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_7059786
_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 N8 Ni O6 Se2, 7[H2O]'
_chemical_formula_sum            'C36 H38 N8 Ni O13 Se2'
_chemical_formula_weight         1007.37
_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             2020-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.681(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.35306(19)
_cell_length_b                   23.6850(5)
_cell_length_c                   22.9755(8)
_cell_measurement_reflns_used    26504
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0190
_cell_measurement_theta_min      2.7830
_cell_volume                     3993.09(19)
_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 0.999
_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  0.0939
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            147443
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.820
_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            orange
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       rod
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0672P)^2^+1.9252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             8164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02447c2.cif
_cod_data_source_block           2Ni
_cod_depositor_comments
;Adding full bibliography for 7059784--7059786.cif.

 Adding full bibliography for 7059784--7059786.cif.
;
_cod_original_cell_volume        3993.10(19)
_cod_database_code               7059786
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2A-C1A \\sim C1B-O2B
 with sigma of 0.02
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
 O1, C8
 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
C8 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
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 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)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 268 electrons were
found in a volume of 1000\%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              9255
_shelx_fab_checksum              89004
_olex2_submission_special_instructions 'No special instructions were received'