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_7132311
_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         'C138 H138 N48 Pb6, 9(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C153 H147 F27 N51 O27 Pb6 S9'
_chemical_formula_weight         5176.89
_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_date             2023-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-28 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                   21.0331(2)
_cell_length_b                   21.0331(2)
_cell_length_c                   58.2510(12)
_cell_measurement_reflns_used    70615
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1.32
_cell_volume                     22317.2(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            'EIGER 2R 1M CDTE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            107507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_min         1.319
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.4
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7551
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         14376
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0931P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8067
_reflns_number_total             14376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           3-r-3
_cod_original_cell_volume        22317.2(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7132311
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.570
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C22 = C21-C23 = C21-C22A = C21-C23A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O4) = Uanis(O5)
Uanis(F3) = Uanis(F4) = Uanis(F5)
4. Others
 Fixed Sof: C22(0.7) H22(0.7) C23(0.7) H23(0.7) C22A(0.3) H22A(0.3) C23A(0.3)
 H23A(0.3) N8(0.5) C00D(0.5) H00A(0.5) H00B(0.5) H00C(0.5) C29(0.5) O2(0.5)
 C24(0.16666) F2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C11(H11), C16(H16), C17(H17), C19(H19),
 C20(H20), C22(H22), C23(H23), C22A(H22A), C23A(H23A)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C00D(H00A,H00B,H00C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 2367 electrons were 
found in a volume of 9246\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[(CF3SO3)], 18[(CH3CN)] per Formula Unit 
which account for 2367 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80575
_shelx_fab_checksum              64775
_olex2_submission_special_instructions 'No special instructions were received'