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_4132637
_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
_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                   41.367(5)
_cell_length_b                   41.367(5)
_cell_length_c                   41.367(5)
_cell_measurement_reflns_used    41831
_cell_measurement_temperature    290
_cell_measurement_theta_max      24.660
_cell_measurement_theta_min      2.469
_cell_volume                     70788(15)
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.1271
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84837
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.660
_diffrn_reflns_theta_max         24.660
_diffrn_reflns_theta_min         2.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.2061 before and 0.0514 after correction. The Ratio of minimum to maximum transmission is 0.8928. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    0.370
_exptl_crystal_description
'The crystal has rhombic dodecahedron shape and is colorless.'
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.026
_refine_ls_extinction_coef       0.000023(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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2703
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0692P)^2^+72.4640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2294
_reflns_number_total             2703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-1004_290K1_DMF.cif
_cod_data_source_block           mof-1004_dmf_290k1_sq
_cod_original_cell_volume        70788(25)
_cod_database_code               4132637
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8-C7
 1.47 with sigma of 0.02
 C9-C10
 1.47 with sigma of 0.02
 C14-C13
 1.47 with sigma of 0.02
 C15-C16
 1.47 with sigma of 0.02
 C14-C15
 1.16 with sigma of 0.02
 C9-C8
 1.16 with sigma of 0.02
3. Restrained planarity
 C6, C7, C8, C9, C10, C12
 with sigma of 0.2
 C12, C13, C14, C15, C16, C17
 with sigma of 0.2
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C6) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Fixed Uiso: H2(0.05)
 Fixed X: H2(0.06744)
 Fixed Y: H2(0.70303)
 Fixed Z: H2(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C12(H12), C17(H17), C11(H11), C6(H6), C5(H5), C3(H3), C4(H4)
6.b Fitted hexagon refined as free rotating group:
 C6(C7,C5,C3,C2,C4)
;
_shelx_res_checksum              39551
_shelx_hkl_checksum              1398
_shelx_fab_checksum              22090
_olex2_submission_original_sample_id MOF-1004_DMF_290K1
_olex2_submission_special_instructions 'No special instructions were received'