Nickel(II) and Cobalt(III) bis(dioxolene) complexes with di(2-pyridyl)imine ligands: Synthesis and magnetic properties
Zolotukhin, Alexey A.; Korshunova, Anastasiya A.; Bubnov, Michael P.; Bogomyakov, Artem S.; Baranov, Evgeny V.; Cherkasov, Vladimir K.; Inorganica Chimica Acta 512 (2020) 119869–; doi:10.1016/j.ica.2020.119869

data_1564067
_publ_section_title
;
 Nickel(II) and Cobalt(III) bis(dioxolene) complexes with
 di(2-pyridyl)imine ligands: Synthesis and magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119869
_journal_paper_doi               10.1016/j.ica.2020.119869
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety         'C51 H65 N3 Ni O4'
_chemical_formula_sum            'C51 H65 N3 Ni O4'
_chemical_formula_weight         842.77
_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                 110.250(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4722(17)
_cell_length_b                   9.5751(7)
_cell_length_c                   21.1469(15)
_cell_measurement_reflns_used    9498
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.30
_cell_volume                     4648.9(6)
_computing_cell_refinement       'SAINT (8.37A)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT (8.37A)'
_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  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12010
_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         28.759
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         12010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0200P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10398
_reflns_number_total             12010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119869.cif
_cod_data_source_block           nisq2n3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564067
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              34650
_shelx_hkl_checksum              7766