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_4127348
_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 H188 N76 Ni14 O12'
_chemical_formula_weight         3997.63
_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                   17.0704(3)
_cell_length_b                   17.0704(3)
_cell_length_c                   32.8329(6)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9020
_cell_measurement_theta_min      4.5550
_cell_volume                     9567.5(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            76959
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.303
_diffrn_reflns_theta_min         2.918
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.95871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8718
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+6.1014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7696
_reflns_number_total             8718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04520_si_002.cif
_cod_data_source_block           Cage1
_cod_original_cell_volume        9567.5(4)
_cod_database_code               4127348
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              80657
_shelx_hkl_checksum              92651
_shelx_fab_checksum              71194