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_4132640
_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(C322.56 H184.32 O112 Zr24), 4(H1 O1)'
_chemical_formula_sum            'C84 H52 O32 Zr6'
_chemical_formula_weight         2120.57
_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                   26.8341(17)
_cell_length_b                   26.8341(17)
_cell_length_c                   26.8341(17)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    260
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.74
_cell_volume                     19322(2)
_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_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.1323
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24149
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.825
_diffrn_reflns_theta_min         1.655
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.3985
_exptl_absorpt_correction_T_min  0.2849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1670 before and 0.1411 after correction. The Ratio of minimum to maximum transmission is 0.7149. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.729
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
TITL 260k1_a.res in Fm-3m
CELL   26.8341   26.8341   26.8341     90.00     90.00     90.00
SPGR Fm-3m
Q101 0.388 0.107 0.393 !       3.32 eA-3
C102 0.381 0.119 0.119 !       1.73 eA-3
C103 0.845 0.154 0.171 !       1.69 eA-3
C104 0.500 0.203-0.004 !       1.59 eA-3
C105 0.402 0.099 0.099 !       1.51 eA-3
C106 0.525 0.477 0.319 !       1.40 eA-3
C107 0.588 0.117 0.117 !       1.39 eA-3
C108 1.000 0.336 0.000 !       1.38 eA-3
C109 0.312 0.313 0.187 !       1.37 eA-3
C110 0.956 0.334 0.046 !       1.32 eA-3
C111 0.385 0.120 0.334 !       1.29 eA-3
C112 0.937 0.398 0.002 !       1.25 eA-3
C113 0.577 0.467 0.477 !       1.19 eA-3
C114 0.141 0.142 0.234 !       1.19 eA-3
C115 1.000 0.367 0.064 !       1.17 eA-3
C116 0.594 0.094 0.148 !       1.16 eA-3
C117 0.140 0.142 0.358 !       1.15 eA-3
C118 0.500 0.503 0.258 !       1.14 eA-3
C119 0.717 0.844 0.651 !       1.11 eA-3
C120 0.217 0.344 0.651 !       1.11 eA-3
C121 0.717 0.344 0.151 !       1.11 eA-3
C122 0.783 0.156 0.849 !       1.11 eA-3
C123 0.202 0.354 0.664 !       1.10 eA-3
C124 0.544 0.456 0.456 !       1.09 eA-3
C125 0.219 0.337 0.318 !       1.07 eA-3
C126 0.071 0.500 0.000 !       1.07 eA-3
C127 0.617 0.022 0.038 !       1.06 eA-3
C128 0.547 0.492 0.334 !       1.06 eA-3
C129 0.374 0.373 0.203 !       1.05 eA-3
C130 0.195 0.076 0.424 !       1.05 eA-3
C131 0.596 0.135 0.146 !       1.05 eA-3
C132 1.000 0.366 0.030 !       1.03 eA-3
C133 0.154 0.348 0.237 !       1.02 eA-3
C134 0.322 0.421 0.457 !       1.00 eA-3
C135 0.750 0.249 0.344 !       1.00 eA-3
C136 0.587 0.025 0.085 !       1.00 eA-3
C137 0.822 0.067 0.393 !       0.99 eA-3
C138 0.627 0.028 0.134 !       0.99 eA-3
C139 0.977 0.455 0.014 !       0.98 eA-3
C140 0.800 0.141 0.195 !       0.98 eA-3
Q141 0.702 0.024 0.355 !       0.98 eA-3
C142 0.589 0.025 0.117 !       0.98 eA-3
C143 0.156 0.341 0.164 !       0.97 eA-3
C144 0.166 0.071 0.429 !       0.96 eA-3
Q145 0.468 0.183 0.259 !       0.96 eA-3
C146 0.555 0.140 0.105 !       0.96 eA-3
C147 0.235 0.123 0.180 !       0.95 eA-3
C148 0.944 0.024 0.303 !       0.95 eA-3
C149 0.837 0.279 0.189 !       0.95 eA-3
C150 0.311 0.309 0.397 !       0.94 eA-3
C151 1.000 0.461 0.061 !       0.94 eA-3
C152 0.633 0.022 0.072 !       0.94 eA-3
C153 0.366 0.204 0.135 !       0.93 eA-3
C154 0.134 0.296 0.865 !       0.93 eA-3
C155 0.866 0.296 0.865 !       0.93 eA-3
C156 0.500 0.114 0.103 !       0.93 eA-3
C157 0.485 0.485 0.274 !       0.92 eA-3
C158 0.215 0.031 0.469 !       0.92 eA-3
C159 1.000 0.367-0.006 !       0.91 eA-3
C160 0.691 0.309 0.309 !       0.90 eA-3
C161 0.618 0.112 0.171 !       0.90 eA-3
C162 0.763 0.263 0.263 !       0.89 eA-3
C163 0.837 0.310 0.190 !       0.89 eA-3
C164 0.371 0.172 0.171 !       0.88 eA-3
C165 0.250 0.316 0.316 !       0.88 eA-3
C166 0.402 0.502 0.313 !       0.88 eA-3
C167 0.297 0.367 0.773 !       0.87 eA-3
C168 0.797 0.367 0.273 !       0.87 eA-3
C169 0.797 0.867 0.773 !       0.87 eA-3
C170 0.703 0.367 0.773 !       0.87 eA-3
C171 0.133 0.774 0.797 !       0.87 eA-3
C172 1.000 0.351 0.080 !       0.87 eA-3
C173 0.707 0.136 0.201 !       0.86 eA-3
C174 0.265 0.848 0.702 !       0.85 eA-3
C175 0.713 0.282 0.273 !       0.85 eA-3
C176 0.281 0.282 0.109 !       0.84 eA-3
C177 0.500 0.163 0.124 !       0.84 eA-3
C178 0.464 0.166 0.128 !       0.83 eA-3
C179 0.119 0.386 0.232 !       0.82 eA-3
C180 0.763 0.381 0.148 !       0.82 eA-3
Q181 0.663 0.247 0.399 !       0.81 eA-3
C182 0.540 0.108 0.108 !       0.81 eA-3
C183 0.770 0.366 0.178 !       0.80 eA-3
C184 0.803 0.275 0.197 !       0.79 eA-3
C185 0.389 0.260 0.238 !       0.78 eA-3
C186 0.181 0.095 0.095 !       0.78 eA-3
Q187 0.696 0.034 0.135 !       0.78 eA-3
C188 0.708 0.102 0.102 !       0.78 eA-3
C189 0.162 0.280 0.220 !       0.77 eA-3
C190 0.542 0.061 0.102 !       0.77 eA-3
C191 0.701 0.090 0.119 !       0.77 eA-3
C192 0.674 0.277 0.777 !       0.76 eA-3
C193 0.674 0.777 0.277 !       0.76 eA-3
C194 0.174 0.277 0.277 !       0.76 eA-3
C195 0.243 0.183 0.778 !       0.75 eA-3
Q196 0.523 0.158 0.158 !       0.75 eA-3
C197 0.364 0.134 0.065 !       0.74 eA-3
C198 0.619 0.078 0.071 !       0.74 eA-3
C199 0.740 0.256 0.299 !       0.73 eA-3
;
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1025
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0976P)^2^+46.6941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                915
_reflns_number_total             1025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uio-67_4defect_DMF_260K1.cif
_cod_data_source_block           UiO-67_4defect_dmf_260K1
_cod_original_cell_volume        19322(4)
_cod_database_code               4132640
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C0AA, C1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1AA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O3(0.48) C1(0.24) C2(0.24) C5(0.24) O1(0.08333) O2(0.08333)
 H2(0.08333) O41(0.02) C1AA(0.48) H1AA(0.48) C0AA(0.48) H0AA(0.48)
 Fixed Uiso: H2(0.05) O41(0.03)
 Fixed X: H2(1.069201)
 Fixed Y: H2(0.569201)
 Fixed Z: H2(0.569201)
5.a Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C0AA(H0AA)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id UiO-67_4defect_260K1
_olex2_submission_special_instructions 'No special instructions were received'