Fine-Tuning Apertures of Metal-Organic Cages: Encapsulation of Carbon Dioxide in Solution and Solid State.
Zhang, Xiang; Dong, Xia; Lu, Weigang; Luo, Dong; Zhu, Xiao-Wei; Li, Xue; Zhou, Xiao-Ping; Li, Dan; Journal of the American Chemical Society 141 (2019) 11621–11627; doi:10.1021/jacs.9b04520

data_4127350
_publ_section_title
;
 Fine-Tuning Apertures of Metal-Organic Cages: Encapsulation of Carbon
 Dioxide in Solution and Solid State.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11621
_journal_page_last               11627
_journal_paper_doi               10.1021/jacs.9b04520
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C144 H192 Cu6 N76 Ni8 O12'
_chemical_formula_weight         4030.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_atom_sites_solution_hydrogens   geom
_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                   17.00574(7)
_cell_length_b                   17.00574(7)
_cell_length_c                   33.0599(2)
_cell_measurement_reflns_used    17898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.1750
_cell_measurement_theta_min      3.6880
_cell_volume                     9560.76(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            28499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        62.994
_diffrn_reflns_theta_max         62.994
_diffrn_reflns_theta_min         3.676
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4164
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.264
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7201
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1376P)^2^+9.8333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6763
_reflns_number_total             7201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04520_si_002.cif
_cod_data_source_block           Cage4
_cod_original_cell_volume        9560.75(10)
_cod_database_code               4127350
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              65314
_shelx_hkl_checksum              26906
_shelx_fab_checksum              47795