A Microporous Zr6@Zr-MOF for the Separation of Xe and Kr
Guo, Fua-An; Zhou, Kang; Liu, Jiaqi; Li, Xingyu; Wang, Hao; Dalton Transactions  (2022) –; doi:10.1039/D2DT01108E

data_7710669
_publ_section_title
;
 A Microporous Zr6@Zr-MOF for the Separation of Xe and Kr
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01108E
_journal_year                    2022
_chemical_formula_moiety         'C51 H24 O32 Zr6, 0.75(C4.6 O11.2 Zr2.1)'
_chemical_formula_sum            'C54.45 H24 O40.4 Zr7.57'
_chemical_formula_weight         2015.53
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.9252(15)
_cell_length_b                   29.9252(15)
_cell_length_c                   29.9252(15)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      72.135
_cell_measurement_theta_min      3.303
_cell_volume                     26799(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            98433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.194
_diffrn_reflns_theta_min         3.302
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.104
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0772 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.9171.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       block
_exptl_crystal_F_000             7815
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         5073
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0635P)^2^+237.4227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             5073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01108e2.cif
_cod_data_source_block           300_wh_0m
_cod_original_cell_volume        26799(4)
_cod_original_formula_sum        'C54.45 H24 O40.40 Zr7.57'
_cod_database_code               7710669
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C13) = Uanis(C14)
4. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C9(0.25) C10(0.25) C11(0.25) C12(0.25) Zr3(0.175) Zr4(0.0875)
 O9(0.35) O10(0.35) O11(0.35) O12(0.35) C13(0.175) C14(0.175) C15(0.225)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69337
_shelx_hkl_checksum              10782
_shelx_fab_checksum              98805
_olex2_submission_special_instructions 'No special instructions were received'