A Double-Walled Knotted Cage for Guest-Adaptive Molecular Recognition.
Tamura, Yukari; Takezawa, Hiroki; Fujita, Makoto; Journal of the American Chemical Society 142 (2020) 5504–5508; doi:10.1021/jacs.0c00459

data_4134394
_publ_contact_author             'Makoto Fujita'
_publ_section_title
;
 A Double-Walled Knotted Cage for Guest-Adaptive Molecular Recognition.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5504
_journal_page_last               5508
_journal_paper_doi               10.1021/jacs.0c00459
_journal_volume                  142
_journal_year                    2020
_chemical_formula_sum            'C713.58 H804.32 N114.89 O350.35 Pd24'
_chemical_formula_weight         19148.69
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   40.908(11)
_cell_length_b                   40.908(11)
_cell_length_c                   28.479(8)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.28
_cell_measurement_theta_min      2.17
_cell_volume                     47659(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1389
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            247406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         0.996
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             19547
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
; 
 Flack x determined using 5412 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.144(10)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         24590
_refine_ls_number_restraints     1034
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1799P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14782
_reflns_number_total             24590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00459_si_002.cif
_cod_data_source_block           i-42d
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4134392--4134394.cif.
;
_cod_original_cell_volume        47657(28)
_cod_database_code               4134394
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              50179
_shelx_hkl_checksum              30310