Impact of Disordered Guest-Framework Interactions on the Crystallography of Metal-Organic Frameworks.
Lee, Seungkyu; Bürgi, Hans-Beat; Alshmimri, Sultan A.; Yaghi, Omar M.; Journal of the American Chemical Society 140 (2018) 8958–8964; doi:10.1021/jacs.8b05271

data_4132635
_publ_section_title
;
 Impact of Disordered Guest-Framework Interactions on the Crystallography
 of Metal-Organic Frameworks.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8958
_journal_page_last               8964
_journal_paper_doi               10.1021/jacs.8b05271
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.25(C258.94 H163.96 O128 Zr24)'
_chemical_formula_sum            'C64.5 H41 O28.5 Zr6'
_chemical_formula_weight         1819.29
_chemical_name_systematic        UiO-67
_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
_audit_creation_date             2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8422(6)
_cell_length_b                   26.8422(6)
_cell_length_c                   26.8422(6)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    260.15
_cell_measurement_theta_max      74.34
_cell_measurement_theta_min      2.85
_cell_volume                     19339.9(7)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      260.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker SMART CCD 1K 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 D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.333
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  0.7176
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1163 before and 0.0800 after correction. The Ratio of minimum to maximum transmission is 0.8697. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.625
_exptl_crystal_description       'Truncated octahedron'
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL 260k1_a.res in Fm-3m
CELL   26.8422   26.8422   26.8422     90.00     90.00     90.00
SPGR Fm-3m
Q101 0.112 0.120 0.106 !       2.28 eA-3
C102 0.500 0.502 0.250 !       1.32 eA-3
C103 0.345 0.343 0.157 !       1.04 eA-3
C104 0.250 0.250 0.250 !       0.90 eA-3
C105 0.326 0.369 0.173 !       0.90 eA-3
C106 0.642 0.321 0.141 !       0.84 eA-3
C107 0.335 0.335 0.225 !       0.80 eA-3
C108 0.617 0.381 0.157 !       0.79 eA-3
C109 0.944 0.323 0.045 !       0.79 eA-3
C110 0.687 0.342 0.158 !       0.78 eA-3
C111 0.666 0.166 0.166 !       0.77 eA-3
C112 0.500 0.042 0.176 !       0.74 eA-3
C113 0.149 0.305 0.151 !       0.73 eA-3
C114 0.135 0.338 0.133 !       0.73 eA-3
C115 0.842 0.213 0.134 !       0.71 eA-3
C116 0.690 0.189 0.347 !       0.70 eA-3
C117 0.781 0.312 0.365 !       0.69 eA-3
C118 0.196 0.466 0.034 !       0.68 eA-3
C119 0.140 0.390 0.139 !       0.68 eA-3
C120 0.544 0.211 0.001 !       0.67 eA-3
C121 0.664 0.132 0.166 !       0.66 eA-3
C122 0.392 0.133 0.001 !       0.66 eA-3
C123 0.368 0.140 0.140 !       0.64 eA-3
C124 1.000 0.080 0.344 !       0.60 eA-3
C125 0.850 0.355 0.225 !       0.59 eA-3
C126 0.912 0.084 0.283 !       0.58 eA-3
C127 0.515 0.015 0.015 !       0.57 eA-3
C128 0.689 0.419 0.419 !       0.56 eA-3
C129 0.500 0.195 0.004 !       0.56 eA-3
C130 0.500 0.140 0.140 !       0.56 eA-3
C131 0.650 0.041 0.041 !       0.55 eA-3
C132 0.118 0.391 0.115 !       0.55 eA-3
Q133 0.815 0.099 0.186 !       0.54 eA-3
C134 0.101 0.313 0.898 !       0.52 eA-3
C135 0.899 0.187 0.602 !       0.52 eA-3
C136 0.399 0.187 0.102 !       0.52 eA-3
Q137 0.730 0.480 0.224 !       0.52 eA-3
C138 0.399 0.602 0.687 !       0.52 eA-3
C139 0.593 0.095 0.015 !       0.52 eA-3
C140 0.725 0.225 0.225 !       0.51 eA-3
C141 0.079 0.353 0.091 !       0.51 eA-3
C142 0.157 0.115 0.285 !       0.51 eA-3
C143 0.345 0.178 0.212 !       0.51 eA-3
Q144 0.233 0.127 0.113 !       0.50 eA-3
C145 0.382 0.070 0.003 !       0.50 eA-3
C146 0.500 0.023 0.000 !       0.50 eA-3
;
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1052
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0353P)^2^+47.0763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                954
_reflns_number_total             1052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uio-67_22defect_DMF_260K1.cif
_cod_data_source_block           UiO-67_22defect_DMF_260K1
_cod_original_cell_volume        19339.9(13)
_cod_original_formula_sum        'C64.50 H41 O28.50 Zr6'
_cod_database_code               4132635
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(O4)=0.5*(1-FVAR(2))
 Sof(C1)=Sof(C2)=Sof(C5)=0.25*FVAR(2)
 Sof(O3)=Sof(C3)=Sof(H3)=Sof(C2AA)=Sof(H2AA)=0.5*FVAR(2)
 Fixed Sof: O1(0.08333) O2(0.08333) H1(0.08333)
 Fixed Uiso: H1(0.05)
 Fixed X: H1(1.069201)
 Fixed Y: H1(0.569201)
 Fixed Z: H1(0.569201)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2AA(H2AA)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id UiO-67_22defect_DMF_260K1
_olex2_submission_special_instructions 'No special instructions were received'