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_4132811
_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)52, (HCO2)44],4(H2NMe2Cl)'
_chemical_formula_sum            'C44 H96 Cl4 O164 Zr36'
_chemical_formula_weight         6674.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           42
_space_group_name_Hall           'F 2 -2'
_space_group_name_H-M_alt        'F m m 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.835(7)
_cell_length_b                   43.607(9)
_cell_length_c                   15.766(3)
_cell_measurement_reflns_used    108640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.425
_cell_measurement_theta_min      0.372
_cell_volume                     23949(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.650
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67380
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        22.955
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    7.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             12720
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Flack x determined using 7235 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(4)
_refine_ls_extinction_coef       0.00040(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         23111
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0881P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                17823
_reflns_number_total             23111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06757_si_001.cif
_cod_data_source_block           ZF-2
_cod_database_code               4132811
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.327
_shelx_estimated_absorpt_t_max   0.481
_exptl_absorpt_special_details   'HKL3000sm Scalepack'
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              79440
_shelx_hkl_checksum              45971