Boat-to-boat conformation inversions of cyclobis[7,8-(<i>para</i>-quinodimethane)-3,7-(9-(<i>p</i>-tolyl)-9<i>H</i>-carbazole)] in the neutral and tetracationic state.
Tong, Zekun; Dong, Shaoqiang; Chemical communications (Cambridge, England) 60 (2024) 12766–12769; doi:10.1039/d4cc04517c

data_7133938
_publ_section_title
;
 Boat-to-boat conformation inversions of
 cyclobis[7,8-(<i>para</i>-quinodimethane)-3,7-(9-(<i>p</i>-tolyl)-9<i>H</i>-carbazole)]
 in the neutral and tetracationic state.
;
_journal_issue                   87
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12766
_journal_page_last               12769
_journal_paper_doi               10.1039/d4cc04517c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C90 H78 N2'
_chemical_formula_sum            'C90 H78 N2'
_chemical_formula_weight         1187.54
_chemical_name_systematic        CBQCz
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-01 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                82.377(4)
_cell_angle_beta                 88.409(3)
_cell_angle_gamma                74.137(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2461(5)
_cell_length_b                   17.5780(8)
_cell_length_c                   17.8214(7)
_cell_measurement_reflns_used    11935
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      31.9650
_cell_measurement_theta_min      1.8190
_cell_volume                     3657.4(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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   -115.00  65.00   1.00    6.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    6.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    6.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002645000
_diffrn_orient_matrix_UB_12      -0.0407497000
_diffrn_orient_matrix_UB_13      0.0062875000
_diffrn_orient_matrix_UB_21      0.0532692000
_diffrn_orient_matrix_UB_22      -0.0104862000
_diffrn_orient_matrix_UB_23      -0.0182001000
_diffrn_orient_matrix_UB_31      0.0280762000
_diffrn_orient_matrix_UB_32      -0.0044161000
_diffrn_orient_matrix_UB_33      0.0352392000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39267
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.822
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dry hexane into dichloromethane solutions.'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0048(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         14946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0874P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7979
_reflns_number_total             14946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04517c2.cif
_cod_data_source_block           r20210630b
_cod_database_code               7133938
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.987
_reflns_odcompleteness_completeness 99.90
_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:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C15(H15),
 C17(H17), C18(H18), C23(H23), C25(H25), C31(H31), C32(H32), C34(H34), C35(H35),
  C39(H39), C41(H41), C47(H47), C48(H48), C51(H51), C52(H52), C54(H54),
 C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C68(H68), C70(H70), C76(H76),
  C77(H77), C79(H79), C80(H80), C84(H84), C86(H86)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C64(H64A,
 H64B,H64C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              78336
_shelx_hkl_checksum              37551
_shelx_fab_checksum              47433
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.809