Influence of Pore Size on Carbon Dioxide Diffusion in Two Isoreticular Metal‒Organic Frameworks
Forse, Alexander C.; Colwell, Kristen A.; Gonzalez, Miguel I.; Benders, Stefan; Torres-Gavosto, Rodolfo M.; Blümich, Bernhard; Reimer, Jeffrey A.; Long, Jeffrey R.; Chemistry of Materials 32 (2020) 3570–3576; doi:10.1021/acs.chemmater.0c00745

data_4003529
_publ_section_title
;
 Influence of Pore Size on Carbon Dioxide Diffusion in Two Isoreticular
 Metal--Organic Frameworks
;
_journal_issue                   8
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3570
_journal_page_last               3576
_journal_paper_doi               10.1021/acs.chemmater.0c00745
_journal_volume                  32
_journal_year                    2020
_chemical_formula_moiety         'C9.546 H2 O9.092 Zn2, 0.216(C2 O4)'
_chemical_formula_sum            'C9.98 H2 O9.96 Zn2'
_chemical_formula_weight         411.91
_chemical_name_common            Zn2(dobdc)(CO2)2.0
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-10
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.931(18)
_cell_length_b                   25.931(18)
_cell_length_c                   6.839(5)
_cell_measurement_reflns_used    4455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      4.54
_cell_volume                     3983(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2016'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10773
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.940
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 10773 reflections, Rint = 0.0838
 (6908 with I > 3sig(I), Rint = 0.0704)
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1122P)^2^+36.7376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1608
_reflns_number_total             1978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c00745_si_002.cif
_cod_data_source_block           AF001S
_cod_depositor_comments
;Adding full bibliography for 4003528--4003529.cif.

 Adding full bibliography for 4003528--4003529.cif.
;
_cod_original_cell_volume        3982(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4003529
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.560(3)
 0.440(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O5B-O4
 2.32 with sigma of 0.01
 O4-O5A
 2.32 with sigma of 0.01
 O6-O7
 2.32 with sigma of 0.01
 O5A-C5A = O5B-C5B = O4-C5B = O4-C5A = O4-C5C = O5C-C5C = O6-C6 = O7-C6
 1.16 with sigma of 0.01
 O4-O5C
 2.32 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C5C \\sim O5C \\sim C5A \\sim O5A \\sim O5B \\sim C5B \\sim O4: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O6 \\sim C6 \\sim O7: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
5. Rigid body (RIGU) restrains
 O6, C6, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5C, O5C, C5A, O5A, O5B, C5B, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O5C)=Sof(C5C)=0.12*FVAR(2)
 Sof(C5B)=Sof(O5B)=0.37*FVAR(2)
 Sof(O5A)=Sof(C5A)=0.51*FVAR(2)
 Sof(O4)=FVAR(1)
 Sof(O7)=Sof(O6)=Sof(C6)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              64463
_shelx_hkl_checksum              93066
_olex2_submission_special_instructions 'No special instructions were received'