Linker Desymmetrization: Access to a Series of Rare-Earth Tetracarboxylate Frameworks with Eight-Connected Hexanuclear Nodes
Lv, Xiu-Liang; Feng, Liang; Xie, Lin-Hua; He, Tao; Wu, Wei; Wang, Kun-Yu; Si, Guangrui; Wang, Bin; Li, Jian-Rong; Zhou, Hong-Cai; Journal of the American Chemical Society  (2021) –; doi:10.1021/jacs.0c11546

data_4135546
_publ_section_title
;
 Linker Desymmetrization: Access to a Series of Rare-Earth
 Tetracarboxylate Frameworks with Eight-Connected Hexanuclear Nodes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11546
_journal_year                    2021
_chemical_formula_sum            'C168 H84 N3 O47 Y9'
_chemical_formula_weight         3696.57
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   25.8315(2)
_cell_length_b                   25.8315(2)
_cell_length_c                   18.5628(3)
_cell_measurement_reflns_used    19980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6290
_cell_measurement_theta_min      4.1460
_cell_volume                     10726.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.1688
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            66868
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.222
_diffrn_reflns_theta_min         3.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    0.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_refine_diff_density_max         2.413
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     457
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1156
_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^)+(0.1000P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2713
_refine_ls_wR_factor_ref         0.2752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3528
_reflns_number_total             4048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11546_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4135546
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              54434
_shelx_hkl_checksum              3564
_shelx_fab_checksum              58991