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_7719941
_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 K5 O52.6 Si W11'
_chemical_formula_weight         3747.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_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                 104.9130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3953(16)
_cell_length_b                   11.5329(8)
_cell_length_c                   27.827(2)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.22
_cell_volume                     6945.2(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            41261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.943
_diffrn_reflns_theta_min         1.515
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    22.403
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.584
_exptl_crystal_description       block
_exptl_crystal_F_000             6539
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.047
_refine_diff_density_max         4.018
_refine_diff_density_min         -4.354
_refine_diff_density_rms         0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8666
_refine_ls_number_restraints     608
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0675
_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^)+1445.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7971
_reflns_number_total             8666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02418h2.cif
_cod_data_source_block           Ir2SiW11
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C20 Cl Ir2 K5 O52.60 Si W11'
_cod_database_code               7719941
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              85789
_shelx_hkl_checksum              3054