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_1564948
_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             2021-03-29
_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                90
_cell_formula_units_Z            4
_cell_length_a                   6.9714(16)
_cell_length_b                   16.139(5)
_cell_length_c                   11.072(3)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.9770
_cell_measurement_theta_min      3.4170
_cell_volume                     1245.7(6)
_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         1298000
_diffrn_ambient_temperature      294(2)
_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 0.905
_diffrn_measured_fraction_theta_max 0.839
_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 39.00 87.00 1.00 30.00 -- 9.93 178.00-120.00 48
 2 \w -9.00 41.00 1.00 30.00 -- 9.93 -77.00-120.00 50
 3 \w 6.00 37.00 1.00 30.00 -- 9.93 -57.00-120.00 31
 4 \w -34.00 32.00 1.00 30.00 -- 9.93 13.00 -3.00 66
 5 \w 18.00 47.00 1.00 30.00 -- 9.93 -99.00-150.00 29
 6 \w 5.00 50.00 1.00 30.00 -- 9.93 -99.00-180.00 45
 7 \w -42.00 11.00 1.00 30.00 -- 9.93 13.00 176.00 53
 8 \w -6.00 31.00 1.00 30.00 -- 9.93 67.00 157.00 37
 9 \w 47.00 96.00 1.00 30.00 -- 9.93-178.00 120.00 49
 10 \w -48.00 -21.00 1.00 30.00 -- -10.87 -13.00 3.00 27
 11 \w -18.00 22.00 1.00 30.00 -- -10.87 -97.00 35.00 40
 12 \w -59.00 -20.00 1.00 30.00 -- -10.87 114.00 -45.00 39
 13 \w -59.00 -20.00 1.00 30.00 -- -10.87 114.00 135.00 39
 14 \w -37.00 -12.00 1.00 30.00 -- -10.87 57.00 30.00 25
 15 \w -7.00 44.00 1.00 30.00 -- -10.87 -13.00-176.00 51
 16 \w -31.00 11.00 1.00 30.00 -- -10.87 -38.00-150.00 42
 17 \w 0.00 28.00 1.00 30.00 -- -10.87 -13.00 3.00 28
 18 \w -25.00 3.00 1.00 30.00 -- -10.87 -81.00 29.00 28
 19 \w -18.00 9.00 1.00 30.00 -- -10.87 -97.00-143.00 27
 20 \w -37.00 -12.00 1.00 30.00 -- -10.87 57.00 120.00 25
 21 \w -37.00 -12.00 1.00 30.00 -- -10.87 57.00 -30.00 25
 22 \w -19.00 31.00 1.00 290.00 -- 9.93 67.00 157.00 50
 23 \w -42.00 47.00 1.00 290.00 -- 9.93 -19.00-180.00 89
 24 \w -16.00 37.00 1.00 290.00 -- 9.93 53.00 -17.00 53
 25 \w 11.00 39.00 1.00 290.00 -- 9.93 -99.00 30.00 28
 26 \w -42.00 6.00 1.00 290.00 -- 9.93 -19.00-120.00 48
 27 \w 11.00 36.00 1.00 290.00 -- 9.93 -99.00-150.00 25
 28 \w -11.00 16.00 1.00 290.00 -- -10.87 26.00 -7.00 27
 29 \w -37.00 -3.00 1.00 290.00 -- -10.87 -53.00 17.00 34
 30 \w -58.00 -20.00 1.00 290.00 -- -10.87 114.00 135.00 38
 31 \w -37.00 -12.00 1.00 290.00 -- -10.87 57.00 0.00 25
 32 \w -3.00 22.00 1.00 290.00 -- -10.87-114.00-135.00 25
 33 \w 12.00 40.00 1.00 290.00 -- -10.87-135.00 57.00 28
 34 \w -24.00 3.00 1.00 290.00 -- -10.87 -26.00 7.00 27
 35 \w -50.00 -24.00 1.00 290.00 -- -10.87 114.00 -45.00 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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0427518000
_diffrn_orient_matrix_UB_12      0.0514533000
_diffrn_orient_matrix_UB_13      -0.0188126000
_diffrn_orient_matrix_UB_21      -0.0870915000
_diffrn_orient_matrix_UB_22      0.0321756000
_diffrn_orient_matrix_UB_23      0.0058037000
_diffrn_orient_matrix_UB_31      0.0306293000
_diffrn_orient_matrix_UB_32      0.0194385000
_diffrn_orient_matrix_UB_33      0.0395654000
_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  0.1471
_diffrn_reflns_av_unetI/netI     0.1533
_diffrn_reflns_Laue_measured_fraction_full 0.905
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2920
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.874
_diffrn_reflns_theta_min         2.524
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35833
_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    1.527
_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 1.3 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         0.332
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.050(14)
_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   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2581
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                1475
_reflns_number_total             2920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5056.cif
_cod_data_source_block           2oAPga_13kbar
_cod_database_code               1564948
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20  H14  O2'
_reflns_odcompleteness_completeness 92.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C24(H24A,H24B,H24C)
;
_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 2.090
_oxdiff_exptl_absorpt_empirical_full_min 0.732