Enriching the Reticular Chemistry Repertoire with Minimal Edge-Transitive Related Nets: Access to Highly Coordinated Metal-Organic Frameworks Based on Double Six-Membered Rings as Net-Coded Building Units.
Chen, Zhijie; Thiam, Zeynabou; Shkurenko, Aleksander; Weselinski, Lukasz J.; Adil, Karim; Jiang, Hao; Alezi, Dalal; Assen, Ayalew H.; O'Keeffe, Michael; Eddaoudi, Mohamed; Journal of the American Chemical Society 141 (2019) 20480–20489; doi:10.1021/jacs.9b11260

data_4133796
_publ_section_title
;
 Enriching the Reticular Chemistry Repertoire with Minimal Edge-Transitive
 Related Nets: Access to Highly Coordinated Metal-Organic Frameworks Based
 on Double Six-Membered Rings as Net-Coded Building Units.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20480
_journal_page_last               20489
_journal_paper_doi               10.1021/jacs.9b11260
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '5(C2 H8 N 1+), (C132 H120 N24 O73 Tb15 5-)'
_chemical_formula_sum            'C142 H160 N29 O73 Tb15'
_chemical_formula_weight         5824.78
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   22.7138(9)
_cell_length_b                   22.7138(9)
_cell_length_c                   50.592(3)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      66.47
_cell_measurement_theta_min      2.85
_cell_volume                     22604.4(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0338
_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       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            119532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        61.159
_diffrn_reflns_theta_max         61.159
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    11.596
_exptl_absorpt_correction_T_max  0.1009
_exptl_absorpt_correction_T_min  0.0144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.1427.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.856
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             5548
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.661
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0846
_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          0.2713
_refine_ls_wR_factor_ref         0.2785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5171
_reflns_number_total             6379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11260_si_005.cif
_cod_data_source_block           Tb_urx_MOF_1
_cod_depositor_comments
'Adding full bibliography for 4133792--4133796.cif.'
_cod_original_cell_volume        22604(2)
_cod_database_code               4133796
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.205
_shelx_estimated_absorpt_t_max   0.722
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              63458
_shelx_hkl_checksum              53512
_shelx_fab_checksum              49854