Guest Exchange through Facilitated Transport in a Seemingly Impenetrable Hydrogen-Bonded Framework.
Li, Yuantao; Handke, Marcel; Chen, Yu-Sheng; Shtukenberg, Alexander G.; Hu, Chunhua T.; Ward, Michael D.; Journal of the American Chemical Society 140 (2018) 12915–12921; doi:10.1021/jacs.8b07065

data_4132868
_publ_section_title
;
 Guest Exchange through Facilitated Transport in a Seemingly Impenetrable
 Hydrogen-Bonded Framework.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12915
_journal_page_last               12921
_journal_paper_doi               10.1021/jacs.8b07065
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C52.3 H72.35 N9 O11.81 S3'
_chemical_formula_weight         1112.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 118.697(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.536(16)
_cell_length_b                   7.566(5)
_cell_length_c                   23.941(17)
_cell_measurement_reflns_used    2253
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.75
_cell_measurement_theta_min      2.56
_cell_volume                     3740(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16566
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        17.486
_diffrn_reflns_theta_max         17.486
_diffrn_reflns_theta_min         1.683
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.5423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_description       needle
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 1091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.20(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.517
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.1524
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3773
_refine_ls_wR_factor_ref         0.4011
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3643
_reflns_number_total             4651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07065_si_002.cif
_cod_data_source_block           1-RT
_cod_original_cell_volume        3740(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C52.30 H72.35 N9 O11.81 S3'
_cod_database_code               4132868
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              92253
_shelx_hkl_checksum              18206
_shelx_fab_checksum              1102