Ligand Rigidification for Enhancing the Stability of Metal-Organic Frameworks.
Lv, Xiu-Liang; Yuan, Shuai; Xie, Lin-Hua; Darke, Hannah F.; Chen, Ya; He, Tao; Dong, Chen; Wang, Bin; Zhang, Yong-Zheng; Li, Jian-Rong; Zhou, Hong-Cai; Journal of the American Chemical Society 141 (2019) 10283–10293; doi:10.1021/jacs.9b02947

data_4128035
_publ_section_title
;
 Ligand Rigidification for Enhancing the Stability of Metal-Organic
 Frameworks.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10283
_journal_page_last               10293
_journal_paper_doi               10.1021/jacs.9b02947
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.13(C320 H176 O128 Zr24)'
_chemical_formula_sum            'C40 H22 O16 Zr3'
_chemical_formula_weight         1032.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.721(5)
_cell_length_b                   31.9499(15)
_cell_length_c                   34.8650(15)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    99.97(14)
_cell_measurement_theta_max      73.6350
_cell_measurement_theta_min      4.4840
_cell_volume                     21968(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega  -75.00   34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355   77.0000   30.0000 109

  2 omega -114.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355  -57.0000   90.0000 100

  3 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1259  -94.0000  150.0000 85

  4 omega   31.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1259  -30.0000  -30.0000 60

  5 omega   39.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1259  -45.0000   30.0000 55

  6 omega   61.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1259  -45.0000 -120.0000 27

  7 omega   79.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1259   30.0000   90.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0569668000
_diffrn_orient_matrix_UB_12      0.0137303000
_diffrn_orient_matrix_UB_13      -0.0275638000
_diffrn_orient_matrix_UB_21      0.0464733000
_diffrn_orient_matrix_UB_22      -0.0091755000
_diffrn_orient_matrix_UB_23      -0.0344046000
_diffrn_orient_matrix_UB_31      -0.0266137000
_diffrn_orient_matrix_UB_32      -0.0453736000
_diffrn_orient_matrix_UB_33      -0.0014934000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            16182
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.328
_diffrn_reflns_theta_min         1.727
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    0.624
_exptl_crystal_description       prism
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1076
_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          0.2795
_refine_ls_wR_factor_ref         0.3029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2784
_reflns_number_total             5624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02947_si_001.cif
_cod_data_source_block           BUT-96
_cod_database_code               4128035
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         ZrCHNO
_chemical_oxdiff_usercomment     Hongliang-P41-Zr
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.947
_reflns_odcompleteness_completeness 97.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              57202
_shelx_hkl_checksum              35541
_olex2_submission_special_instructions 'No special instructions were received'