Tailoring Pore Aperture and Structural Defects in Zirconium-Based Metal‒Organic Frameworks for Krypton/Xenon Separation
Idrees, Karam B.; Chen, Zhijie; Zhang, Xuan; Mian, Mohammad Rasel; Drout, Riki J.; Islamoglu, Timur; Farha, Omar K.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.9b05048

data_4003494
_publ_section_title
;
 Tailoring Pore Aperture and Structural Defects in Zirconium-Based
 Metal--Organic Frameworks for Krypton/Xenon Separation
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b05048
_journal_year                    2020
_chemical_formula_moiety         '0.25(C240 H288 O128 Zr24)'
_chemical_formula_sum            'C60 H72 O32 Zr6'
_chemical_formula_weight         1852.49
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5606(5)
_cell_length_b                   20.5606(5)
_cell_length_c                   20.5606(5)
_cell_measurement_reflns_used    5173
_cell_measurement_temperature    146(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.80
_cell_volume                     8691.8(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      146.41
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.586
_diffrn_reflns_theta_min         1.715
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0947 before and 0.0753 after correction. The Ratio of minimum to maximum transmission is 0.8763. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.477
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         675
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0889
_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^)+(0.1655P)^2^+260.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                610
_reflns_number_total             675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b05048_si_002.cif
_cod_data_source_block           xz149_0m_a
_cod_original_cell_volume        8691.8(6)
_cod_database_code               4003494
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C4-H4
 1 with sigma of 0.02
 C3-H4
 2.58 with sigma of 0.02
 C4-C2 \\sim C3-C2
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C4(0.25) H4(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'