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_7059784
_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         'C24 H16 Cl Cu N5 O3 Se, 7[H2O]'
_chemical_formula_sum            'C24 H30 Cl Cu N5 O10 Se'
_chemical_formula_weight         726.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 91.725(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5617(2)
_cell_length_b                   15.7974(3)
_cell_length_c                   22.4261(7)
_cell_measurement_reflns_used    11957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1000
_cell_measurement_theta_min      2.9880
_cell_volume                     2677.70(12)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2012)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2012)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2012)'
_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      293(2)
_diffrn_detector_area_resol_mean 5.2170
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       rod
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.724
_exptl_crystal_size_mid          0.0427
_exptl_crystal_size_min          0.0343
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0732P)^2^+3.2241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4155
_reflns_number_total             5487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02447c2.cif
_cod_data_source_block           3Cu
_cod_depositor_comments
;Adding full bibliography for 7059784--7059786.cif.

 Adding full bibliography for 7059784--7059786.cif.
;
_cod_database_code               7059784
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.b Me refined with riding coordinates:
 C12(H12A,H12B,H12C)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 280 electrons were
found in a volume of 640\%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              59797
_shelx_fab_checksum              80926
_olex2_submission_special_instructions 'No special instructions were received'