Efficient formation of [3]pseudorotaxane based on cooperative complexation of dibenzo-24-crown-8 with diphenylviologen axle.
Sakata, Yoko; Ogura, Takaya; Akine, Shigehisa; Chemical communications (Cambridge, England) 56 (2020) 8735–8738; doi:10.1039/d0cc03131c

data_7126666
_publ_section_title
;
 Efficient formation of [3]pseudorotaxane based on cooperative
 complexation of dibenzo-24-crown-8 with diphenylviologen axle.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8735
_journal_page_last               8738
_journal_paper_doi               10.1039/d0cc03131c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         C141H119B2Cl9F48N2O23
_chemical_formula_sum            'C141 H119 B2 Cl9 F48 N2 O23'
_chemical_formula_weight         3462.05
_chemical_name_common
(C24H18N2O4)(C24H32O8)2(C32H12BF24)2(CHCl3)3(MeOH)2(H2O)
_chemical_properties_physical    Efflorescent
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;
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_cell_angle_gamma                72.895(2)
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_cell_length_b                   20.4221(10)
_cell_length_c                   21.1299(11)
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_cell_measurement_temperature    90
_cell_measurement_theta_max      67.069
_cell_measurement_theta_min      2.345
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_computing_cell_refinement       'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service V4.2.9 '
_computing_data_reduction        'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
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_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0463
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_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            159701
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    2.496
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Sheldrick, 1996 / Bruker AXS)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3516
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/MeOH/pentane'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2444
_refine_ls_number_reflns         28315
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1204P)^2^+9.7990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25162
_reflns_number_total             28315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03131c2.cif
_cod_data_source_block           ogura009
_cod_depositor_comments          'Adding full bibliography for 7126666.cif.'
_cod_database_code               7126666
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              33095