Synthesis and structural evaluation of closed-shell folded and open-shell twisted hexabenzo[5.6.7]quinarene.
Nishiuchi, Tomohiko; Uchida, Kazuyuki; Kubo, Takashi; Chemical communications (Cambridge, England) 59 (2023) 7379–7382; doi:10.1039/d3cc02157b

data_7131717
_publ_section_title
;
 Synthesis and structural evaluation of closed-shell folded and open-shell
 twisted hexabenzo[5.6.7]quinarene.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7379
_journal_page_last               7382
_journal_paper_doi               10.1039/d3cc02157b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C42 H26'
_chemical_formula_sum            'C42 H26'
_chemical_formula_weight         530.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-14 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.766(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2349(11)
_cell_length_b                   10.4272(3)
_cell_length_c                   24.3603(10)
_cell_measurement_reflns_used    13269
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      30.8120
_cell_measurement_theta_min      1.8230
_cell_volume                     5539.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.852
_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    -61.00 -23.00   0.50    7.29    --   12.33 -57.00 -90.00   76
  2  \w    -11.00  52.00   0.50    7.29    --   12.33 -99.00-150.00  126
  3  \w    -11.00  52.00   0.50    7.29    --   12.33 -99.00 -30.00  126
  4  \w      2.00  56.00   0.50    7.29    --   12.33-107.00  96.00  108
  5  \w    -81.00  16.00   0.50    7.29    --   -7.01 -57.00   0.00  194
  6  \w    -11.00  52.00   0.50    7.29    --   12.33 -99.00  30.00  126
  7  \w    -81.00  16.00   0.50    7.29    --   -7.01 -57.00 150.00  194
  8  \w    -84.00  16.00   0.50    7.29    --   -7.01 -37.00-120.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0168834000
_diffrn_orient_matrix_UB_12      -0.0548182000
_diffrn_orient_matrix_UB_13      -0.0018138000
_diffrn_orient_matrix_UB_21      -0.0273708000
_diffrn_orient_matrix_UB_22      0.0367555000
_diffrn_orient_matrix_UB_23      -0.0165009000
_diffrn_orient_matrix_UB_31      -0.0049155000
_diffrn_orient_matrix_UB_32      -0.0164666000
_diffrn_orient_matrix_UB_33      -0.0308449000
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.764
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+2.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5409
_reflns_number_total             7363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02157b2.cif
_cod_data_source_block           xtn201212-2
_cod_depositor_comments
'Adding full bibliography for 7131716--7131717.cif.'
_cod_database_code               7131717
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H26'
_chemical_oxdiff_usercomment     567_folded
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.986
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C26(H26), C23(H23), C18(H18), C17(H17), C3(H3), C36(H36),
 C4(H4), C25(H25), C6(H6), C24(H24), C33(H33), C35(H35), C30(H30), C38(H38),
 C12(H12), C41(H41), C39(H39), C9(H9), C31(H31), C40(H40), C5(H5), C11(H11),
 C32(H32), C10(H10)
;
_shelx_res_checksum              93785
_shelx_hkl_checksum              9372
_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 1.900
_oxdiff_exptl_absorpt_empirical_full_min 0.500