Reaction of a Cp*Ir(III) Cation with mono-and di-lacunary Keggintype heterpolytungstates, and dimer of hexa-lacunary Dawsontype phosphopolytungstate
Sugiarto, Sugiarto; Shinogi, Jun; Ebied, Sherif E.; Hong, Dachao; Kon, Yoshihiro; Sadakane, Masahiro; Dalton Transactions  (2025) –; doi:10.1039/D5DT02418H

data_7719940
_publ_section_title
;
 Reaction of a Cp*Ir(III) Cation with mono-and di-lacunary Keggintype
 heterpolytungstates, and dimer of hexa-lacunary Dawsontype
 phosphopolytungstate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02418H
_journal_year                    2025
_chemical_formula_sum            'C40 H60 Ir4 K23 O156 Si4 W40'
_chemical_formula_weight         12171.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-20 deposited with the CCDC.	2025-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.071(3)
_cell_length_b                   31.071(3)
_cell_length_c                   15.191(2)
_cell_measurement_reflns_used    8962
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.38
_cell_volume                     14665(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35539
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.420
_diffrn_reflns_theta_min         1.492
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    17.830
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_description       block
_exptl_crystal_F_000             10618
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.093
_refine_diff_density_max         3.743
_refine_diff_density_min         -3.187
_refine_diff_density_rms         0.366
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         13480
_refine_ls_number_restraints     515
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+794.9680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10984
_reflns_number_total             13480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02418h2.cif
_cod_data_source_block           IrSiW10_sq
_cod_database_code               7719940
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              15254
_shelx_hkl_checksum              81107
_shelx_fab_checksum              71269