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_7712991
_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         'C27 H21 Br2 Co N5 O, C6 H6'
_chemical_formula_sum            'C33 H27 Br2 Co N5 O'
_chemical_formula_weight         728.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                67.3691(8)
_cell_angle_beta                 79.1286(8)
_cell_angle_gamma                73.1164(8)
_cell_formula_units_Z            2
_cell_length_a                   9.1830(3)
_cell_length_b                   12.4243(4)
_cell_length_c                   14.7547(5)
_cell_measurement_reflns_used    35715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.38
_cell_measurement_theta_min      2.33
_cell_volume                     1481.17(9)
_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 1.000
_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  0.0517
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            91337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.574
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.5041
_exptl_absorpt_correction_T_min  0.1485
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group -1 for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.001   0.005
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   5   8
 wR2(int) =  0.1508 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0605 (selected reflections only, after parameter refinement)

   94205 total and  11708 unique reflections assuming Friedel's law
 plus   5423 total and  2933 unique reflections in fast scans
 Reflections rejected for which |I-<I>|/su >   3.00
   93677 total and  11708 unique reflections left after |I-<I>|/su test
 plus   5282 total and  2913 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  24.0  0.0483  0.319 - 0.545  0.886 - 1.062  0.841  0.0434  23.0   10757    7866
   2  24.0  0.0598  0.202 - 0.496  0.886 - 1.169  0.933  0.0434  23.0   10607    7469
   3  24.0  0.0539  0.175 - 0.449  0.889 - 1.168  0.903  0.0434  23.0   10674    7694
   4  24.0  0.0542  0.261 - 0.631  0.899 - 1.168  0.838  0.0434  23.0   10595    7798
   5  24.0  0.0492  0.360 - 0.483  0.886 - 1.098  0.834  0.0434  23.0   10526    7723
   6  24.0  0.0480  0.213 - 0.419  0.886 - 1.166  0.871  0.0434  23.0   17121   13513
   7  24.0  0.0503  0.222 - 0.643  0.886 - 1.153  0.896  0.0434  23.0   15285   11519
   8   0.0  0.0612  0.331 - 0.528  0.901 - 1.166  0.997  0.0434  23.0    8112    6088
   9f  0.0  0.1501  3.249 - 5.346  0.886 - 1.167  1.085  0.0434  23.0    5282    2772

       2 Overloads replaced by fast scan measurements
   93679 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.1485  0.5041
 Additional spherical absorption correction applied with mu*r =  0.4880
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       prism
_exptl_crystal_F_000             730
_exptl_crystal_recrystallization_method
'liquid diffusion at r.t.: DMF/diethyl ether-benzene'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.204
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         10770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.7229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8946
_reflns_number_total             10770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz_ss
_cod_database_code               7712991
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.551
_shelx_res_checksum              64031
_shelx_hkl_checksum              18465