Maximizing completeness in single-crystal high-pressure diffraction experiments: phase transitions in 2{^i̧rc}AP
Tchoń, D.; Makal, A.; IUCrJ 8 (2021) –; doi:10.1107/S2052252521009532

data_1564949
_publ_section_title
;
 Maximizing completeness in single-crystal high-pressure diffraction
 experiments: phase transitions in 2{^\,irc}AP
;
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252521009532
_journal_volume                  8
_journal_year                    2021
_chemical_formula_moiety         'C20 H14 O2'
_chemical_formula_sum            'C20 H14 O2'
_chemical_formula_weight         286.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ac'
_space_group_name_H-M_alt        'P 1 1 21/a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                95.074(17)
_cell_formula_units_Z            4
_cell_length_a                   6.8697(19)
_cell_length_b                   15.960(2)
_cell_length_c                   11.1099(18)
_cell_measurement_reflns_used    2865
_cell_measurement_temperature    295.4(4)
_cell_measurement_theta_max      27.0460
_cell_measurement_theta_min      3.4460
_cell_volume                     1213.3(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with parabar oil'
_diffrn_ambient_pressure         2029000
_diffrn_ambient_temperature      295.4(4)
_diffrn_crystal_treatment
'Pressurized slowly in parabar oil as a hydrostatic medium.'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.848
_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    -11.00  24.00   1.00   80.00    --    6.97  81.00 151.00   35
  2  \w    -37.00 -11.00   1.00   80.00    --    6.97 -53.00  17.00   26
  3  \w    -30.00  10.00   1.00   80.00    --    6.97  19.00-180.00   40
  4  \w    -37.00 -10.00   1.00   80.00    --    6.97 -53.00-162.00   27
  5  \w     10.00  38.00   1.00   80.00    --    6.97 -77.00-120.00   28
  6  \w     -7.00  33.00   1.00   80.00    --    6.97 -53.00  17.00   40
  7  \w    -17.00  59.00   1.00   80.00    --    6.97 -13.00   3.00   76
  8  \w    -10.00  24.00   1.00   80.00    --    6.97  81.00 -29.00   34
  9  \w     -9.00  33.00   1.00   80.00    --    6.97 -53.00-162.00   42
 10  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00  30.00   23
 11  \w    -33.00  -8.00   1.00   80.00    --   -8.77 -13.00-176.00   25
 12  \w    -19.00  16.00   1.00   80.00    --   -8.77 -97.00-143.00   35
 13  \w     -1.00  33.00   1.00   80.00    --   -8.77 -13.00-176.00   34
 14  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00 120.00   23
 15  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00-150.00   23
 16  \w    -19.00  18.00   1.00   80.00    --   -8.77 -97.00  35.00   37
 17  \w    -39.00  49.00   1.00   80.00    --   -8.77   0.00   0.00   88
 18  \w    -57.00 -14.00   1.00   80.00    --   -8.77 114.00 -45.00   43
 19  \w    -47.00 -15.00   1.00   80.00    --   -8.77  97.00 143.00   32
 20  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00 -60.00   23
 21  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00 150.00   23
 22  \w    -64.00 -38.00   1.00  320.00    --   -8.77 135.00 123.00   26
 23  \w    -24.00   7.00   1.00  320.00    --   -8.77  53.00 -17.00   31
 24  \w     10.00  36.00   1.00  320.00    --   -8.77  53.00 -17.00   26
 25  \w     -6.00  39.00   1.00  320.00    --   -8.77-114.00-135.00   45
 26  \w    -24.00  14.00   1.00  320.00    --   -8.77 -39.00  12.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support
'Diamond Anvil Cell, effective opening angle of 55 degrees'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116852000
_diffrn_orient_matrix_UB_12      0.0366314000
_diffrn_orient_matrix_UB_13      -0.0827159000
_diffrn_orient_matrix_UB_21      -0.0381792000
_diffrn_orient_matrix_UB_22      -0.0323998000
_diffrn_orient_matrix_UB_23      -0.0167023000
_diffrn_orient_matrix_UB_31      -0.0198297000
_diffrn_orient_matrix_UB_32      0.0410794000
_diffrn_orient_matrix_UB_33      0.0600251000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1529
_diffrn_reflns_av_unetI/netI     0.2781
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4304
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.888
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50558
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using parabar oil as pressure medium.'
_exptl_crystal_pressure_history
'Pressurized to 2.0 GPa and left to stabilize over 24 hours.'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.013(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.2303
_refine_ls_R_factor_gt           0.0813
_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^)+(0.0825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1532
_reflns_number_total             4304
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9795\% 
around [1.00 -0.00 -0.04] (reciprocal) or [1.00 -0.00 0.01] (direct)
;
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPde_20kbar
_cod_database_code               1564949
_shelx_shelxl_version_number     2016/6
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.594(2)
 0.406(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'