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_1564942
_publ_section_title
;
 Maximizing completeness in single-crystal high-pressure diffraction
 experiments: phase transitions in 2{^\,irc}AP
;
_journal_coeditor_code           FC5056
_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             2021-05-13
_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                90
_cell_formula_units_Z            4
_cell_length_a                   7.21024(18)
_cell_length_b                   16.4876(5)
_cell_length_c                   11.2792(3)
_cell_measurement_reflns_used    10439
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      40.1750
_cell_measurement_theta_min      3.3290
_cell_volume                     1340.87(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0013
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9870
_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 -21.00 69.00 1.00 4.00 -- 0.00 57.00 120.00 90
 2 \w -70.00 30.00 1.00 4.00 -- 0.00 -77.00 0.00 100
 3 \w 16.00 116.00 1.00 20.00 -- 46.30 77.00 90.00 100
 4 \w 16.00 116.00 1.00 20.00 -- 46.30 77.00-150.00 100
 5 \w -23.00 59.00 1.00 20.00 -- 46.30 -57.00 -60.00 82
 6 \w 75.00 110.00 1.00 20.00 -- 46.30 125.00-150.00 35
 7 \w 16.00 42.00 1.00 20.00 -- 46.30 77.00 60.00 26
 8 \w 74.00 102.00 1.00 20.00 -- 46.30 77.00 60.00 28
 9 \w 16.00 113.00 1.00 20.00 -- 46.30 77.00 150.00 97
 10 \w -1.00 74.00 1.00 20.00 -- 46.30 -77.00 120.00 75
 11 \w 16.00 112.00 1.00 20.00 -- 46.30 77.00 -30.00 96
 12 \w 5.00 104.00 1.00 20.00 -- 46.30-125.00 -60.00 99
 13 \w 16.00 114.00 1.00 20.00 -- 46.30 77.00 -90.00 98
 14 \w -21.00 39.00 1.00 20.00 -- 46.30 -77.00-150.00 60
 15 \w 16.00 42.00 1.00 20.00 -- 46.30 77.00 120.00 26
 16 \w 86.00 113.00 1.00 20.00 -- 46.30 77.00 120.00 27
 17 \w 16.00 42.00 1.00 20.00 -- 46.30 77.00 30.00 26
 18 \w 47.00 111.00 1.00 20.00 -- 46.30 77.00 30.00 64
 19 \w -20.00 75.00 1.00 20.00 -- 46.30 -77.00 30.00 95
 20 \w 73.00 117.00 1.00 20.00 -- 46.30 125.00 -90.00 44
 21 \w -21.00 69.00 1.00 40.00 -- 0.00 57.00 120.00 90
 22 \w -70.00 30.00 1.00 40.00 -- 0.00 -77.00 0.00 100
 23 \w 16.00 116.00 1.00 130.00 -- 46.30 77.00 90.00 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0157812000
_diffrn_orient_matrix_UB_12      -0.0418760000
_diffrn_orient_matrix_UB_13      -0.0103468000
_diffrn_orient_matrix_UB_21      -0.0362876000
_diffrn_orient_matrix_UB_22      -0.0041295000
_diffrn_orient_matrix_UB_23      0.0581383000
_diffrn_orient_matrix_UB_31      -0.0900694000
_diffrn_orient_matrix_UB_32      0.0089909000
_diffrn_orient_matrix_UB_33      -0.0215768000
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9870
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4493
_diffrn_reflns_point_group_measured_fraction_full 0.9984
_diffrn_reflns_point_group_measured_fraction_max 0.9870
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         41.06
_diffrn_reflns_theta_min         2.47
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
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    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             600.297
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.4887
_refine_diff_density_min         -0.5380
_refine_diff_density_rms         0.1086
_refine_ls_d_res_high            0.5410
_refine_ls_d_res_low             8.2438
_refine_ls_goodness_of_fit_ref   0.9394
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9394
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2997
_reflns_number_total             4492
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPal_0kbar
_cod_original_cell_volume        1340.86(6)
_cod_database_code               1564942
_chemical_oxdiff_formula         'C20 H14 O2'
_chemical_oxdiff_usercomment     '2oAP sample for High-res'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     40.15
_olex2_refinement_description
;
;
_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 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.805