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_4134431
_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         'C136 H96 N24 Zn4, 6(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C144 H108 B6 F24 N28 Zn4'
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_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_reflns_used    9098
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      2.40
_cell_volume                     17580.5(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w shuterless scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            123515
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.959
_diffrn_reflns_theta_max         66.959
_diffrn_reflns_theta_min         2.398
_diffrn_source                   'Cu-ImuS DIAMOND microfocus tube'
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.120
_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 tetrafluoroborate anion and three molecules of the acetonitrile solvent [1540/16 = 96 e per asymmetric unit; half a molecule of BF4 and three molecules of C2H3N1 would give 86 e].'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 3212 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7821
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1533P)^2^+15.8972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                7366
_reflns_number_total             7821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00896_si_005.cif
_cod_data_source_block           jmljfa190430
_cod_depositor_comments
'Adding full bibliography for 4134428--4134431.cif.'
_cod_original_cell_volume        17580.5(13)
_cod_database_code               4134431
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.928
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              70728
_shelx_hkl_checksum              99001
_shelx_fab_checksum              14297