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_4128033
_publ_section_title
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 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_sum            'C168 H90 O24 Zr9'
_chemical_formula_weight         3313.37
_space_group_crystal_system      hexagonal
_space_group_IT_number           189
_space_group_name_Hall           'P -6 -2'
_space_group_name_H-M_alt        'P -6 2 m'
_symmetry_space_group_name_Hall  'P -6 -2'
_symmetry_space_group_name_H-M   'P -6 2 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   23.0014(4)
_cell_length_b                   23.0014(4)
_cell_length_c                   18.5185(5)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.5570
_cell_measurement_theta_min      3.8230
_cell_volume                     8484.9(3)
_computing_cell_refinement
; 
'Mon Sep 12 15:35:43 2016' 
;
_computing_data_collection
; 
'Mon Sep 12 15:35:43 2016' 
;
_computing_data_reduction
; 
'Mon Sep 12 15:35:43 2016' 
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3376
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.825
_diffrn_reflns_theta_min         3.843
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'Mon Sep 12 15:35:43 2016' 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.648
_exptl_crystal_description
; 
'Mon Sep 12 15:35:43 2016' 
;
_exptl_crystal_F_000             1650
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.445
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
; 
 Refined as a perfect inversion twin. 
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.0106(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         5719
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1621
_refine_ls_R_factor_gt           0.1346
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3414
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3746
_reflns_number_total             5719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02947_si_001.cif
_cod_data_source_block           BUT-93
_cod_original_cell_volume        8484.9(4)
_cod_database_code               4128033
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.618
_shelx_estimated_absorpt_t_max   0.713
_shelx_res_checksum              26671
_shelx_hkl_checksum              50196
_shelx_fab_checksum              46084