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_4134959
_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         'C120 H120 O40 Zr12, 4(Cl)'
_chemical_formula_sum            'C120 H120 Cl4 O40 Zr12'
_chemical_formula_weight         3438.59
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   36.587(4)
_cell_length_b                   36.587(4)
_cell_length_c                   36.587(4)
_cell_measurement_reflns_used    1346
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.63
_cell_measurement_theta_min      4.01
_cell_volume                     48976(9)
_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      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0642
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8337
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        33.853
_diffrn_reflns_theta_max         33.853
_diffrn_reflns_theta_min         2.091
_exptl_absorpt_coefficient_mu    4.763
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 
RESPONSE: As in similar MOPS, this compound consistently deposits 
as weakly diffracting crystals. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_description       block
_exptl_crystal_F_000             13664
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         548
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+1501.8511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                414
_reflns_number_total             548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02806_si_002.cif
_cod_data_source_block           eric171_sq
_cod_depositor_comments
'Adding full bibliography for 4134956--4134960.cif.'
_cod_original_cell_volume        48976(17)
_cod_database_code               4134959
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              11769
_shelx_hkl_checksum              21680
_shelx_fab_checksum              32118