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_4132638
_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(C129.36 H81.92 O64 Zr12)'
_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                   26.6840(14)
_cell_length_b                   26.6840(14)
_cell_length_c                   26.6840(14)
_cell_measurement_reflns_used    2170
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.297
_cell_measurement_theta_min      2.869
_cell_volume                     19000.0(17)
_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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_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 APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6689
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        36.303
_diffrn_reflns_theta_max         36.303
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.4676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1071 before and 0.0744 after correction. The Ratio of minimum to maximum transmission is 0.6258. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.636
_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 110K in Fm-3m #225
CELL   26.6840   26.6840   26.6840     90.00     90.00     90.00
SPGR Fm-3m
C101 0.111 0.111 0.111 !       1.43 eA-3
C102 1.000 0.498 0.242 !       1.05 eA-3
C103 0.342 0.345 0.155 !       0.76 eA-3
C104 0.827 0.177 0.177 !       0.74 eA-3
C105 0.712 0.155 0.345 !       0.73 eA-3
C106 1.000 0.500 0.000 !       0.69 eA-3
C107 0.618 0.118 0.118 !       0.68 eA-3
C108 0.366 0.135 0.173 !       0.66 eA-3
C109 0.250 0.250 0.250 !       0.66 eA-3
C110 0.315 0.056 0.056 !       0.65 eA-3
C111 0.521 0.027 0.209 !       0.62 eA-3
C112 0.500 0.074 0.166 !       0.58 eA-3
Q113 0.500 0.504 0.109 !       0.56 eA-3
C114 0.828 0.172 0.328 !       0.53 eA-3
C115 0.322 0.093 0.093 !       0.53 eA-3
;
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         280
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0425P)^2^+414.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                246
_reflns_number_total             280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uio-67_22defect_DMF_100K.cif
_cod_data_source_block           UiO-67_22defect_DMF_100K
_cod_original_cell_volume        19000(3)
_cod_original_formula_sum        'C64.50 H41 O28.50 Zr6'
_cod_database_code               4132638
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O0AA-Zr1
 2.18 with sigma of 0.02
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3 \\sim C4 \\sim C5 \\sim C2: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O2) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) = Uanis(O1)
5. Others
 Fixed Sof: O3(0.385) C1(0.1925) C2(0.1925) C5(0.1925) C3(0.385) H3(0.385)
 C4(0.385) H4(0.385) O1(0.08333) O2(0.08333) H2(0.08333) O0AA(0.115)
 Fixed Uiso: H2(0.1) O0AA(0.1)
 Fixed X: H2(1.067301)
 Fixed Y: H2(0.567301)
 Fixed Z: H2(0.567301)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id UiO-67_22defect_DMF_100K
_olex2_submission_special_instructions 'No special instructions were received'