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_4132641
_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
'0.33(C360 H216 O96 Zr18), 0.33(C72 O19.2 Zr3.6)'
_chemical_formula_sum            'C144 H72 O38.4 Zr7.2'
_chemical_formula_weight         3073.20
_chemical_name_systematic        MOF-1005
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-23
_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            3
_cell_length_a                   38.764(3)
_cell_length_b                   38.764(3)
_cell_length_c                   38.764(3)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.50
_cell_volume                     58249(8)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      290.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_wavelength     1.1271
_diffrn_reflns_av_R_equivalents  0.1584
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            124988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.666
_diffrn_reflns_theta_max         24.666
_diffrn_reflns_theta_min         0.833
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.4190
_exptl_absorpt_correction_T_min  0.3307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1624 before and 0.1367 after correction. The Ratio of minimum to maximum transmission is 0.7893. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.263
_exptl_crystal_description       'The crystal has rhombic dodecahedron shape'
_exptl_crystal_F_000             4594
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL shelx     P m -3 m     R = 0.28
CELL   38.7640   38.7640   38.7640     90.00     90.00     90.00
SPGR Pm-3m
C101 0.500 0.497 0.203 !       1.09 eA-3
C102 0.500 0.070 0.363 !       1.07 eA-3
C103 0.847 0.504 0.844 !       1.05 eA-3
C104 0.023 0.023 0.023 !       1.02 eA-3
C105 0.500 0.500 0.500 !       0.94 eA-3
Q106 0.500 0.937 0.155 !       0.93 eA-3
C107 0.500 0.657 0.108 !       0.89 eA-3
Q108 0.950 0.956 0.387 !       0.87 eA-3
Q109 0.366 1.001 0.453 !       0.83 eA-3
C110 0.668 0.999 0.102 !       0.79 eA-3
Q111 0.855 0.954 0.401 !       0.78 eA-3
C112 0.066 0.024 0.024 !       0.78 eA-3
C113 0.066 0.066 0.066 !       0.76 eA-3
C114 0.750 0.750 0.750 !       0.71 eA-3
C115 1.000 0.289 0.002 !       0.65 eA-3
Q116 0.565 0.888 0.112 !       0.61 eA-3
Q117 1.000 0.098 0.455 !       0.60 eA-3
C118 0.553 0.553 0.553 !       0.57 eA-3
C119 0.354 0.393 0.351 !       0.54 eA-3
C120 0.500 0.503 0.156 !       0.53 eA-3
C121 0.915 0.916 0.962 !       0.53 eA-3
;
_refine_diff_density_max         0.763
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      2.230
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.1560
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4181
_refine_ls_wR_factor_ref         0.4636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1879
_reflns_number_total             2479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-1005_290K1_DMF.cif
_cod_data_source_block           MOF-1005_290K_DMF
_cod_original_cell_volume        58246(12)
_cod_original_formula_sum        'C144 H72 O38.40 Zr7.20'
_cod_database_code               4132641
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O2A-O4A
 -2.2 with sigma of 0.02
 C2A-C1A
 1.45 with sigma of 0.02
 C8A-C7A
 1.45 with sigma of 0.02
 C15A_$1-C13A
 1.45 with sigma of 0.02
 C12A-C10A
 1.35 with sigma of 0.02
 C11A_$3-C12A_$3
 1.5 with sigma of 0.02
 C9A_$3-C10A_$3
 1.5 with sigma of 0.02
 Zr1-O1
 -2 with sigma of 0.02
 C3A-C7A
 2.4 with sigma of 0.04
 C5A-C6A
 2.4 with sigma of 0.04
 C7A-C4A
 2.4 with sigma of 0.04
 C3A-C4A
 2.4 with sigma of 0.04
 C15A-C15A_$1
 2.4 with sigma of 0.04
 C14A-C14A_$2
 2.4 with sigma of 0.04
 C2A-C5A
 2.4 with sigma of 0.04
 C6A-C2A
 2.4 with sigma of 0.04
 C9A-C13A
 2.4 with sigma of 0.04
 C8A-C12A
 2.4 with sigma of 0.04
 C10A-C13A
 2.4 with sigma of 0.04
 C8A-C11A
 2.4 with sigma of 0.04
 Zr1A-O2A \\sim Zr2A-O4A
 with sigma of 0.02
 C2A-C3A \\sim C5A-C7A \\sim C6A-C4A
 with sigma of 0.02
 C3A-C1A \\sim C1A-C4A
 with sigma of 0.02
 O2A-C1A \\sim C1A-O4A
 with sigma of 0.02
 C5A-C8A \\sim C8A-C6A
 with sigma of 0.02
 C8A-C10A \\sim C12A-C13A
 with sigma of 0.02
 C8A-C9A \\sim C11A-C13A
 with sigma of 0.02
 C9A-C11A \\sim C10A-C12A
 with sigma of 0.02
 O3-C1 \\sim C1-O4
 with sigma of 0.02
3. Restrained planarity
 C13A, C15A_$1, C14A, C15A, C14A_$2
 with sigma of 0.1
 C8A, C10A, C12A, C13A
 with sigma of 0.1
 C8A, C9A, C11A, C13A
 with sigma of 0.1
4. Rigid bond restraints
 C5, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, Zr2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, Zr1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C10 \\sim C8 \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C9 \\sim C11 \\sim C13 \\sim C12 \\sim C8 \\sim C10: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O4) = Uanis(O3)
6. Others
 Fixed Sof: C10(0.5) H10(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5) C9(0.5)
 H9(0.5) Zr2A(0.025) Zr1A(0.05) O4A(0.1) O3A(0.1) O2A(0.1) C1A(0.1) C5A(0.1)
 C2A(0.1) C7A(0.1) C3A(0.1) C6A(0.1) C4A(0.1) C8A(0.1) C14A(0.1) C9A(0.1)
 C15A(0.1) C11A(0.1) C13A(0.1) C12A(0.1) C10A(0.1) O1A(0.1)
 Fixed Uiso: O3A(0.2) C7A(0.2) C3A(0.2) C6A(0.2) C4A(0.2) C14A(0.2) C15A(0.2)
 O1A(0.2)
 Fixed X: O1(0.541881)
 Fixed Y: O1(0)
 Fixed Z: O1(0.603181)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C3(H3), C6(H6), C10(H10), C12(H12), C11(H11), C9(H9), C15(H15)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id MOF-1005_260K_DMF
_olex2_submission_special_instructions 'No special instructions were received'