Simultaneous Generation of a [2 ×2] Grid-Like Complex and a Linear Double Helicate: a Three-Level Self-Sorting Process.
Ayme, Jean-François; Lehn, Jean-Marie; Bailly, Corinne; Karmazin, Lydia; Journal of the American Chemical Society 142 (2020) 5819–5824; doi:10.1021/jacs.0c00896

data_4134430
_publ_section_title
;
 Simultaneous Generation of a [2 \\times 2] Grid-Like Complex and a Linear
 Double Helicate: a Three-Level Self-Sorting Process.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5819
_journal_page_last               5824
_journal_paper_doi               10.1021/jacs.0c00896
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety
'C120 H104 Cu4 N16 O8, 4(C24 H20 B), 7(C6 H6)'
_chemical_formula_sum            'C258 H226 B4 Cu4 N16 O8'
_chemical_formula_weight         3975.93
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.858(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5777(8)
_cell_length_b                   25.8125(8)
_cell_length_c                   35.2575(11)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.70
_cell_measurement_theta_min      2.63
_cell_volume                     21290.1(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w shuterless scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            170270
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.710
_diffrn_reflns_theta_max         66.710
_diffrn_reflns_theta_min         2.590
_diffrn_source                   'Cu-ImuS DIAMOND microfocus tube'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       plate
_exptl_crystal_F_000             8344
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_platon_squeeze_details
'The residual electron density was assigned to half a molecule of the benzene solvent [184/4= 23 e per asymmetric unit; half a molecule of C6H6 would give 21 e].'
_refine_diff_density_max         1.333
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         18630
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0998P)^2^+131.6198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15133
_reflns_number_total             18630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00896_si_003.cif
_cod_data_source_block           jmljfa190306
_cod_depositor_comments
'Adding full bibliography for 4134428--4134431.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4134430
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.945
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              18693
_shelx_hkl_checksum              27748
_shelx_fab_checksum              18036