Cationic-anionic complexes of Cu(II) and Co(II) with <i>N</i>-scorpionate ligand - structure, spectroscopy, and catecholase activity.
Zienkiewicz-Machnik, Małgorzata; Luboradzki, Roman; Mech-Piskorz, Justyna; Angulo, Gonzalo; Nogala, Wojciech; Ratajczyk, Tomasz; Aleshkevych, Pavlo; Kubas, Adam; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5268–5285; doi:10.1039/d4dt03478c

data_7718173
_publ_section_title
;
 Cationic-anionic complexes of Cu(II) and Co(II) with <i>N</i>-scorpionate
 ligand - structure, spectroscopy, and catecholase activity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5268
_journal_page_last               5285
_journal_paper_doi               10.1039/d4dt03478c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H27 Cl Co N7, C6 H11 Cl3 Co N3'
_chemical_formula_sum            'C24 H38 Cl4 Co2 N10'
_chemical_formula_weight         726.313
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-17 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.559(3)
_cell_angle_beta                 80.492(3)
_cell_angle_gamma                78.970(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4702(4)
_cell_length_b                   11.8660(5)
_cell_length_c                   12.9663(3)
_cell_measurement_reflns_used    19782
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.3260
_cell_measurement_theta_min      2.6110
_cell_volume                     1544.78(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9390
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -75.00 -13.00   1.00   37.50    --  -25.34 113.00 144.00   62
  2  \w    -20.00  70.00   1.00   37.50    --   28.46 -99.00-120.00   90
  3  \w     -8.00  78.00   1.00   37.50    --   28.46-113.00  53.00   86
  4  \w    -44.00  54.00   1.00   37.50    --   28.46 -37.00 -30.00   98
  5  \w    -44.00  54.00   1.00   37.50    --   28.46 -37.00  60.00   98
  6  \w    -42.00  59.00   1.00   37.50    --   28.46 -77.00 -60.00  101
  7  \w      8.00  97.00   1.00   37.50    --   28.46  57.00-150.00   89
  8  \w    -95.00   5.00   1.00   37.50    --  -25.34 -77.00  60.00  100
  9  \w      8.00  97.00   1.00   37.50    --   28.46  57.00 -60.00   89
 10  \w     -2.00  99.00   1.00   37.50    --   28.46  77.00 -30.00  101
 11  \w      8.00  97.00   1.00   37.50    --   28.46  57.00 120.00   89
 12  \w     35.00 104.00   1.00   37.50    --   28.46 178.00-120.00   69
 13  \w      8.00  97.00   1.00   37.50    --   28.46  57.00  30.00   89
 14  \w    -95.00   5.00   1.00   37.50    --  -25.34 -77.00 150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118288000
_diffrn_orient_matrix_UB_12      -0.0579155000
_diffrn_orient_matrix_UB_13      0.0082925000
_diffrn_orient_matrix_UB_21      0.0200982000
_diffrn_orient_matrix_UB_22      -0.0038735000
_diffrn_orient_matrix_UB_23      -0.0544726000
_diffrn_orient_matrix_UB_31      0.0656703000
_diffrn_orient_matrix_UB_32      -0.0202589000
_diffrn_orient_matrix_UB_33      0.0099534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9390
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49087
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9390
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.63
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             750.985
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.0143
_refine_diff_density_min         -0.5308
_refine_diff_density_rms         0.0982
_refine_ls_d_res_high            0.6591
_refine_ls_d_res_low             10.1782
_refine_ls_goodness_of_fit_ref   1.0486
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     410
_refine_ls_number_reflns         10605
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.0483
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.1196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                9225
_reflns_number_total             10605
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03478c2.cif
_cod_data_source_block           mzm3_02
_cod_depositor_comments
'Adding full bibliography for 7718172--7718173.cif.'
_cod_database_code               7718173
_chemical_oxdiff_formula         'C10 H10 N6 Co1 Cl2'
_olex2_refinement_description
;
1. Rigid bond restraints
 C24, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.04 within
1.7A
: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within
1.7A
C24 \\sim N10: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 1.7A
3. Others
 Sof(H10e)=1-FVAR(1)
 Sof(H10d)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C12(H12a,H12b), C18(H18a,H18b), C24(H24a,H24b)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C14(H14), C20(H20)
4.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c),
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), N10(H10d,H10e,H10f), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c)
;
_olex2_date_sample_data_collection 2022-10-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.045
_oxdiff_exptl_absorpt_empirical_full_min 0.388