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_7712990
_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         'C34 H28 Co N4 O4'
_chemical_formula_sum            'C34 H28 Co N4 O4'
_chemical_formula_weight         615.53
_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                77.3928(10)
_cell_angle_beta                 77.0413(10)
_cell_angle_gamma                88.9629(10)
_cell_formula_units_Z            4
_cell_length_a                   10.3708(4)
_cell_length_b                   15.4254(6)
_cell_length_c                   21.0842(8)
_cell_measurement_reflns_used    39327
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.18
_cell_volume                     3206.1(2)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_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_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15493
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.939547
_exptl_absorpt_correction_T_min  0.778490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1

 Equivalent reflections defined according to point group -1
 Mean and maximum errors in direction cosine check function =   0.000   0.003

    18099 data (   2053 unique ) involve domain  1 only,  mean I/sigma  14.0
    17812 data (   1945 unique ) involve domain  2 only,  mean I/sigma   9.3
   175693 data (  13500 unique ) involve   2 domains,  mean I/sigma   8.1
      129 data (    110 unique ) involve   3 domains,  mean I/sigma   4.2

 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   3   6

 Parameter refinement for twin component  1
 ------------------------------------------
 wR2(int) =  0.1060 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0455 (selected reflections only, after parameter refinement)

 Parameter refinement for twin component  2
 ------------------------------------------
 wR2(int) =  0.1777 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0528 (selected reflections only, after parameter refinement)

 ------------------------------------------
  211733 total and  17608 unique reflections assuming Friedel's law.
  210859 total and  17595 unique reflections after rejecting pathological cases
  205225 total and  17593 unique reflections left after |I-<I>|/su test
 g = 0.0166 gave best error model; g set to 0.0166 for further calculations

 Statistics for singles of twin component  1
 -------------------------------------------
 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   17.5  0.0339   0.437 - 0.608   1.000 - 1.046   1.200    1835    1474
    2   23.4  0.0265   0.417 - 0.758   0.997 - 1.044   1.217    1149     967
    3   17.5  0.0219   0.284 - 0.514   0.997 - 1.046   1.177     628     535
    4   23.4  0.0273   0.407 - 0.644   1.003 - 1.045   1.267     723     601
    5   17.5  0.0239   0.340 - 0.491   0.997 - 1.047   1.143    1442    1244
    6   17.5  0.0250   0.413 - 0.720   1.002 - 1.046   1.208     601     491
    7   17.5  0.0262   0.455 - 0.641   1.000 - 1.044   1.211     726     575
    8   23.4  0.0261   0.385 - 0.505   0.997 - 1.047   1.146    1755    1499
    9   17.5  0.0260   0.389 - 0.556   1.004 - 1.047   1.229     809     649
   10   17.5  0.0261   0.407 - 0.552   0.997 - 1.048   1.176    2124    1774
   11   17.5  0.0217   0.335 - 0.543   0.998 - 1.047   1.197     599     483
   12   17.5  0.0284   0.415 - 0.819   1.000 - 1.049   1.239     677     561
   13   17.5  0.0315   0.430 - 0.581   1.001 - 1.047   1.209    1122     893
   14   17.5  0.0217   0.308 - 0.553   0.997 - 1.048   1.168     916     801
   15   17.5  0.0258   0.318 - 0.732   1.000 - 1.049   1.271    1161     980
   16   17.5  0.0233   0.411 - 0.687   0.997 - 1.044   1.252     886     747
   17    0.0  0.0414   0.269 - 0.397   1.002 - 1.047   1.209     805     602
   All scans  0.0268   0.269 - 0.819   0.997 - 1.049   1.207   17958   14876

 Statistics for singles of twin component  2
 -------------------------------------------
 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   17.5  0.0347   0.135 - 0.180   1.125 - 1.196   1.200    1801    1419
    2   23.4  0.0462   0.382 - 0.518   1.124 - 1.194   1.217    1149     870
    3   17.5  0.0271   0.143 - 0.222   1.126 - 1.202   1.177     602     492
    4   23.4  0.0320   0.155 - 0.246   1.127 - 1.202   1.267     698     561
    5   17.5  0.0375   0.200 - 0.276   1.128 - 1.198   1.143    1432    1138
    6   17.5  0.0369   0.238 - 0.349   1.127 - 1.200   1.208     582     441
    7   17.5  0.0281   0.155 - 0.212   1.126 - 1.202   1.211     702     543
    8   23.4  0.0396   0.248 - 0.315   1.125 - 1.200   1.146    1728    1343
    9   17.5  0.0302   0.125 - 0.187   1.127 - 1.198   1.229     807     615
   10   17.5  0.0469   0.304 - 0.398   1.125 - 1.191   1.176    2105    1553
   11   17.5  0.0284   0.125 - 0.197   1.125 - 1.203   1.197     564     456
   12   17.5  0.0423   0.344 - 0.492   1.124 - 1.202   1.239     641     497
   13   17.5  0.0346   0.131 - 0.173   1.127 - 1.195   1.209    1101     856
   14   17.5  0.0334   0.181 - 0.291   1.129 - 1.201   1.168     887     724
   15   17.5  0.0371   0.168 - 0.450   1.128 - 1.195   1.271    1134     893
   16   17.5  0.0480   0.378 - 0.494   1.124 - 1.191   1.252     892     668
   17    0.0  0.0761   0.166 - 0.276   1.125 - 1.202   1.209     822     496
   All scans  0.0392   0.125 - 0.518   1.124 - 1.203   1.207   17647   13565

 Statistics for all composite reflections
 ----------------------------------------
 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   17.5  0.0876   0.164 - 0.561   1.013 - 1.162   1.200   10597    7288
    2   23.4  0.0946   0.396 - 0.741   1.006 - 1.152   1.217    9884    6691
    3   17.5  0.0652   0.161 - 0.488   1.007 - 1.188   1.177   10251    7712
    4   23.4  0.0954   0.176 - 0.601   1.015 - 1.175   1.267    9372    6209
    5   17.5  0.0719   0.215 - 0.473   1.005 - 1.181   1.143   10644    7846
    6   17.5  0.0864   0.259 - 0.695   1.014 - 1.170   1.208   10749    7106
    7   17.5  0.0754   0.185 - 0.596   1.007 - 1.165   1.211    9817    7041
    8   23.4  0.0838   0.267 - 0.494   1.005 - 1.172   1.146    9630    6830
    9   17.5  0.0887   0.145 - 0.522   1.014 - 1.177   1.229    9645    6616
   10   17.5  0.0899   0.322 - 0.543   1.006 - 1.166   1.176   10670    7301
   11   17.5  0.0694   0.145 - 0.516   1.006 - 1.170   1.197   10067    7436
   12   17.5  0.0893   0.356 - 0.792   1.009 - 1.156   1.239   10600    7038
   13   17.5  0.0835   0.162 - 0.544   1.016 - 1.168   1.209    9577    6699
   14   17.5  0.0692   0.194 - 0.531   1.008 - 1.185   1.168   10278    7647
   15   17.5  0.0786   0.187 - 0.692   1.012 - 1.178   1.271   15437   11395
   16   17.5  0.0996   0.391 - 0.673   1.004 - 1.148   1.252    8719    5751
   17    0.0  0.1147   0.195 - 0.379   1.027 - 1.172   1.209    3683    2485
   All scans  0.0832   0.145 - 0.792   1.004 - 1.188   1.207  169620  119091

 Statistics for all single and composite reflections
 ---------------------------------------------------
 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   17.5  0.0707   0.135 - 0.608   1.000 - 1.196   1.200   14233   10181
    2   23.4  0.0754   0.382 - 0.758   0.997 - 1.194   1.217   12182    8528
    3   17.5  0.0579   0.143 - 0.514   0.997 - 1.202   1.177   11481    8739
    4   23.4  0.0812   0.155 - 0.644   1.003 - 1.202   1.267   10793    7371
    5   17.5  0.0579   0.200 - 0.491   0.997 - 1.198   1.143   13518   10228
    6   17.5  0.0773   0.238 - 0.720   1.002 - 1.200   1.208   11932    8038
    7   17.5  0.0667   0.155 - 0.641   1.000 - 1.202   1.211   11245    8159
    8   23.4  0.0625   0.248 - 0.505   0.997 - 1.200   1.146   13113    9672
    9   17.5  0.0753   0.125 - 0.556   1.004 - 1.198   1.229   11261    7880
   10   17.5  0.0667   0.304 - 0.552   0.997 - 1.191   1.176   14899   10628
   11   17.5  0.0619   0.125 - 0.543   0.998 - 1.203   1.197   11230    8375
   12   17.5  0.0793   0.344 - 0.819   1.000 - 1.202   1.239   11918    8096
   13   17.5  0.0719   0.131 - 0.581   1.001 - 1.195   1.209   11800    8448
   14   17.5  0.0583   0.181 - 0.553   0.997 - 1.201   1.168   12081    9172
   15   17.5  0.0683   0.168 - 0.732   1.000 - 1.195   1.271   17732   13268
   16   17.5  0.0803   0.378 - 0.687   0.997 - 1.191   1.252   10497    7166
   17    0.0  0.0932   0.166 - 0.397   1.002 - 1.202   1.209    5310    3583
   All scans  0.0699   0.125 - 0.819   0.997 - 1.203   1.207  205225  147532

 HKLF 5 dataset constructed from all observed data
   31274 Corrected reflections written to file hkl
 Reflections merged according to point-group -1
 Single reflections that also occur in composites not omitted
 Minimum and maximum apparent transmission:  0.778490  0.939547
 Additional spherical absorption correction applied with mu*r =  0.0420
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plank
_exptl_crystal_F_000             1276
_exptl_crystal_recrystallization_method
'liquid diffusion at r.t.: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         15493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+4.9445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13517
_reflns_number_total             15493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00347g1.cif
_cod_data_source_block           khriz010_sq
_cod_database_code               7712990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              69605
_shelx_hkl_checksum              43652
_shelx_fab_checksum              11811