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_4132634
_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         '0.17(C792 H384 O192 Zr36)'
_chemical_formula_sum            'C132 H64 O27 Zr6'
_chemical_formula_weight         2629.15
_chemical_name_systematic        MOF-1004_100K_DMf
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   mixed
_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            6
_cell_length_a                   40.561(6)
_cell_length_b                   40.561(6)
_cell_length_c                   40.561(6)
_cell_measurement_reflns_used    6263
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      19.90
_cell_measurement_theta_min      2.252
_cell_volume                     66731(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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.1271
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41442
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        18.342
_diffrn_reflns_theta_max         18.342
_diffrn_reflns_theta_min         2.252
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1447 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.8728. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.393
_exptl_crystal_description       'The crystal has rhombic dodecahedron shape'
_exptl_crystal_F_000             7872
_exptl_crystal_preparation
'synthesized crystals were evacuated and charged with DMF.'
_exptl_crystal_recrystallization_method 'See supporting information'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL 100K_plbg_135 in Pm-3n #223
CELL   40.5610   40.5610   40.5610     90.00     90.00     90.00
SPGR Pm-3n
C101 1.000 0.181 0.390 !       1.05 eA-3
C102 0.500 0.140 0.125 !       0.91 eA-3
C103 0.852 0.328 0.503 !       0.87 eA-3
C104 0.250 0.250 0.250 !       0.80 eA-3
C105 0.500 0.998 0.078 !       0.79 eA-3
Q106 0.750 0.548 0.048 !       0.77 eA-3
C107 0.500 0.628 0.046 !       0.72 eA-3
C108 1.000 0.501 0.336 !       0.71 eA-3
C109 1.000 0.497 0.375 !       0.70 eA-3
C110 0.092 0.406 0.252 !       0.67 eA-3
C111 0.272 0.949 0.429 !       0.55 eA-3
C112 0.619 0.117 0.252 !       0.51 eA-3
C113 0.757 1.000 0.414 !       0.50 eA-3
;
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.117
_refine_diff_density_rms         0.022
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1121
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0660
_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^)+(0.1492P)^2^+144.6241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                664
_reflns_number_total             1121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-1004_100K_DMF.cif
_cod_data_source_block           MOF-1004_100K_DMF
_cod_original_cell_volume        66731(31)
_cod_database_code               4132634
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 C7-C8
 1.47 with sigma of 0.02
 C13-C14
 1.47 with sigma of 0.02
 C19-C20
 -1.2 with sigma of 0.02
 C14-C15
 1.16 with sigma of 0.04
 C15-C16
 1.47 with sigma of 0.04
 C8-C9
 1.16 with sigma of 0.02
 C10-C9
 1.47 with sigma of 0.02
 C9-C10
 1.47 with sigma of 0.02
 C10-C11
 -1.3 with sigma of 0.02
 C1-C2
 1.45 with sigma of 0.01
 Zr1_$2-O5
 -2.1 with sigma of 0.02
 C17-C19
 2.4 with sigma of 0.04
 C12-C11
 2.4 with sigma of 0.04
 C12-C13
 2.8 with sigma of 0.04
 C17-C17_$1
 2.4 with sigma of 0.04
 C16-C18
 2.4 with sigma of 0.04
 C16-C19
 2.8 with sigma of 0.04
 C10-C13
 2.4 with sigma of 0.04
 O5-O5_$1
 2.4 with sigma of 0.04
 C6-C8 \\sim C8-C5
 with sigma of 0.02
 C4-C1 \\sim C1-C3
 with sigma of 0.02
 C16-C17 \\sim C18-C19
 with sigma of 0.02
 C12-C10 \\sim C11-C13
 with sigma of 0.02
3. Restrained planarity
 O5, C20, C19, O5_$1
 with sigma of 0.1
 C11, C14, C15, C16
 with sigma of 0.2
 C16, C17, C18, C19
 with sigma of 0.1
 C12, C10, C11, C13
 with sigma of 0.1
4. Rigid bond restraints
 C1, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr2, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr1, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr2, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, Zr1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C4 \\sim C6 \\sim C7 \\sim C5 \\sim C3 \\sim C2: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C10 \\sim C11 \\sim C13 \\sim C12: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C9) = Uanis(C8)
6. Rigid body (RIGU) restrains
 C9, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed X: H2(0.06403)
 Fixed Y: H2(0.70228)
 Fixed Z: H2(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C5(H5), C3(H3), C4(H4), C12(H12), C17(H17), C18(H18)
8.b Fitted hexagon refined as free rotating group:
 C6(C7,C5,C3,C2,C4)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_exptl_crystal_mounting_method
'The prepared crystal was mounted on the goniometer with mineral oil'
_olex2_submission_original_sample_id MOF-1004_100K_DMF
_olex2_submission_special_instructions 'No special instructions were received'