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_7132310
_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         'C120 H126 N48 Pb6, 12(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C138 H135 F36 N51 O36 Pb6 S12'
_chemical_formula_weight         5395.82
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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            2
_cell_length_a                   21.0549(6)
_cell_length_b                   21.0549(6)
_cell_length_c                   31.7103(14)
_cell_measurement_reflns_used    40636
_cell_measurement_temperature    150
_cell_measurement_theta_max      63.98
_cell_measurement_theta_min      2.43
_cell_volume                     12174.1(7)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            Dectris
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.952
_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  0.0964
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51469
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         64.052
_diffrn_reflns_theta_min         2.108
_exptl_absorpt_coefficient_mu    6.457
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_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    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.250
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9933
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5261
_reflns_number_total             9933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           1-p63m
_cod_original_cell_volume        12174.1(9)
_cod_database_code               7132310
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.444
_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
 C24-F6 = C24-F7
 1.33 with sigma of 0.02
 C22-S2
 1.85 with sigma of 0.02
 C24-S4
 1.85 with sigma of 0.02
 C22-F2
 1.33 with sigma of 0.02
 S3-C23
 1.82 with sigma of 0.02
 C23-F3 = C23-F4 = C23-F5
 1.33 with sigma of 0.02
 C22-O2
 2.578 with sigma of 0.04
 S3-O3 \\sim S3-O4 \\sim S3-O5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F7)
Uanis(F3) = Uanis(F4) = Uanis(F5)
Uanis(O3) = Uanis(O4) = Uanis(O5)
4. Others
 Fixed Sof: F2(0.5) O2(0.5) C22(0.16666) N9(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C16(H16), C17(H17), C19(H19),
 C20(H20)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17904
_shelx_fab_checksum              42589
_olex2_submission_special_instructions 'No special instructions were received'