Janus-type diiridium complexes with functional carbene cyclometalates for high-energy phosphorescence.
Ni, Guowei; Pan, Yi; Zhou, Muyu; Sang, Yufeng; Yiu, Shek-Man; Lau, Kai Chung; Chi, Yun; Dalton transactions (Cambridge, England : 2003) 55 (2026) 904–916; doi:10.1039/d5dt02691a

data_7720476
_publ_section_title
;
 Janus-type diiridium complexes with functional carbene cyclometalates for
 high-energy phosphorescence.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              904
_journal_page_last               916
_journal_paper_doi               10.1039/d5dt02691a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C131 H143 Ir2 N13, 0.5 [CH2Cl2]'
_chemical_formula_sum            'C131.5 H144 Cl Ir2 N13'
_chemical_formula_weight         2326.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-12-02 deposited with the CCDC.	2025-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.8974(9)
_cell_length_b                   14.5469(3)
_cell_length_c                   22.9823(5)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      74.6071
_cell_measurement_theta_min      5.0281
_cell_measurement_wavelength     1.54178
_cell_volume                     13338.5(5)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.0.27.Release'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=  27.500 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start= 196.0; len= 319.0; end= 515.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg omega= 107.818 deg chi= -24.000 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi= 240.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len= 359.7; end= 719.7 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg omega= 313.968 deg chi=  44.500 deg] 
measure for 2.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi=  80.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Phi   scan: start= 332.0; len= 199.1; end= 531.1 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg omega=  11.517 deg chi=  24.000 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.303 deg phi= 180.000 deg chi= -44.500 deg] 
measure for 9.9 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi= 280.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi= 120.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi=   0.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Phi   scan: start= 282.4; len= 187.0; end= 469.4 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg omega= 311.772 deg chi=  24.000 deg] 
measure for 2.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=   1.4; len= 112.2; end= 113.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg phi= 200.000 deg chi=  65.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.303 deg phi= 270.000 deg chi= -44.500 deg] 
measure for 9.9 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.303 deg phi=  90.000 deg chi= -44.500 deg] 
measure for 9.9 seconds; frame angle 1.10 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 359.7; end= 359.7 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.803 deg omega= 105.685 deg chi= -44.500 deg] 
measure for 16.0 seconds; frame angle 1.10 degrees, wavelength=1.54184>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109555
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.836
_diffrn_reflns_theta_min         3.234
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.1
_diffrn_source_target            Cu
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.354
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             4780
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.226(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         13498
_refine_ls_number_restraints     1634
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+7.2696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                12920
_reflns_number_total             13498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02691a2.cif
_cod_data_source_block           5_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/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 
;
_cod_original_formula_sum        'C131.50 H144 Cl Ir2 N13'
_cod_database_code               7720476
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.8577
_bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 1000'
_diffrn_measurement_bruker_total_exposure_time 25961.5
_diffrn_reflns_bruker_av_norm_i  26529.094
_diffrn_reflns_bruker_number_gt  112762
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              32385
_shelx_fab_checksum              65301
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 2836\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Formula Unit 
which account for 84 electrons 
per unit cell.
;