A pair of conjoined trinuclear sub-frameworks in a pentanuclear double-cavity discrete coordination cage.
Sharma, Shruti; Krishnaswamy, Shobhana; Prusty, Soumyakanta; Chand, Dillip Kumar; Chemical science 15 (2024) 11287–11301; doi:10.1039/d4sc01078g

data_1572012
_publ_section_title
;
 A pair of conjoined trinuclear sub-frameworks in a pentanuclear
 double-cavity discrete coordination cage.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11287
_journal_page_last               11301
_journal_paper_doi               10.1039/d4sc01078g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C224 H168 N29 O83 Pd5 S6'
_chemical_formula_weight         5318.22
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.82(6)
_cell_length_b                   40.82(6)
_cell_length_c                   24.82(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.816
_cell_measurement_theta_min      2.71
_cell_volume                     41357(11)
_computing_cell_refinement       'APEX4/SAINT (Bruker, 2021)'
_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2021)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012), Mercury'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019), WinGX'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker D8 Venture Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2402
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            212853
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        16.223
_diffrn_reflns_theta_max         16.223
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.7141
_exptl_absorpt_correction_T_min  0.5199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.854
_exptl_crystal_description       block
_exptl_crystal_F_000             10820
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1364
_refine_ls_number_reflns         10237
_refine_ls_number_restraints     2815
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.1068
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_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          0.2758
_refine_ls_wR_factor_ref         0.3308
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                7328
_reflns_number_total             10237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01078g2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1572011--1572013.cif.'
_cod_original_cell_volume        41350(131)
_cod_database_code               1572012
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              68217
_shelx_fab_checksum              5933