A Charged Coordination Cage-Based Porous Salt.
Gosselin, Eric J.; Decker, Gerald E.; Antonio, Alexandra M.; Lorzing, Gregory R.; Yap, Glenn P. A.; Bloch, Eric D.; Journal of the American Chemical Society 142 (2020) 9594–9598; doi:10.1021/jacs.0c02806

data_4134956
_publ_section_title
;
 A Charged Coordination Cage-Based Porous Salt.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9594
_journal_page_last               9598
_journal_paper_doi               10.1021/jacs.0c02806
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety
'C210 H114 Cu24 N6 O192 S24, 2(C120 H120 O40 Zr12), 6(C3 H7 N O)'
_chemical_formula_sum            'C468 H396 Cu24 N12 O278 S24 Zr24'
_chemical_formula_weight         15119.62
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   31.6505(13)
_cell_length_b                   31.6505(13)
_cell_length_c                   28.6511(15)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.11
_cell_measurement_theta_min      2.79
_cell_volume                     24856.1(19)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            247844
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.585
_diffrn_reflns_theta_min         1.612
_exptl_absorpt_coefficient_mu    3.487
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_description       block
_exptl_crystal_F_000             7552
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.000082(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         17053
_refine_ls_number_restraints     2020
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+48.5016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11953
_reflns_number_total             17053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02806_si_002.cif
_cod_data_source_block           eric326_sq
_cod_depositor_comments
'Adding full bibliography for 4134956--4134960.cif.'
_cod_original_cell_volume        24856(2)
_cod_database_code               4134956
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.445
_shelx_estimated_absorpt_t_max   0.652
_shelx_res_checksum              15395
_shelx_hkl_checksum              99056
_shelx_fab_checksum              4030