Cobalt(II) coordination to N4-acenaphthene-based ligand and its sodium complex
Khrizanforova, Vera; Fayzullin, Robert R.; Bogomyakov, Artem; Morozov, Vladimir; Batulin, Ruslan Germanovich; Gerasimova, Tatiana; Islamov, Daut; Budnikova, Yulia H.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00347G

data_7712993
_publ_section_title
;
 Cobalt(II) coordination to N4-acenaphthene-based ligand and its sodium
 complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00347G
_journal_year                    2023
_chemical_formula_moiety         'C48 H28 Br2 Co N8, C H2 Cl2, C2 H3 N'
_chemical_formula_sum            'C51 H33 Br2 Cl2 Co N9'
_chemical_formula_weight         1061.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.8077(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.7657(7)
_cell_length_b                   13.6667(4)
_cell_length_c                   25.2714(6)
_cell_measurement_reflns_used    98532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.57
_cell_measurement_theta_min      2.59
_cell_volume                     9158.2(4)
_computing_cell_refinement       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_reduction        'APEX4 v2021.10-0 (Bruker AXS)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            682590
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         1.826
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    2.284
_exptl_absorpt_correction_T_max  0.6017
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group 2/m for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.000   0.003
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   5   8
 wR2(int) =  0.1359 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0716 (selected reflections only, after parameter refinement)

  705451 total and  23441 unique reflections assuming Friedel's law
 plus  12994 total and  3767 unique reflections in fast scans
 Reflections rejected for which |I-<I>|/su >   3.00
  697467 total and  23440 unique reflections left after |I-<I>|/su test
 plus  12600 total and  3763 unique reflections in fast scans

 Error model 5: refine all K and overall g
 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  28.3  0.0622  0.133 - 0.186  0.891 - 1.095  0.807  0.0531  18.8   35967   25811
   2  28.3  0.0635  0.113 - 0.192  0.891 - 1.095  0.778  0.0531  18.8   35417   25099
   3  28.4  0.0608  0.135 - 0.230  0.896 - 1.095  0.796  0.0531  18.8   35979   25610
   4  28.4  0.0578  0.114 - 0.222  0.929 - 1.095  0.810  0.0531  18.8   36517   25841
   5  28.4  0.0599  0.120 - 0.217  0.929 - 1.095  0.784  0.0531  18.8   36309   25832
   6  28.4  0.0636  0.163 - 0.246  0.891 - 1.071  0.794  0.0531  18.8   36483   25506
   7  28.3  0.0550  0.094 - 0.153  0.891 - 1.095  0.778  0.0531  18.8   36482   26672
   8  28.4  0.0609  0.093 - 0.189  0.891 - 1.095  0.793  0.0531  18.8   35519   25432
   9  28.4  0.0564  0.117 - 0.160  0.891 - 1.095  0.779  0.0531  18.8   36453   26534
  10  28.3  0.0576  0.103 - 0.198  0.909 - 1.095  0.738  0.0531  18.8   36074   26268
  11 -28.4  0.0555  0.116 - 0.220  0.928 - 1.095  0.795  0.0531  18.8   35440   25557
  12 -28.4  0.0622  0.132 - 0.201  0.892 - 1.095  0.841  0.0531  18.8   35304   25284
  13  28.3  0.0582  0.128 - 0.243  0.912 - 1.095  0.788  0.0531  18.8   36017   25711
  14 -28.4  0.0608  0.127 - 0.208  0.930 - 1.095  0.806  0.0531  18.8   35386   25628
  15 -28.4  0.0623  0.096 - 0.168  0.891 - 1.095  0.817  0.0531  18.8   34918   25137
  16  28.3  0.0566  0.150 - 0.244  0.891 - 1.060  0.840  0.0531  18.8   25470   19073
  17  28.4  0.0631  0.145 - 0.267  0.925 - 1.077  0.796  0.0531  18.8   36684   25651
  18   0.0  0.0491  0.136 - 0.280  0.891 - 1.095  0.995  0.0531  18.8   49970   42189
  19   0.0  0.0509  0.183 - 0.243  0.891 - 1.074  0.933  0.0531  18.8   21557   18076
  20   0.0  0.0731  0.149 - 0.242  0.891 - 1.095  0.934  0.0531  18.8   25521   18166
  21f  0.0  0.1572  1.235 - 2.578  0.891 - 1.095  1.141  0.0531  18.8   12600    6301

       8 Overloads replaced by fast scan measurements
  697475 Corrected reflections written to file sad.hkl
 Estimated minimum and maximum transmission:  0.2740  0.6017
 Additional spherical absorption correction applied with mu*r =  0.3570
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       prism
_exptl_crystal_F_000             4264
_exptl_crystal_recrystallization_method
'liquid diffusion at r.t.: acetonitrile/dichloromethane'
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.216
_refine_diff_density_max         1.945
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         22169
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+11.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19218
_reflns_number_total             22169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz003_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7712993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.638
_shelx_res_checksum              49334
_shelx_hkl_checksum              35625
_shelx_fab_checksum              77461