Enriching the Reticular Chemistry Repertoire: Merged Nets Approach for the Rational Design of Intricate Mixed-Linker Metal-Organic Framework Platforms.
Jiang, Hao; Jia, Jiangtao; Shkurenko, Aleksander; Chen, Zhijie; Adil, Karim; Belmabkhout, Youssef; Weselinski, Lukasz J.; Assen, Ayalew H.; Xue, Dong-Xu; O'Keeffe, Michael; Eddaoudi, Mohamed; Journal of the American Chemical Society 140 (2018) 8858–8867; doi:10.1021/jacs.8b04745

data_4132543
_publ_section_title
;
 Enriching the Reticular Chemistry Repertoire: Merged Nets Approach for
 the Rational Design of Intricate Mixed-Linker Metal-Organic Framework
 Platforms.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8858
_journal_page_last               8867
_journal_paper_doi               10.1021/jacs.8b04745
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C2 H8 N 1+), (C174 H122 N6 O38 Tb6 2-)'
_chemical_formula_sum            'C178 H138 N8 O38 Tb6'
_chemical_formula_weight         3950.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   39.740(1)
_cell_length_b                   39.740(1)
_cell_length_c                   56.261(2)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      47.35
_cell_measurement_theta_min      2.22
_cell_volume                     88851(4)
_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_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0835
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26832
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         1.572
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.837
_exptl_absorpt_correction_T_max  0.1183
_exptl_absorpt_correction_T_min  0.0438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0483 before and 0.0329 after correction.
The Ratio of minimum to maximum transmission is 0.3702.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.591
_exptl_crystal_description       'tetragonal bipyramid'
_exptl_crystal_F_000             15648
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 3187 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.497(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.467
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         7268
_refine_ls_number_restraints     1597
_refine_ls_restrained_S_all      2.267
_refine_ls_R_factor_all          0.1430
_refine_ls_R_factor_gt           0.1404
_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          0.3705
_refine_ls_wR_factor_ref         0.3748
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                7108
_reflns_number_total             7268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04745_si_006.cif
_cod_data_source_block           Tb_sph_MOF_4
_cod_original_cell_volume        88849(6)
_cod_database_code               4132543
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.531
_shelx_estimated_absorpt_t_max   0.794
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              80983
_shelx_hkl_checksum              6148
_shelx_fab_checksum              18041