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_7131716
_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         '2(Cl6 Sb), C H2 Cl2, C42 H26'
_chemical_formula_sum            'C43 H28 Cl14 Sb2'
_chemical_formula_weight         1284.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 97.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6573(2)
_cell_length_b                   34.0386(6)
_cell_length_c                   14.0166(2)
_cell_measurement_reflns_used    30035
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      29.8670
_cell_measurement_theta_min      1.5760
_cell_volume                     5036.34(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.883
_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    -29.00  67.00   0.50    3.94    --   -7.01  57.00  60.00  192
  2  \w    -11.00  86.00   0.50    3.94    --   12.17  57.00 150.00  194
  3  \w    -11.00  66.00   0.50    3.94    --   12.17  57.00  60.00  154
  4  \w    -29.00  67.00   0.50    3.94    --   -7.01  57.00 120.00  192
  5  \w    -11.00  52.00   0.50    3.94    --   12.17 -99.00   0.00  126
  6  \w     19.00  67.00   0.50    3.94    --   12.17-128.00  59.00   96
  7  \w    -11.00  52.00   0.50    3.94    --   12.17 -99.00 -30.00  126
  8  \w     26.00  76.00   0.50    3.94    --   12.17-142.00-111.00  100
  9  \w    -17.00  55.50   0.50    3.94    --   12.17  77.00-150.00  145
 10  \w    -84.00  16.00   0.50    3.94    --   -7.01 -37.00 -60.00  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      -0.0189361000
_diffrn_orient_matrix_UB_12      0.0024151000
_diffrn_orient_matrix_UB_13      0.0462179000
_diffrn_orient_matrix_UB_21      0.0013996000
_diffrn_orient_matrix_UB_22      -0.0206646000
_diffrn_orient_matrix_UB_23      0.0065515000
_diffrn_orient_matrix_UB_31      0.0644626000
_diffrn_orient_matrix_UB_32      0.0011680000
_diffrn_orient_matrix_UB_33      0.0207485000
_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  0.0750
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            111156
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.735
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80674
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       needle
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         13835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0737
_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^)+(0.0522P)^2^+6.9110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9880
_reflns_number_total             13835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02157b2.cif
_cod_data_source_block           xtn201212
_cod_depositor_comments
'Adding full bibliography for 7131716--7131717.cif.'
_cod_database_code               7131716
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H26 Cl12 Sb2'
_chemical_oxdiff_usercomment     567_dication
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.607
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(Cl12)=Sof(Cl11)=Sof(Cl13)=Sof(Cl14)=1-FVAR(1)
 Sof(Cl16)=Sof(Cl17)=Sof(Cl15)=Sof(Cl18)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C41(H41), C23(H23), C38(H38), C36(H36), C25(H25), C35(H35),
 C24(H24), C16(H16), C40(H40), C19(H19), C30(H30), C3(H3), C31(H31), C39(H39),
 C18(H18), C9(H9), C12(H12), C33(H33), C32(H32), C17(H17), C6(H6), C11(H11),
 C5(H5), C4(H4), C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35430
_shelx_hkl_checksum              82002
_shelx_fab_checksum              19400
_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 2.861
_oxdiff_exptl_absorpt_empirical_full_min 0.513