A stable ultra-microporous hafnium-based metal–organic framework with high performance for CO2 adsorption and separation
Ma, Yali; Wang, Haitang; Wang, Hailong; Wang, Jiani; Jiang, Shuaiyu; Zheng, Qiang; Jia, Songyan; Li, Xue; Ma, Tianyi; CrystEngComm 25 (2023) 6489–6495; doi:10.1039/D3CE01022H

data_7247705
_publ_section_title
;
 A stable ultra-microporous hafnium-based metal--organic framework with
 high performance for CO2 adsorption and separation
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              6489
_journal_page_last               6495
_journal_paper_doi               10.1039/D3CE01022H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C120 H72 Hf6 O32'
_chemical_formula_sum            'C120 H72 Hf6 O32'
_chemical_formula_weight         3096.71
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-05
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-10-15 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.238(6)
_cell_length_b                   30.238(6)
_cell_length_c                   15.131(5)
_cell_measurement_reflns_used    4035
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.686
_cell_measurement_theta_min      2.334
_cell_volume                     11981(5)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1138
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25290
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.347
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_T_max  0.08123
_exptl_absorpt_correction_T_min  0.01256
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     822
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0948P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2959
_reflns_number_total             4674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01022h2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7247705.cif.'
_cod_original_cell_volume        11981(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7247705
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.506
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5
\\sim O6: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 5A
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C19(H19)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86252
_shelx_fab_checksum              60505
_olex2_submission_special_instructions 'No special instructions were received'