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_7718297
_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 I Ir N2 O2, C3 H6 O'
_chemical_formula_sum            'C43 H52 Br4 I Ir N2 O3'
_chemical_formula_weight         1283.60
_chemical_name_common            '(Briq)2IrI . C3H6O'
_chemical_name_systematic
'Bis(N-(2,6-dibromo)-4,6-di-tert-butyl-iminoxolene)iodoiridium acetone solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2025-01-19 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.202(2)
_cell_length_b                   15.082(3)
_cell_length_c                   29.489(6)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.097
_cell_measurement_theta_min      2.411
_cell_volume                     4537.4(16)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_collection       'Bruker APEX-4 (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD Area Detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEX-II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            113473
_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         29.459
_diffrn_reflns_theta_min         1.381
_diffrn_source_current           35.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.184
_exptl_absorpt_correction_T_max  0.5982
_exptl_absorpt_correction_T_min  0.4158
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_recrystallization_method
'Crystals were grown by slow evaporation of an acetone solution of the complex at ambient temperature.'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.116
_exptl_transmission_factor_max   0.5982
_exptl_transmission_factor_min   0.4158
_refine_diff_density_max         2.360
_refine_diff_density_min         -3.346
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Flack x determined using 4837 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         12542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+25.5437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11573
_reflns_number_total             12542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00244c3.cif
_cod_data_source_block           iri
_cod_depositor_comments
'Adding full bibliography for 7718295--7718301.cif.'
_cod_database_code               7718297
_shelx_estimated_absorpt_t_min   0.325
_shelx_estimated_absorpt_t_max   0.490
_shelxl_version_number           2013-4
_shelx_res_checksum              19780
_shelx_hkl_checksum              2362