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_7710668
_publ_section_title
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 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
'C372 H204 O256 Zr48, 6(C2.965 O11.985 Zr2.224)'
_chemical_formula_sum            'C389.79 H204 O327.91 Zr61.34'
_chemical_formula_weight         15728.99
_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             2021-09-24
_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            1
_cell_length_a                   29.9798(6)
_cell_length_b                   29.9798(6)
_cell_length_c                   29.9798(6)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      68.269
_cell_measurement_theta_min      2.553
_cell_volume                     26945.5(9)
_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  0.1084
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            59176
_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         68.319
_diffrn_reflns_theta_min         2.084
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.122
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1035 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.8843.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       block
_exptl_crystal_F_000             7620
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4762
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0775
_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^)+(0.0925P)^2^+242.6785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01108e2.cif
_cod_data_source_block           664_gfa_0m
_cod_original_cell_volume        26945.5(16)
_cod_database_code               7710668
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.821
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004 within 2A
3. Others
 Sof(Zr4)=0.125*FVAR(2)
 Sof(Zr3)=Sof(C10)=Sof(C11)=0.25*FVAR(2)
 Sof(O9)=Sof(O10)=Sof(O12)=Sof(O13)=0.5*FVAR(2)
 Fixed Sof: O3(0.5) O3A(0.5) O5(0.25) O5A(0.25) O6(0.25) O6A(0.25) C9(0.25)
 H9(0.25) O11(0.01563)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51699
_shelx_hkl_checksum              47049
_shelx_fab_checksum              22510
_olex2_submission_special_instructions 'No special instructions were received'