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_4128036
_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         '0.5(C368 H272 O128 Zr24)'
_chemical_formula_sum            'C184 H136 O64 Zr12'
_chemical_formula_weight         4465.56
_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
_atom_sites_solution_primary     iterative
_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            2
_cell_length_a                   21.1397(9)
_cell_length_b                   32.4825(8)
_cell_length_c                   33.8974(9)
_cell_measurement_reflns_used    8682
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3810
_cell_measurement_theta_min      4.1190
_cell_volume                     23276.3(13)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -50.00   32.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355   38.0000  120.0000 82

  2 omega  -75.00   34.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355   77.0000    0.0000 109

  3 omega   23.00   98.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.9355 -125.0000  -90.0000 75

  4 omega   30.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -77.0000  -90.0000 108

  5 omega   33.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -45.0000    0.0000 65

  6 omega   30.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000  -60.0000 61

  7 omega   30.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000 -180.0000 61

  8 omega   30.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000  150.0000 61

  9 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000 -120.0000 84

 10 omega -118.00  -53.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355  -77.0000  150.0000 65

 11 omega -118.00   -9.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.9355  -77.0000   30.0000 109
;
_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      -0.0363031000
_diffrn_orient_matrix_UB_12      0.0385482000
_diffrn_orient_matrix_UB_13      -0.0138518000
_diffrn_orient_matrix_UB_21      0.0204448000
_diffrn_orient_matrix_UB_22      0.0228959000
_diffrn_orient_matrix_UB_23      0.0377536000
_diffrn_orient_matrix_UB_31      0.0596717000
_diffrn_orient_matrix_UB_32      0.0155675000
_diffrn_orient_matrix_UB_33      -0.0212424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            28871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.769
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52892
_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.'
_exptl_crystal_density_diffrn    0.637
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         2.086
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         5504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4439
_reflns_number_total             5504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02947_si_001.cif
_cod_data_source_block           BUT-97
_cod_database_code               4128036
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHONZr
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H00D(0.5) H00E(0.5) H00G(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00H(H00H), C00J(H00J), C00K(H00K)
3.b Idealised Me refined as rotating group:
 C00E(H00A,H00B,H00C), C00L(H00D,H00E,H00G)
;
_shelx_res_checksum              38322
_shelx_hkl_checksum              25154
_olex2_submission_special_instructions 'No special instructions were received'