phase
Aldum, J. Collen; Jones, Isabelle; McGonigal, Paul R.; Spagnoli, Dino; Stapleton, Nicholas D.; Turner, Gemma F.; Moggach, Stephen A.; CrystEngComm  (2022) –; doi:10.1039/D2CE01157C

data_7245600
_publ_section_title
;
 The structure of methanol at 5.09 GPa: the fortuitous formation of a new
 high-pressure phase
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01157C
_journal_year                    2022
_chemical_formula_moiety         'C H4 O'
_chemical_formula_sum            'C H4 O'
_chemical_formula_weight         32.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.69(7)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   4.3989(19)
_cell_length_b                   11.809(16)
_cell_length_c                   10.981(5)
_cell_measurement_reflns_used    787
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.2140
_cell_measurement_theta_min      4.5890
_cell_volume                     457.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.609
_diffrn_measured_fraction_theta_max 0.609
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      4.00  70.00   0.50   30.00    --   27.00   0.00 150.00  132
  2  \w     -5.00  57.00   0.50   30.00    --   27.00 -53.00  17.00  124
  3  \w    -51.00 -18.00   0.50   30.00    --   27.00 134.00 123.00   66
  4  \w    -30.00  27.00   0.50   30.00    --   27.00  39.00 -12.00  114
  5  \w    -25.00  33.00   0.50   30.00    --   27.00  13.00  -3.00  116
  6  \w      8.00  74.00   0.50   30.00    --   27.00 -97.00-143.00  132
  7  \w    -28.00   4.00   0.50   30.00    --   27.00  97.00 -35.00   64
  8  \w    -57.00   5.00   0.50   30.00    --  -27.00  53.00 -17.00  124
  9  \w    -14.00  15.00   0.50   30.00    --  -27.00 -81.00  29.00   58
 10  \w     -6.00  26.00   0.50   30.00    --  -27.00 -97.00  35.00   64
 11  \w    -22.00  13.00   0.50   30.00    --  -27.00 -53.00  17.00   70
 12  \w     -6.00  27.00   0.50   30.00    --  -27.00 -97.00-143.00   66
 13  \w    -20.00  11.00   0.50   30.00    --   27.00  81.00 151.00   62
 14  \w    -29.00   3.00   0.50   30.00    --   27.00  97.00 -35.00   64
 15  \w     16.00  46.00   0.50   30.00    --   27.00-114.00  44.00   60
 16  \w    -52.00  17.00   0.50   30.00    --  -27.00  39.00 167.00  138
 17  \w    -25.00  29.00   0.50   30.00    --  -27.00 -39.00  12.00  108
 18  \w    -28.00  28.00   0.50   30.00    --  -27.00 -39.00-167.00  112
 19  \w      5.00  39.00   0.50   30.00    --  -27.00-114.00  44.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0325343000
_diffrn_orient_matrix_UB_12      0.0567113000
_diffrn_orient_matrix_UB_13      0.0271396000
_diffrn_orient_matrix_UB_21      0.0368828000
_diffrn_orient_matrix_UB_22      -0.0199844000
_diffrn_orient_matrix_UB_23      0.0684780000
_diffrn_orient_matrix_UB_31      0.1948301000
_diffrn_orient_matrix_UB_32      -0.0054304000
_diffrn_orient_matrix_UB_33      0.0321988000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.609
_diffrn_reflns_Laue_measured_fraction_max 0.609
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1821
_diffrn_reflns_point_group_measured_fraction_full 0.609
_diffrn_reflns_point_group_measured_fraction_max 0.609
_diffrn_reflns_theta_full        19.330
_diffrn_reflns_theta_max         19.330
_diffrn_reflns_theta_min         4.630
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1632P)^2^+0.2380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                181
_reflns_number_total             234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01157c2.cif
_cod_data_source_block           tpe_10_hp1
_cod_database_code               7245600
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H20'
_chemical_oxdiff_usercomment     'TPE_as_10 @ 5.094 GPa'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.976
_reflns_odcompleteness_completeness 37.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O001) = Uanis(C006) = Uanis(O002) = Uanis(C004) = Uanis(O003) =
Uanis(C005)
3.a Idealised Me refined as rotating group:
 C004(H00D,H00E,H00F), C005(H00G,H00H,H00I), C006(H00A,H00B,H00C)
3.b Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003)
;
_shelx_res_checksum              78383
_shelx_hkl_checksum              53653
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.529
_oxdiff_exptl_absorpt_empirical_full_min 0.476