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_7718301
_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, C10 H10 Co, 2(C6 H6)'
_chemical_formula_sum            'C62 H68 Br4 Co Ir N2 O2'
_chemical_formula_weight         1443.95
_chemical_name_common            '[CoCp2][(Briq)2Ir] . 2 C6H6'
_chemical_name_systematic
'Cobaltocenium bis(N-(2,6-dibromophenyl)-4,6-di-tert-butyl-iminoxolene)iridate dibenzene 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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;FinalCif V144 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-01-19 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7924(5)
_cell_length_b                   19.3444(6)
_cell_length_c                   22.2366(8)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.9975
_cell_measurement_theta_min      2.1635
_cell_volume                     5749.8(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2022)'
_computing_data_collection       'Bruker APEX (Bruker, 2022)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2022)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material  'FinalCIF (Kratzert, 2023)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON-III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'HELIOS Multi-layer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            205171
_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         28.296
_diffrn_reflns_theta_min         1.901
_diffrn_source                   micro-focus
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec IuS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.424
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2726
_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    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method
'Crystals are obtained from a layered benzene solution of [(Briq)2Ir]2(mu-N) with a benzene solution of cobaltocene at RT in an NMR tube in a nitrogen glovebox.'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.2726
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         14275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0169P)^2^+10.1055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11355
_reflns_number_total             14275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00244c3.cif
_cod_data_source_block           KN_4_118_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718295--7718301.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7718301
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.388
_shelx_estimated_absorpt_t_max   0.671
_shelx_res_checksum              40691
_shelx_hkl_checksum              65094