Isolation and characterization of carbene-supported air stable Co(II)-radical complexes with bileptic redox non-innocent ligands: stability, bonding, ring-opening copolymerization studies and photo-catalytic ring cyclization activity.
Das, Sujit; Mondal, Sangita; Suthar, Sonam; Ray, Ranay Kumar; Mondal, Karunamayee; Raveendran, Avany A.; Ahamed, Subuhan; Maji, Chandan; Baidya, Mahiuddin; Schwarz, Björn; Chakraborty, Debashis; Ungur, Liviu; Mondal, Kartik Chandra; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11182–11192; doi:10.1039/d5dt00727e

data_7718985
_publ_section_title
;
 Isolation and characterization of carbene-supported air stable
 Co(II)-radical complexes with bileptic redox non-innocent ligands:
 stability, bonding, ring-opening copolymerization studies and
 photo-catalytic ring cyclization activity.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11182
_journal_page_last               11192
_journal_paper_doi               10.1039/d5dt00727e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C47 H65 Cl Co N3 S3'
_chemical_formula_weight         862.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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
;
2025-05-23 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.056(3)
_cell_length_b                   18.248(3)
_cell_length_c                   28.434(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      17.9181
_cell_measurement_theta_min      2.2321
_cell_measurement_wavelength     0.71073
_cell_volume                     9887(3)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_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_temperature      300(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len=   0.5; end= 360.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg omega= 270.316 deg chi=  24.000 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.0; end= 390.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  11.079 deg phi= 108.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.0; end= 390.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  11.079 deg phi= 252.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.0; end= 390.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  11.079 deg phi= 324.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 106.0; end= 111.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg phi=   0.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 106.0; end= 111.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg phi= 144.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.0; end= 390.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  11.079 deg phi=  36.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.0; end= 390.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  11.079 deg phi= 180.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 106.0; end= 111.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg phi= 216.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  53.0; end= 377.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   4.793 deg phi= 360.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 106.0; end= 111.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg phi= 288.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 106.0; end= 111.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg phi=  72.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg omega= 359.214 deg chi= -24.000 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  47.0; end= 371.6 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   1.597 deg phi= 360.000 deg chi=  68.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=   3.195 deg omega=   3.942 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2624
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            677418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.107
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.402
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.741
_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            'dark blue'
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       needle
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         15092
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.2076
_refine_ls_R_factor_gt           0.0805
_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^)+(0.0373P)^2^+10.4052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6295
_reflns_number_total             15092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00727e2.cif
_cod_data_source_block           Sujit_Co8aAir_a
_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/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 7718983--7718985.cif.
;
_cod_database_code               7718985
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.9035
_shelx_estimated_absorpt_t_min   0.741
_shelx_estimated_absorpt_t_max   0.969
_diffrn_measurement_bruker_total_exposure_time 9060.0
_diffrn_reflns_bruker_av_norm_i  68.002
_diffrn_reflns_bruker_number_gt  104797
_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              30343