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_7712986
_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 N4'
_chemical_formula_sum            'C24 H14 N4'
_chemical_formula_weight         358.39
_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                 109.9641(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2713(5)
_cell_length_b                   13.6010(3)
_cell_length_c                   7.2095(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.58
_cell_measurement_theta_min      2.37
_cell_volume                     1683.95(8)
_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 0.974
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            80644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.589
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9376
_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 =  0.0060
 Maximum odd and even orders for spherical harmonics =   1   4
 wR2(int) =  0.1526 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0477 (selected reflections only, after parameter refinement)

   82768 total and   4178 unique reflections assuming Friedel's law
 plus   8945 total and  1561 unique reflections in fast scans
 Reflections rejected for which |I-<I>|/su >   3.00
   82180 total and   4178 unique reflections left after |I-<I>|/su test
 plus   8823 total and  1560 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  27.2  0.0299  0.223 - 0.463  0.993 - 1.023  1.006  0.0260  38.5    6382    5445
   2  27.2  0.0345  0.378 - 0.845  0.993 - 1.016  1.030  0.0260  38.5    6508    5402
   3  27.2  0.0266  0.303 - 0.498  0.993 - 1.021  0.970  0.0260  38.5    6433    5518
   4  27.2  0.0326  0.350 - 0.700  0.993 - 1.019  0.995  0.0260  38.5    6424    5430
   5  27.2  0.0266  0.298 - 0.420  0.993 - 1.024  0.967  0.0260  38.5    6395    5510
   6  27.2  0.0296  0.327 - 0.739  0.995 - 1.021  0.984  0.0260  38.5    6462    5432
   7 -27.2  0.0288  0.342 - 0.673  0.993 - 1.021  0.965  0.0260  38.5    6220    5269
   8  27.2  0.0314  0.366 - 0.910  0.993 - 1.020  0.964  0.0260  38.5    6498    5421
   9  27.2  0.0266  0.268 - 0.456  0.993 - 1.023  0.944  0.0260  38.5    6435    5546
  10  27.2  0.0281  0.223 - 0.435  0.993 - 1.017  0.988  0.0260  38.5    6331    5439
  11  27.2  0.0302  0.322 - 0.494  0.993 - 1.024  1.017  0.0260  38.5    4908    4278
  12  27.2  0.0278  0.299 - 0.433  0.994 - 1.023  0.987  0.0260  38.5    4384    3826
  13  27.2  0.0284  0.324 - 0.621  0.993 - 1.020  0.959  0.0260  38.5    6445    5475
  14   0.0  0.0301  0.330 - 0.723  0.993 - 1.019  1.177  0.0260  38.5    2355    2085
  15f  0.0  0.0549  0.322 - 0.785  0.993 - 1.021  1.097  0.0260  38.5    4589    3254
  16f  0.0  0.1181  2.779 - 4.359  0.995 - 1.016  0.944  0.0260  38.5    4234    2272

      63 Overloads replaced by fast scan measurements
   82243 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.9376  0.9754
 Additional spherical absorption correction applied with mu*r =  0.0142
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method 'a DCM solution at r.t.'
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0637P)^2^+0.6356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3751
_reflns_number_total             4057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz006
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7712986
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              57376
_shelx_hkl_checksum              97920