Physical properties, ligand substitution reactions, and biological activity of Co(iii)-Schiff base complexes.
King, A. Paden; Gellineau, Hendryck A.; MacMillan, Samantha N.; Wilson, Justin J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5987–6002; doi:10.1039/c8dt04606a

data_7048708
_publ_section_title
;
 Physical properties, ligand substitution reactions, and biological
 activity of Co(iii)-Schiff base complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5987
_journal_page_last               6002
_journal_paper_doi               10.1039/c8dt04606a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H18 Co F6 N4 O2, C H4 O, Cl'
_chemical_formula_sum            'C13 H22 Cl Co F6 N4 O3'
_chemical_formula_weight         490.72
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_audit_update_record
;
2018-08-28 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                65.768(2)
_cell_angle_beta                 89.306(2)
_cell_angle_gamma                82.092(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9661(2)
_cell_length_b                   11.0108(2)
_cell_length_c                   11.9024(2)
_cell_measurement_reflns_used    11262
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.7700
_cell_measurement_theta_min      2.0400
_cell_volume                     941.82(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -65.00  21.00   0.50    2.60    --    6.71 -57.00 -90.00  172
  2  \w    -26.00  24.00   0.50    2.60    --   -7.81 -99.00-150.00  100
  3  \w    -26.00  24.00   0.50    2.60    --   -7.81 -99.00   0.00  100
  4  \w    -26.00  24.00   0.50    2.60    --   -7.81 -99.00 120.00  100
  5  \w    -65.00  28.00   0.50    2.60    --    6.71 -77.00 150.00  186
  6  \w     -3.00  79.00   0.50    2.60    --    6.71  37.00 -90.00  164
  7  \w     -3.00  79.00   0.50    2.60    --    6.71  37.00 150.00  164
  8  \w    -66.00  18.00   0.50    2.60    --    6.71 -37.00 -30.00  168
  9  \w    -66.00 -21.00   0.50    2.60    --    6.71 -37.00-180.00   90
 10  \w    -66.00  18.00   0.50    2.60    --    6.71 -37.00  60.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0609658000
_diffrn_orient_matrix_UB_12      -0.0335589000
_diffrn_orient_matrix_UB_13      -0.0141357000
_diffrn_orient_matrix_UB_21      0.0054999000
_diffrn_orient_matrix_UB_22      0.0402161000
_diffrn_orient_matrix_UB_23      -0.0637966000
_diffrn_orient_matrix_UB_31      0.0659810000
_diffrn_orient_matrix_UB_32      -0.0485263000
_diffrn_orient_matrix_UB_33      -0.0033599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23740
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.128
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5022
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0314P)^2^+0.3062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4400
_reflns_number_total             5022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04606a2.cif
_cod_data_source_block           '[Co(tfacen)(NH3)2]+'
_cod_depositor_comments
'Adding full bibliography for 7048707--7048709.cif.'
_cod_database_code               7048708
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C13H22ClCoF6N4O3
_chemical_oxdiff_usercomment     MeOH/Ether
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3D
 0.84 with sigma of 0.02
 N3-H3A = N3-H3C = N3-H3B = N4-H4C = N4-H4B = N4-H4A
 0.88 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.832