Halide-triggered assembly and selective bisulfate recognition in a quadruply interlocked coordination cage.
Virtue, Jemma I.; Tsoukatos, Steven; Johnston, Martin R.; Bloch, Witold M.; Chemical science 15 (2024) 19119–19125; doi:10.1039/d4sc04913f

data_1572939
_publ_section_title
;
 Halide-triggered assembly and selective bisulfate recognition in a
 quadruply interlocked coordination cage.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              19119
_journal_page_last               19125
_journal_paper_doi               10.1039/d4sc04913f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'(C84 H56 N24 Pd)2, (B F4)7, Br, (C H Cl3)9, (C2 H3 N)5'
_chemical_formula_sum            'C187 H136 B7 Br Cl27 F28 N53 Pd4'
_chemical_formula_weight         5195.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.864(3)
_cell_length_b                   57.355(12)
_cell_length_c                   27.051(5)
_cell_measurement_reflns_used    12570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      0.74
_cell_volume                     23062(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            108068
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         0.710
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             10376
_exptl_crystal_recrystallization_method 'slow vapour diffusion'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.18(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1743
_refine_ls_number_reflns         16236
_refine_ls_number_restraints     4175
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0784
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2491
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                12659
_reflns_number_total             16236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04913f2.cif
_cod_data_source_block           Br_2
_cod_depositor_comments
'Adding full bibliography for 1572937--1572941.cif.'
_cod_database_code               1572939
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              34332
_shelx_fab_checksum              94206