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_7712992
_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         'C24 H14 Br2 Co N4, C3 H7 N O'
_chemical_formula_sum            'C27 H21 Br2 Co N5 O'
_chemical_formula_weight         650.24
_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_method           SHELXL-2018/3
_audit_update_record
;
2023-05-06 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5204(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6562(14)
_cell_length_b                   6.7890(4)
_cell_length_c                   15.9607(9)
_cell_measurement_reflns_used    40117
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31.70
_cell_measurement_theta_min      2.57
_cell_volume                     2502.4(3)
_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      105(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0841
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            116888
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.446
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    3.911
_exptl_absorpt_correction_T_max  0.5908
_exptl_absorpt_correction_T_min  0.2889
_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 =   0.001   0.007
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   5   8
 wR2(int) =  0.1363 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0949 (selected reflections only, after parameter refinement)

  137491 total and   9269 unique reflections assuming Friedel's law
 Reflections rejected for which |I-<I>|/su >   3.00
  132243 total and   9266 unique reflections left after |I-<I>|/su test

 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  21.9  0.0805  0.032 - 0.060  0.979 - 1.220  0.920  0.0748  13.4   16413   10449
   2  22.0  0.1048  0.035 - 0.060  0.979 - 1.245  1.055  0.0748  13.4   11909    7075
   3  21.9  0.0780  0.031 - 0.056  0.983 - 1.185  0.850  0.0748  13.4   11534    7234
   4  21.9  0.0871  0.032 - 0.048  0.979 - 1.168  0.930  0.0748  13.4   12570    7775
   5  21.9  0.0885  0.033 - 0.052  0.979 - 1.253  0.915  0.0748  13.4    6688    4369
   6  21.9  0.0997  0.040 - 0.060  0.981 - 1.253  0.920  0.0748  13.4   14004    8752
   7  21.9  0.0822  0.031 - 0.049  0.998 - 1.222  0.943  0.0748  13.4    8902    6042
   8   0.0  0.0922  0.026 - 0.046  0.979 - 1.253  1.014  0.0748  13.4   25729   17053
   9  21.9  0.0857  0.031 - 0.053  0.979 - 1.233  0.965  0.0748  13.4   12874    8754
  10   0.0  0.0767  0.028 - 0.053  0.979 - 1.253  1.006  0.0748  13.4   11620    8273

  132243 Corrected reflections written to file sad.hkl
 Estimated minimum and maximum transmission:  0.2889  0.5908
 Additional spherical absorption correction applied with mu*r =  0.2610
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_recrystallization_method 'DMF/diethyl ether'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.033
_refine_diff_density_max         3.245
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0743P)^2^+48.4061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5233
_reflns_number_total             6278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz008
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7712992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.461
_shelx_estimated_absorpt_t_max   0.882
_shelx_res_checksum              38572
_shelx_hkl_checksum              58152