Binuclear iminopyridine-bridged 3d late transition metal complexes with o-semiquinones
Zolotukhin, Alexey A.; Bubnov, Michael P.; Bogomyakov, Artem S.; Cherkasov, Anton V.; Fukin, Georgy; Cherkasov, Vladimir K.; Inorganica Chimica Acta 502 (2020) 119346–; doi:10.1016/j.ica.2019.119346

data_1565388
_publ_section_title
;
 Binuclear iminopyridine-bridged 3d late transition metal complexes with
 o-semiquinones
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119346
_journal_paper_doi               10.1016/j.ica.2019.119346
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C60 H78 Co2 N4 O8, 4(C7 H8)'
_chemical_formula_sum            'C102 H126 Co2 N4 O8'
_chemical_formula_weight         1653.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                89.399(3)
_cell_angle_beta                 80.523(3)
_cell_angle_gamma                74.561(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1147(4)
_cell_length_b                   13.3341(6)
_cell_length_c                   17.7612(5)
_cell_measurement_reflns_used    8518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5031
_cell_measurement_theta_min      2.9621
_cell_volume                     2276.10(16)
_computing_cell_refinement       'CrysAlis Pro 1.171.35.19'
_computing_data_collection       'CrysAlis Pro 1.171.35.19'
_computing_data_reduction        'CrysAlis Pro 1.171.35.19'
_computing_structure_refinement  'SHELXL 2017/1'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, EOS (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46384
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis Pro 1.171.35.19. Empirical absorption correction using
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         13299
_refine_ls_number_restraints     681
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0899P)^2^+0.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8798
_reflns_number_total             13299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           cosqpyal1
_cod_database_code               1565388
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.786
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              77848
_shelx_hkl_checksum              86475