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_4133792
_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+), (C138 H140 Dy15 N26 Na2 O79 5-)'
_chemical_formula_sum            'C148 H180 Dy15 N31 Na2 O79'
_chemical_formula_weight         6140.70
_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                   22.6832(9)
_cell_length_b                   22.6832(9)
_cell_length_c                   50.192(2)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      52.00
_cell_measurement_theta_min      2.86
_cell_volume                     22365.3(15)
_computing_cell_refinement       'SAINT v7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker AXS Inc., 2009)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_structure_refinement  'SHELXS (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            37585
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        35.112
_diffrn_reflns_theta_max         52.722
_diffrn_reflns_theta_min         1.760
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    13.508
_exptl_absorpt_correction_T_max  0.1263
_exptl_absorpt_correction_T_min  0.0225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1562 before and 0.0991 after correction.
The Ratio of minimum to maximum transmission is 0.1781.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.912
_exptl_crystal_description       'thin hexagonal plate'
_exptl_crystal_F_000             5858
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.765
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4581
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.865
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.1350
_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          0.4270
_refine_ls_wR_factor_ref         0.4365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3539
_reflns_number_total             4581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11260_si_006.cif
_cod_data_source_block           Dy_urx_MOF_1
_cod_depositor_comments
'Adding full bibliography for 4133792--4133796.cif.'
_cod_original_cell_volume        22365(2)
_cod_database_code               4133792
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.140
_shelx_estimated_absorpt_t_max   0.774
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              15545
_shelx_hkl_checksum              15323
_shelx_fab_checksum              80478