Porous metal‒organic frameworks based on 3,6-bis(4-benzoic acid)-N-(4-benzoic acid)carbazole for HPLC separation of small organic molecules
Chen, Dong-Hui; Zhuo, Chao; Wen, Yue-Hong; Lin, Ling; Zhang, Yu-Xiao; Hu, Sheng-Min; Fu, Rui-Biao; Wu, Xin-Tao; Materials Chemistry Frontiers 2 (2018) 1508–; doi:10.1039/C8QM00147B

data_1554216
_publ_section_title
;
 Porous metal--organic frameworks based on 3,6-bis(4-benzoic
 acid)-N-(4-benzoic acid)carbazole for HPLC separation of small organic
 molecules
;
_journal_issue                   8
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              1508
_journal_paper_doi               10.1039/C8QM00147B
_journal_volume                  2
_journal_year                    2018
_chemical_formula_sum            'C39 H25 Cu1.5 N2.5 O6'
_chemical_formula_weight         719.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           137
_space_group_name_Hall           '-P 4ac 2a'
_space_group_name_H-M_alt        'P 42/n m c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.8272(3)
_cell_length_b                   31.8272(3)
_cell_length_c                   27.8945(8)
_cell_measurement_reflns_used    12617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.5550
_cell_measurement_theta_min      4.1460
_cell_volume                     28256.3(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60043
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.529
_diffrn_reflns_theta_min         3.460
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    0.677
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.185
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         14706
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0985
_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^)+(0.2650P)^2^+0.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3260
_refine_ls_wR_factor_ref         0.3548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10076
_reflns_number_total             14706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qm00147b2.cif
_cod_data_source_block           YCZ-1
_cod_original_cell_volume        28256.3(10)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_original_formula_sum        'C39 H25 Cu1.50 N2.50 O6'
_cod_database_code               1554216
_shelx_shelxl_version_number     2018/1
_platon_squeeze_void_probe_radius 1.20
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.867
_shelx_res_checksum              26033
_shelx_hkl_checksum              88876