Ligand-Directed Reticular Synthesis of Catalytically Active Missing Zirconium-Based Metal-Organic Frameworks.
Chen, Zhijie; Li, Penghao; Wang, Xingjie; Otake, Ken-Ichi; Zhang, Xuan; Robison, Lee; Atilgan, Ahmet; Islamoglu, Timur; Hall, Morgan G.; Peterson, Gregory W.; Stoddart, J. Fraser; Farha, Omar K.; Journal of the American Chemical Society 141 (2019) 12229–12235; doi:10.1021/jacs.9b06179

data_4128655
_publ_section_title
;
 Ligand-Directed Reticular Synthesis of Catalytically Active Missing
 Zirconium-Based Metal-Organic Frameworks.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12229
_journal_page_last               12235
_journal_paper_doi               10.1021/jacs.9b06179
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C88.50 H45.20 O36 Zr6'
_chemical_formula_sum            'C88.5 H45.2 O36 Zr6'
_chemical_formula_weight         2231.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-09 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.975(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   21.6317(10)
_cell_length_b                   12.2815(5)
_cell_length_c                   21.6273(10)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.71
_cell_measurement_theta_min      2.36
_cell_volume                     4977.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16957
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        54.224
_diffrn_reflns_theta_max         54.224
_diffrn_reflns_theta_min         2.358
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2014/5; Krause et al., 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.745
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.748
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         5932
_refine_ls_number_restraints     1613
_refine_ls_restrained_S_all      1.671
_refine_ls_R_factor_all          0.1602
_refine_ls_R_factor_gt           0.1328
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3947
_refine_ls_wR_factor_ref         0.4298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4046
_reflns_number_total             5932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06179_si_002.cif
_cod_data_source_block           NU-1600
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_original_formula_sum        'C88.50 H45.20 O36 Zr6'
_cod_database_code               4128655
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              78099
_shelx_hkl_checksum              89522
_shelx_fab_checksum              34892