Anion-encapsulating, discrete prism and extended frusta, from trimetallated triangular macrocycles and linkers.
Wang, Hai-Ping; Eichhöfer, Andreas; Gu, Zhi-Gang; Gruber, Nathalie; Stadler, Adrian-Mihail; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc00137g

data_7132313
_publ_section_title
;
 Anion-encapsulating, discrete prism and extended frusta, from
 trimetallated triangular macrocycles and linkers.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc00137g
_journal_year                    2023
_chemical_formula_moiety
'C126 H132 N48 Pb6, 9(C F3 O3 S), 6(C F1.5 O1.5 S0.5)'
_chemical_formula_sum            'C141 H132 F36 N48 O36 Pb6 S12'
_chemical_formula_weight         5386.80
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-11-02 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.1054(2)
_cell_length_b                   21.1054(2)
_cell_length_c                   51.1319(10)
_cell_measurement_reflns_used    61587
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.14
_cell_measurement_theta_min      2.23
_cell_volume                     19724.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3(Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            93267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         64.473
_diffrn_reflns_theta_min         2.233
_exptl_absorpt_coefficient_mu    6.185
_exptl_absorpt_correction_T_max  0.577
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7830
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.155
_refine_diff_density_min         -3.416
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         11021
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.003
_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          0.2498
_refine_ls_wR_factor_ref         0.2730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7300
_reflns_number_total             11021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7132313
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.577
_shelx_res_checksum              17913