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_4132639
_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         '0.5(C85.44 H42.72 O56 Zr12), 4(H1 O1)'
_chemical_formula_sum            'C42.7 H25.4 O32.04 Zr6'
_chemical_formula_weight         1598.39
_chemical_name_systematic        UiO-66
_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                   20.7549(6)
_cell_length_b                   20.7549(6)
_cell_length_c                   20.7549(6)
_cell_measurement_reflns_used    5248
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.85
_cell_volume                     8940.5(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)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker Photon 2'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker Photon 2'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.1209
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.011
_diffrn_reflns_theta_min         1.743
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.5732
_exptl_absorpt_correction_T_min  0.4619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1427 before and 0.1161 after correction. The Ratio of minimum to maximum transmission is 0.8058. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       'Truncated octahedron'
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
TITL shelx     F m -3 m     R = 0.07
CELL   20.7549   20.7549   20.7549     90.00     90.00     90.00
SPGR Fm-3m
C101 0.824 0.171 0.239 !       1.88 eA-3
Q102 0.646 0.365 0.135 !       1.73 eA-3
C103 0.173 0.173 0.173 !       1.23 eA-3
C104 0.658 0.287 0.287 !       1.16 eA-3
C105 0.162 0.208 0.208 !       1.15 eA-3
C106 0.188 0.282 0.195 !       1.15 eA-3
C107 0.658 0.250 0.250 !       1.09 eA-3
C108 0.408 0.092 0.092 !       1.04 eA-3
C109 0.162 0.500 0.000 !       1.02 eA-3
C110 0.661 0.652 0.348 !       1.00 eA-3
C111 0.161 0.152 0.348 !       1.00 eA-3
C112 0.339 0.839 0.839 !       0.99 eA-3
C113 0.563 0.437 0.437 !       0.86 eA-3
C114 0.152 0.342 0.301 !       0.84 eA-3
Q115 1.000 0.499 0.234 !       0.81 eA-3
C116 0.874 0.361 0.129 !       0.79 eA-3
C117 0.301 0.144 0.144 !       0.78 eA-3
Q118 0.630 0.308 0.192 !       0.76 eA-3
Q119 0.630 0.808 0.692 !       0.76 eA-3
Q120 0.870 0.692 0.308 !       0.76 eA-3
Q121 0.183 0.808 0.880 !       0.76 eA-3
C122 0.859 0.251 0.139 !       0.74 eA-3
Q123 0.566 0.297 0.001 !       0.73 eA-3
C124 0.500 0.112 0.035 !       0.70 eA-3
C125 0.980 0.102 0.419 !       0.70 eA-3
Q126 0.098 0.236 0.125 !       0.70 eA-3
Q127 0.713 0.379 0.823 !       0.69 eA-3
Q128 0.104 0.301 0.301 !       0.67 eA-3
C129 0.119 0.400 0.121 !       0.65 eA-3
C130 0.109 0.484 0.106 !       0.64 eA-3
C131 0.731 0.262 0.238 !       0.64 eA-3
Q132 0.500 0.081 0.220 !       0.58 eA-3
Q133 0.036 0.265 0.265 !       0.58 eA-3
Q134 0.804 0.463 0.064 !       0.55 eA-3
C135 0.537 0.401 0.469 !       0.51 eA-3
;
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         608
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0508P)^2^+69.3864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                523
_reflns_number_total             608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            UiO-66_Tswing_100K1.cif
_cod_data_source_block           UiO-66_Tswing_100K1
_cod_original_cell_volume        8940.5(8)
_cod_original_formula_sum        'C42.70 H25.40 O32.04 Zr6'
_cod_database_code               4132639
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H2-O2
 0.8 with sigma of 0.01
3. Others
 Fixed Sof: O3(0.445) O2(0.08333) H2(0.08333) C1(0.2225) C2(0.2225) C3(0.445)
 H3(0.445) O1(0.08333) O3A(0.055)
 Fixed Uiso: H2(0.03) O3A(0.03)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id UiO-66_Tswing_100K1
_olex2_submission_special_instructions 'No special instructions were received'