Formation of metal-radical species upon reduction of late transition metal complexes with heteroleptic ligands: an experimental and theoretical study
Malček, Michal; Kožíšková, Júlia; Herich, Peter; Rapta, Peter; Stepanenko, Iryna; Arion, Vladimir B.; New Journal of Chemistry 44 (2020) 13195–13206; doi:10.1039/D0NJ02447C

data_7059785
_publ_section_title
;
 Formation of metal-radical species upon reduction of late transition
 metal complexes with heteroleptic ligands: an experimental and
 theoretical study
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13195
_journal_page_last               13206
_journal_paper_doi               10.1039/D0NJ02447C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C36 H24 Co N8 O6 Se2, 7[H2O]'
_chemical_formula_sum            'C36 H38 Co N8 O13 Se2'
_chemical_formula_weight         1007.60
_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   geom
_audit_creation_date             2019-08-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7014(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.18143(15)
_cell_length_b                   23.6904(7)
_cell_length_c                   22.8941(5)
_cell_measurement_reflns_used    18569
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.41
_cell_measurement_theta_min      2.69
_cell_volume                     3881.89(16)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.2383
_diffrn_reflns_av_unetI/netI     0.1472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            105405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.058
_diffrn_reflns_theta_min         2.689
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    6.285
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.379
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       rod
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7411
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3232
_reflns_number_total             7492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02447c2.cif
_cod_data_source_block           1Co
_cod_depositor_comments
;Adding full bibliography for 7059784--7059786.cif.

 Adding full bibliography for 7059784--7059786.cif.
;
_cod_database_code               7059785
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C1B-C8
 1.5 with sigma of 0.002
 C1B-O1
 1.25 with sigma of 0.002
 C1A-C8
 1.5 with sigma of 0.002
 C1A-O1
 1.25 with sigma of 0.002
3. Rigid bond restraints
 O2A, C1A, O2B, C1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2A \\sim C1A \\sim O2B \\sim C1B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Others
 Sof(O2B)=Sof(C1B)=1-FVAR(1)
 Sof(O2A)=Sof(C1A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C23(H23A,H23B)
6.b Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C14(H14), C17(H17), C18(H18), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 268 electrons were
found in a volume of 904\%A^3 in 1 void per unit cell.
This is consistent with the presence of 7[H2O] per Asymmetric Unit 
which account for 280 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23371
_shelx_fab_checksum              58381
_olex2_submission_special_instructions 'No special instructions were received'