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_7132315
_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
'2(C67 H66 F12 N24 O12 Pb3 S4), F6 P [+ solvent]'
_chemical_formula_sum            'C134 H132 F30 N48 O24 P Pb6 S8 en lv so t'
_chemical_formula_weight         4899.46
_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-2018/3
_audit_update_record
;
2023-09-07 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                   21.1133(6)
_cell_length_b                   21.1133(6)
_cell_length_c                   51.250(3)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.27
_cell_volume                     19785.0(14)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            117507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.929
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7107
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+121.8275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8716
_reflns_number_total             10519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           2PF6
_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_original_cell_volume        19784.9(15)
_cod_original_formula_sum        'C134 H132 F30 N48 O24 P Pb6 S8,solvent'
_cod_database_code               7132315
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              88115
_shelx_fab_checksum              65788