Postsynthetic Metalation of a Robust Hydrogen-Bonded Organic Framework for Heterogeneous Catalysis.
Han, Bin; Wang, Hailong; Wang, Chiming; Wu, Hui; Zhou, Wei; Chen, Banglin; Jiang, Jianzhuang; Journal of the American Chemical Society 141 (2019) 8737–8740; doi:10.1021/jacs.9b03766

data_4127582
_publ_section_title
;
 Postsynthetic Metalation of a Robust Hydrogen-Bonded Organic Framework
 for Heterogeneous Catalysis.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8737
_journal_page_last               8740
_journal_paper_doi               10.1021/jacs.9b03766
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C21 H12 N12 O6'
_chemical_formula_weight         528.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.212(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0932(15)
_cell_length_b                   8.0164(4)
_cell_length_c                   20.0514(18)
_cell_measurement_reflns_used    2255
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      71.6120
_cell_measurement_theta_min      4.5420
_cell_volume                     3581.9(5)
_computing_cell_refinement       'SAINT [9]'
_computing_data_collection       'SMART [9]'
_computing_data_reduction        SAINT[9]
_computing_molecular_graphics    'SHELXL-2014 [10]'
_computing_structure_refinement  'SHELXL-2014 [10]'
_computing_structure_solution    'SHELXL-2014 [10]'
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean 5.1688
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5603
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        62.976
_diffrn_reflns_theta_max         62.976
_diffrn_reflns_theta_min         3.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1375P)^2^+2.0922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2400
_reflns_number_total             3110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03766_si_002.cif
_cod_data_source_block           HOF-19
_cod_database_code               4127582
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              95567
_shelx_hkl_checksum              2335