Bis(iminoxolene)iridium complexes over four oxidation states: from sodium-iridium bonding to ligand-centered radicals.
Nugraha, Kahargyan; Do, Thomas H.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5896–5905; doi:10.1039/d5dt00244c

data_7718299
_publ_section_title
;
 Bis(iminoxolene)iridium complexes over four oxidation states: from
 sodium-iridium bonding to ligand-centered radicals.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5896
_journal_page_last               5905
_journal_paper_doi               10.1039/d5dt00244c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H46 Br4 Ir N2 O2, 2(C H Cl3)'
_chemical_formula_sum            'C42 H48 Br4 Cl6 Ir N2 O2'
_chemical_formula_weight         1337.36
_chemical_name_common            '(Briq)2Ir . 2 CHCl3'
_chemical_name_systematic
'Bis(N-(2,6-dibromophenyl)-4,6-di-tert-butyliminoxolene)-iridium di-chloroform solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2025-01-19 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7892(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6386(4)
_cell_length_b                   10.6069(3)
_cell_length_c                   14.7633(4)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.283
_cell_measurement_theta_min      2.336
_cell_volume                     2397.24(11)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32230
_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         28.300
_diffrn_reflns_theta_min         2.336
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.490
_exptl_absorpt_correction_T_max  0.5032
_exptl_absorpt_correction_T_min  0.3838
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_recrystallization_method
;
Crystals deposited from solution of CHCl3/MeOH.
;
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.129
_refine_diff_density_max         1.784
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0166P)^2^+3.4434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5245
_reflns_number_total             5950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00244c3.cif
_cod_data_source_block           briq2ir
_cod_depositor_comments
'Adding full bibliography for 7718295--7718301.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7718299
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.396
_shelx_estimated_absorpt_t_max   0.488
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              66063
_shelx_hkl_checksum              16022