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_1564947
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-31
_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                   7.0202(15)
_cell_length_b                   16.0775(18)
_cell_length_c                   11.1610(16)
_cell_measurement_reflns_used    4245
_cell_measurement_temperature    295.4(9)
_cell_measurement_theta_max      27.2700
_cell_measurement_theta_min      2.2080
_cell_volume                     1259.7(4)
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      'Diamond Anvil Cell filled with parabar oil'
_diffrn_ambient_pressure         1157500
_diffrn_ambient_temperature      295.4(9)
_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 0.930
_diffrn_measured_fraction_theta_max 0.858
_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      -0.0782258664
_diffrn_orient_matrix_UB_12      0.0080029493
_diffrn_orient_matrix_UB_13      -0.0385821295
_diffrn_orient_matrix_UB_21      -0.0189170399
_diffrn_orient_matrix_UB_22      0.0374155992
_diffrn_orient_matrix_UB_23      0.0314239729
_diffrn_orient_matrix_UB_31      0.0611427897
_diffrn_orient_matrix_UB_32      0.0219236480
_diffrn_orient_matrix_UB_33      -0.0395420814
_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  0.1248
_diffrn_reflns_av_unetI/netI     0.1233
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2639
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08017
_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    1.510
_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 1.2 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         0.276
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.027(7)
_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   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2639
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.761
_reflns_number_gt                1520
_reflns_number_total             2639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPga_12kbar
_cod_database_code               1564947
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H14 O2'
_chemical_oxdiff_usercomment     'Yellow block with own faces, ~1.1GPa'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.980
_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
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C6(H6), C14(H14), C4(H4), C8(H8), C3(H3), C7(H7)
2.b Idealised Me refined as rotating group:
 C24(H24B,H24A,H24C), C18(H18C,H18B,H18A)
;
_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 7.526
_oxdiff_exptl_absorpt_empirical_full_min 0.474