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_1564943
_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                   7.2462(11)
_cell_length_b                   16.536(3)
_cell_length_c                   11.255(3)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    293.4(5)
_cell_measurement_theta_max      29.3090
_cell_measurement_theta_min      3.2940
_cell_volume                     1348.6(5)
_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         247000
_diffrn_ambient_temperature      293.4(5)
_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 0.9283
_diffrn_measured_fraction_theta_max 0.8257
_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 -6.00 22.00 1.00 20.00 -- -0.88 -39.00 12.00 28
 2 \w -54.00 -6.00 1.00 20.00 -- -0.88 0.00-120.00 48
 3 \w -20.00 1.00 1.00 20.00 -- -0.88 38.00 -60.00 21
 4 \w 33.00 60.00 1.00 20.00 -- -0.88-135.00-123.00 27
 5 \w -32.00 -1.00 1.00 20.00 -- -0.88 77.00-180.00 31
 6 \w -26.00 3.00 1.00 20.00 -- -0.88 -81.00-151.00 29
 7 \w 5.00 30.00 1.00 20.00 -- -0.88 -99.00 0.00 25
 8 \w -25.00 15.00 1.00 20.00 -- -0.88 -81.00 29.00 40
 9 \w -1.00 41.00 1.00 20.00 -- -0.88 39.00 -12.00 42
 10 \w -35.00 -9.00 1.00 20.00 -- -0.88 -39.00 12.00 26
 11 \w -36.00 36.00 1.00 210.00 -- 9.85 -53.00 17.00 72
 12 \w 5.00 50.00 1.00 210.00 -- 9.85 13.00 -3.00 45
 13 \w -40.00 26.00 1.00 210.00 -- 9.85 13.00 176.00 66
 14 \w 5.00 50.00 1.00 210.00 -- 9.85 -99.00-180.00 45
 15 \w 48.00 86.00 1.00 210.00 -- 9.85 178.00 120.00 38
 16 \w 15.00 50.00 1.00 210.00 -- 9.85 -99.00-150.00 35
 17 \w -1.00 31.00 1.00 210.00 -- 9.85 67.00 157.00 32
 18 \w -9.00 41.00 1.00 210.00 -- 9.85 -77.00-120.00 50
 19 \w 8.00 37.00 1.00 210.00 -- 9.85 -57.00-120.00 29
 20 \w -45.00 2.00 1.00 210.00 -- 9.85 13.00 -3.00 47
 21 \w -17.00 11.00 1.00 210.00 -- -10.71 -38.00-150.00 28
 22 \w -1.00 27.00 1.00 210.00 -- -10.71 -13.00 3.00 28
 23 \w -18.00 10.00 1.00 210.00 -- -10.71 -97.00 35.00 28
 24 \w -47.00 -8.00 1.00 210.00 -- -10.71 19.00-150.00 39
 25 \w -37.00 -12.00 1.00 210.00 -- -10.71 57.00 120.00 25
 26 \w -36.00 14.00 1.00 210.00 -- -10.71 53.00 162.00 50
 27 \w -18.00 13.00 1.00 210.00 -- -10.71 -97.00-143.00 31
 28 \w -71.00 -41.00 1.00 210.00 -- -10.71 135.00 123.00 30
 29 \w -59.00 -18.00 1.00 210.00 -- -10.71 114.00 -45.00 41
 30 \w -37.00 -12.00 1.00 210.00 -- -10.71 57.00 -30.00 25
;
_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  0.1567
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_Laue_measured_fraction_full 0.9283
_diffrn_reflns_Laue_measured_fraction_max 0.8257
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1578
_diffrn_reflns_point_group_measured_fraction_full 0.9283
_diffrn_reflns_point_group_measured_fraction_max 0.8257
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01456
_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    1.410
_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 0.2 GPa and left to stabilize over 24 hours.'
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.5950
_refine_diff_density_min         -0.7652
_refine_diff_density_rms         0.1352
_refine_ls_d_res_high            0.7248
_refine_ls_d_res_low             9.3043
_refine_ls_extinction_coef       0.037(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0221
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0221
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -19
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                853
_reflns_number_total             1577
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPal_2kbar
_cod_database_code               1564943
_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
;