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_4134428
_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         'C68 H56 Fe2 N12, 4(F6 P), 8(C2 H3 N)'
_chemical_formula_sum            'C84 H80 F24 Fe2 N20 P4'
_chemical_formula_weight         2061.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0650(4)
_cell_length_b                   29.3865(9)
_cell_length_c                   11.9523(4)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.67
_cell_measurement_theta_min      3.01
_cell_volume                     4588.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0919
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54392
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.800
_diffrn_reflns_theta_max         66.800
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'Cu-ImuS Diamond microfocus tube'
_exptl_absorpt_coefficient_mu    4.120
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
 The residual electron density was assigned to half a
 molecule of the acetonitrile solvent [42/4 = 11 e per
 asymmetric unit; half a molecule of CH3CN would give 11e].
;
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.192(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0334P)^2^+17.7603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7530
_reflns_number_total             7991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00896_si_002.cif
_cod_data_source_block           jmljfa190401
_cod_depositor_comments
'Adding full bibliography for 4134428--4134431.cif.'
_cod_database_code               4134428
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.638
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58776
_shelx_hkl_checksum              32923
_shelx_fab_checksum              98413