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_7719942
_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            'C20 Cl Ir2 K3.4 O47.63 P W11'
_chemical_formula_weight         3608.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_audit_creation_method           SHELXL-2014/7
_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            8
_cell_length_a                   35.1781(13)
_cell_length_b                   35.1781(13)
_cell_length_c                   11.3965(6)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.21
_cell_volume                     14103.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41257
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         1.637
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    21.966
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.399
_exptl_crystal_description       block
_exptl_crystal_F_000             12525
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.426
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8541
_refine_ls_number_restraints     741
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+1044.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6792
_reflns_number_total             8541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02418h2.cif
_cod_data_source_block           IrPW11_sq
_cod_original_cell_volume        14103.2(13)
_cod_original_formula_sum        'C20 Cl Ir2 K3.40 O47.63 P W11'
_cod_database_code               7719942
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              44219
_shelx_hkl_checksum              29279
_shelx_fab_checksum              13881