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_1565387
_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         'C74 H94 Mn2 N4 O8, 2(C4 H10 O)'
_chemical_formula_sum            'C82 H114 Mn2 N4 O10'
_chemical_formula_weight         1425.65
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 102.49(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.695(4)
_cell_length_b                   14.854(4)
_cell_length_c                   21.447(3)
_cell_measurement_reflns_used    5658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.712
_cell_measurement_theta_min      3.353
_cell_volume                     3948.6(18)
_computing_cell_refinement       'CrysAlis Pro 1.171.37.35'
_computing_data_collection       'CrysAlis Pro 1.171.37.35'
_computing_data_reduction        'CrysAlis Pro 1.171.37.35'
_computing_structure_refinement  'SHELXL 2017/1'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, EOS (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_unetI/netI     0.1711
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22424
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.910
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis Pro 1.171.37.35. Analytical numeric absorption correction
using a multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid. Empirical absorption correction
using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         9063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4914
_reflns_number_total             9063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           mnnn
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565387
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              62503
_shelx_hkl_checksum              87353