The crystal structure of hexaphenylbenzene under high hydrostatic pressure
Turner, Gemma F.; Stapleton, Nicholas; Brookes, James; Spagnoli, Dino; Sussardi, Alif N.; Jones, Anita C.; McGonigal, Paul R.; Moggach, Stephen A.; CrystEngComm 26 (2024) 459–467; doi:10.1039/D3CE01122D

data_7247915
_publ_section_title
;
 The crystal structure of hexaphenylbenzene under high hydrostatic
 pressure
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              459
_journal_page_last               467
_journal_paper_doi               10.1039/D3CE01122D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C42 H30'
_chemical_formula_sum            'C42 H30'
_chemical_formula_weight         534.66
_chemical_name_common            C6Ph6
_chemical_name_systematic        Hexaphenylbenzene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
;
2023-11-08 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1820(4)
_cell_length_b                   11.7900(4)
_cell_length_c                   20.8728(8)
_cell_measurement_pressure       101.325
_cell_measurement_reflns_used    8077
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.3030
_cell_measurement_theta_min      3.4410
_cell_volume                     2997.87(18)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_pressure         101.325
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'Hybrid Photon'
_diffrn_detector_type            HyPix-6000HE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -27.00  61.00   0.50   35.00    --  -21.85  19.00 -90.00  176
  2  \w    -23.00  37.00   0.50   35.00    --  -21.85 -99.00  60.00  120
  3  \w    -40.00  32.00   0.50   35.00    --  -21.85 -91.00 -28.00  144
  4  \w    -27.00  61.00   0.50   35.00    --  -21.85  19.00 150.00  176
  5  \w   -114.00  36.00   0.50   35.00    --  -21.85 -31.00 125.00  300
  6  \w   -123.00 -39.00   0.50   35.00    --  -21.85 178.00  30.00  168
  7  \w   -125.00 -41.00   0.50   35.00    --  -21.85-178.00   0.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0210914000
_diffrn_orient_matrix_UB_12      0.0486955000
_diffrn_orient_matrix_UB_13      -0.0156862000
_diffrn_orient_matrix_UB_21      0.0100145000
_diffrn_orient_matrix_UB_22      0.0258024000
_diffrn_orient_matrix_UB_23      0.0301542000
_diffrn_orient_matrix_UB_31      0.0533218000
_diffrn_orient_matrix_UB_32      -0.0241158000
_diffrn_orient_matrix_UB_33      0.0005665000
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22696
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.247
_diffrn_reflns_theta_max         23.247
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.105
_refine_diff_density_min         -0.123
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Flack x determined using 1389 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -5.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0505P)^2^+0.2370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3478
_reflns_number_total             4282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01122d2.cif
_cod_data_source_block           C6Ph6_Ambient
_cod_depositor_comments
'Adding full bibliography for 7247910--7247915.cif.'
_cod_database_code               7247915
_chemical_oxdiff_formula         'C42 H30'
_chemical_oxdiff_usercomment     'Hexaphenylbenzene under ambient conditions'
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C20(H20), C8(H8), C42(H42), C40(H40), C14(H14), C26(H26), C39(H39),
 C29(H29), C21(H21), C38(H38), C28(H28), C27(H27), C10(H10), C9(H9), C34(H34),
 C32(H32), C12(H12), C23(H23), C24(H24), C11(H11), C33(H33), C41(H41), C22(H22),
  C36(H36), C18(H18), C35(H35), C15(H15), C16(H16), C17(H17)
;
_olex2_exptl_crystal_mounting_method
'Mounted on a 200 micron MiTeGen loop in immersion oil.'
_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 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.649