Zirconium-Formate Macrocycles and Supercage: Molecular Packing versus MOF-like Network for Water Vapor Sorption.
Choi, Jong In; Chun, Hyungphil; Lah, Myoung Soo; Journal of the American Chemical Society 140 (2018) 10915–10920; doi:10.1021/jacs.8b06757

data_4132812
_publ_section_title
;
 Zirconium-Formate Macrocycles and Supercage: Molecular Packing versus
 MOF-like Network for Water Vapor Sorption.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10915
_journal_page_last               10920
_journal_paper_doi               10.1021/jacs.8b06757
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '[Zr36 O24 (OH)48 (HCO2)48], 3(KCl)'
_chemical_formula_sum            'C48 H96 Cl3 K3 O168 Zr36'
_chemical_formula_weight         6868.81
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.539(4)
_cell_length_b                   37.539(4)
_cell_length_c                   37.539(4)
_cell_measurement_reflns_used    349677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     52899(10)
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program(Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND 4(Putz & Brandenburg, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL-XS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            242139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.992
_diffrn_reflns_theta_min         1.309
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       cube
_exptl_crystal_F_000             26208
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details
;
 Flack x determined using 5583 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(13)
_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     438
_refine_ls_number_reflns         15553
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13062
_reflns_number_total             15553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06757_si_002.cif
_cod_data_source_block           ZF-3
_cod_original_cell_volume        52899(18)
_cod_database_code               4132812
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.965
_exptl_absorpt_special_details   'HKL3000sm Scalepack'
_shelx_res_checksum              98187
_shelx_hkl_checksum              303