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_1564944
_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         286.333
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_audit_creation_date             2021-06-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.11 svn.re2ff6fc for OlexSys, GUI svn.r6348)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.15(1)
_cell_length_b                   16.17(3)
_cell_length_c                   11.288(9)
_cell_measurement_reflns_used    170
_cell_measurement_temperature    295.4(6)
_cell_measurement_theta_max      26.6510
_cell_measurement_theta_min      3.6030
_cell_volume                     1305(3)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with parabar oil'
_diffrn_ambient_pressure         520500
_diffrn_ambient_temperature      295.4(6)
_diffrn_crystal_treatment
'Pressurized slowly in parabar oil as a hydrostatic medium.'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9182
_diffrn_measured_fraction_theta_max 0.8061
_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    -37.00  33.00   1.00   80.00    --    6.97 -53.00-162.00   70
  2  \w    -46.00  35.00   1.00   80.00    --    6.97 -26.00   7.00   81
  3  \w    -53.00  50.00   1.00   80.00    --    6.97  13.00  -3.00  103
  4  \w    -20.00   6.00   1.00   80.00    --    6.97 -19.00-180.00   26
  5  \w     19.00  44.00   1.00   80.00    --    6.97 -19.00-180.00   25
  6  \w    -30.00  -4.00   1.00   80.00    --    6.97  19.00-180.00   26
  7  \w     -8.00  24.00   1.00   80.00    --    6.97  81.00 -29.00   32
  8  \w    -19.00   7.00   1.00   80.00    --   -8.77 -97.00-143.00   26
  9  \w    -35.00 -12.00   1.00   80.00    --   -8.77  57.00 -60.00   23
 10  \w    -35.00 -12.00   1.00  320.00    --   -8.77  57.00 120.00   23
 11  \w    -69.00 -30.00   1.00  320.00    --   -8.77 135.00 123.00   39
 12  \w    -19.00  17.00   1.00  320.00    --   -8.77 -97.00  35.00   36
 13  \w      5.00  31.00   1.00  320.00    --   -8.77 -99.00  60.00   26
;
_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_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.9182
_diffrn_reflns_Laue_measured_fraction_max 0.8061
_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       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1411
_diffrn_reflns_point_group_measured_fraction_full 0.9182
_diffrn_reflns_point_group_measured_fraction_max 0.8061
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26651
_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    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             600.297
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using parabar oil as pressure medium.'
_exptl_crystal_pressure_history
'Pressurized to 0.5 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         0.3988
_refine_diff_density_min         -0.3837
_refine_diff_density_rms         0.0951
_refine_ls_d_res_high            0.7390
_refine_ls_d_res_low             9.2559
_refine_ls_extinction_coef       0.0075(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9283
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0031P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              12
_reflns_limit_l_min              -13
_reflns_number_gt                845
_reflns_number_total             1409
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPal_5kbar
_cod_database_code               1564944
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
;
_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
;