#------------------------------------------------------------------------------
#$Date: 2021-10-16 05:10:36 +0300 (Sat, 16 Oct 2021) $
#$Revision: 269978 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564942.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1564942
loop_
_publ_author_name
'Tchoń, D.'
'Makal, A.'
_publ_section_title
;
 Maximizing completeness in single-crystal high-pressure diffraction
 experiments: phase transitions in 2{^i̧rc}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 tₑₓₚ ω θ κ φ Frames
--------------------------------------------------------------------------
 1 ω -21.00 69.00 1.00 4.00 -- 0.00 57.00 120.00 90
 2 ω -70.00 30.00 1.00 4.00 -- 0.00 -77.00 0.00 100
 3 ω 16.00 116.00 1.00 20.00 -- 46.30 77.00 90.00 100
 4 ω 16.00 116.00 1.00 20.00 -- 46.30 77.00-150.00 100
 5 ω -23.00 59.00 1.00 20.00 -- 46.30 -57.00 -60.00 82
 6 ω 75.00 110.00 1.00 20.00 -- 46.30 125.00-150.00 35
 7 ω 16.00 42.00 1.00 20.00 -- 46.30 77.00 60.00 26
 8 ω 74.00 102.00 1.00 20.00 -- 46.30 77.00 60.00 28
 9 ω 16.00 113.00 1.00 20.00 -- 46.30 77.00 150.00 97
 10 ω -1.00 74.00 1.00 20.00 -- 46.30 -77.00 120.00 75
 11 ω 16.00 112.00 1.00 20.00 -- 46.30 77.00 -30.00 96
 12 ω 5.00 104.00 1.00 20.00 -- 46.30-125.00 -60.00 99
 13 ω 16.00 114.00 1.00 20.00 -- 46.30 77.00 -90.00 98
 14 ω -21.00 39.00 1.00 20.00 -- 46.30 -77.00-150.00 60
 15 ω 16.00 42.00 1.00 20.00 -- 46.30 77.00 120.00 26
 16 ω 86.00 113.00 1.00 20.00 -- 46.30 77.00 120.00 27
 17 ω 16.00 42.00 1.00 20.00 -- 46.30 77.00 30.00 26
 18 ω 47.00 111.00 1.00 20.00 -- 46.30 77.00 30.00 64
 19 ω -20.00 75.00 1.00 20.00 -- 46.30 -77.00 30.00 95
 20 ω 73.00 117.00 1.00 20.00 -- 46.30 125.00 -90.00 44
 21 ω -21.00 69.00 1.00 40.00 -- 0.00 57.00 120.00 90
 22 ω -70.00 30.00 1.00 40.00 -- 0.00 -77.00 0.00 100
 23 ω 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       'ω 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/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/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
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z+1/2
3 -x,y+1/2,-z
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z-1/2
7 x,-y-1/2,z
8 x-1/2,y,-z-1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C15 C 0.62035(8) 0.75 0.55460(5) 0.01147(10) Uani 1.000000 2 S T P
C16 C 0.65046(8) 0.75 0.42904(5) 0.01251(10) Uani 1.000000 2 S T P
C2 C 0.60449(5) 0.67440(2) 0.61596(3) 0.01169(7) Uani 1.000000 1 . . .
C1 C 0.57847(6) 0.67567(2) 0.74052(3) 0.01207(7) Uani 1.000000 1 . . .
C3 C 0.62126(6) 0.60020(3) 0.54928(4) 0.01433(8) Uani 1.000000 1 . . .
H3 H 0.6131(9) 0.5443(4) 0.5940(5) 0.0316(17) Uani 1.000000 1 . . .
C4 C 0.64850(6) 0.60108(3) 0.43011(4) 0.01521(8) Uani 1.000000 1 . . .
H4 H 0.6594(9) 0.5460(4) 0.3818(5) 0.0322(16) Uani 1.000000 1 . . .
C14 C 0.57213(8) 0.75 0.79920(5) 0.01235(11) Uani 1.000000 2 S T P
H14 H 0.5502(12) 0.75 0.8938(8) 0.028(2) Uani 1.000000 2 S T P
C5 C 0.66355(6) 0.67567(3) 0.36597(4) 0.01408(8) Uani 1.000000 1 . . .
C17 C 0.55000(6) 0.60053(3) 0.81294(4) 0.01412(8) Uani 1.000000 1 . . .
O1 O 0.47250(5) 0.540961(19) 0.77291(3) 0.02157(8) Uani 1.000000 1 . . .
C7 C 0.70443(10) 0.75 0.18231(6) 0.01928(13) Uani 1.000000 2 S T P
H7 H 0.7277(12) 0.75 0.0888(8) 0.035(2) Uani 1.000000 2 S T P
C6 C 0.69068(7) 0.67670(3) 0.24287(4) 0.01778(9) Uani 1.000000 1 . . .
H6 H 0.7012(10) 0.6196(4) 0.1968(5) 0.0386(18) Uani 1.000000 1 . . .
C18 C 0.61529(8) 0.60200(3) 0.94002(4) 0.01685(9) Uani 1.000000 1 . . .
H18A H 0.7482(10) 0.6296(4) 0.9481(5) 0.0438(18) Uani 1.000000 1 . . .
H18C H 0.5203(10) 0.6369(4) 0.9929(5) 0.0398(18) Uani 1.000000 1 . . .
H18B H 0.6181(10) 0.5417(4) 0.9740(5) 0.0419(19) Uani 1.000000 1 . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.0415
0 -1 0 0.0437
0 1 0 0.0357
5 1 2 0.0871
-1 0 0 0.0763
0 -1 1 0.0374
0 1 -1 0.0374
0 -1 -1 0.0415
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C15 C16 119.37(3) . . ?
C2 C15 C16 119.37(3) 7_575 . ?
C2 C15 C2 121.27(5) 7_575 . ?
C5 C16 C15 120.34(3) . . ?
C5 C16 C15 120.34(3) 7_575 . ?
C5 C16 C5 119.30(5) 7_575 . ?
C1 C2 C15 118.50(4) . . ?
C3 C2 C15 118.72(4) . . ?
C3 C2 C1 122.75(4) . . ?
C14 C1 C2 119.22(4) . . ?
C17 C1 C2 123.11(4) . . ?
C17 C1 C14 117.63(4) . . ?
C4 C3 C2 121.30(4) . . ?
C5 C4 C3 121.36(4) . . ?
C1 C14 C1 123.14(5) 7_575 . ?
C4 C5 C16 118.91(4) . . ?
C6 C5 C16 119.65(4) . . ?
C6 C5 C4 121.44(4) . . ?
O1 C17 C1 121.87(4) . . ?
C18 C17 C1 117.51(4) . . ?
C18 C17 O1 120.58(4) . . ?
C6 C7 C6 120.54(6) 7_575 . ?
C7 C6 C5 120.43(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C15 C16 1.4328(8) . ?
C15 C2 1.4304(5) 7_575 ?
C15 C2 1.4304(5) . ?
C16 C5 1.4202(5) . ?
C16 C5 1.4202(5) 7_575 ?
C2 C1 1.4175(5) . ?
C2 C3 1.4410(6) . ?
C1 C14 1.3935(5) . ?
C1 C17 1.4981(6) . ?
C3 C4 1.3585(6) . ?
C4 C5 1.4309(6) . ?
C5 C6 1.4023(6) . ?
C17 O1 1.2169(5) . ?
C17 C18 1.5088(6) . ?
C7 C6 1.3918(6) . ?
C7 C6 1.3918(6) 7_575 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 C16 C5 C4 -0.77(6) . . . . ?
C15 C16 C5 C4 0.77(6) . . 7_575 7_575 ?
C15 C16 C5 C6 -179.19(5) . . 7_575 7_575 ?
C15 C16 C5 C6 179.19(5) . . . . ?
C15 C2 C1 C14 -1.00(5) . . . . ?
C15 C2 C1 C14 -1.00(5) 7_575 . . . ?
C15 C2 C1 C17 176.63(4) 7_575 . . . ?
C15 C2 C1 C17 176.63(4) . . . . ?
C15 C2 C3 C4 -1.10(5) 7_575 . . . ?
C15 C2 C3 C4 -1.10(5) . . . . ?
C16 C5 C4 C3 0.31(5) . . . . ?
C16 C5 C4 C3 0.31(5) 7_575 . . . ?
C16 C5 C6 C7 -0.13(6) 7_575 . . . ?
C16 C5 C6 C7 -0.13(6) . . . . ?
C2 C1 C14 C1 4.19(3) . . . 7_575 ?
C2 C1 C17 O1 -31.35(5) . . . . ?
C2 C1 C17 C18 150.74(4) . . . . ?
C2 C3 C4 C5 0.63(5) . . . . ?
C1 C14 C1 C17 173.58(5) . . 7_575 7_575 ?
C3 C4 C5 C6 -179.65(4) . . . . ?
C4 C5 C6 C7 179.83(5) . . . . ?
C5 C6 C7 C6 -0.28(3) . . . 7_575 ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 0.9999 0.9999 -0.0522 0.0540 -0.0126
0.0000 -1.0000 -0.0000 0.0419 0.0041 -0.0090
-0.0000 1.0000 0.0000 -0.0419 -0.0041 0.0090
4.9990 0.9994 1.9997 -0.1414 -0.0693 -0.4844
-0.9998 0.0001 0.0000 0.0158 0.0363 0.0901
0.0000 -1.0001 0.9999 0.0315 0.0623 -0.0306
-0.0000 1.0001 -0.9999 -0.0315 -0.0623 0.0306
0.0000 -0.9999 -0.9999 0.0522 -0.0540 0.0126
