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_7048709
_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         'C26 H28 Co F8 N4 O2, C4 H10 O, Cl'
_chemical_formula_sum            'C30 H38 Cl Co F8 N4 O3'
_chemical_formula_weight         749.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-16
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4493(3)
_cell_length_b                   15.4493(3)
_cell_length_c                   14.4740(5)
_cell_measurement_reflns_used    8396
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.7100
_cell_measurement_theta_min      2.3210
_cell_volume                     3454.67(15)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      3.00  77.00   0.50   17.00    --    6.71   8.00 131.00  148
  2  \w     54.00  79.00   0.50   17.00    --    6.71  57.00-180.00   50
  3  \w     -7.00  38.00   0.50   17.00    --    6.71  57.00-180.00   90
;
_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      0.0208324000
_diffrn_orient_matrix_UB_12      0.0407214000
_diffrn_orient_matrix_UB_13      -0.0040509000
_diffrn_orient_matrix_UB_21      -0.0409131000
_diffrn_orient_matrix_UB_22      0.0205597000
_diffrn_orient_matrix_UB_23      -0.0039454000
_diffrn_orient_matrix_UB_31      -0.0016489000
_diffrn_orient_matrix_UB_32      0.0050662000
_diffrn_orient_matrix_UB_33      0.0486601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.704
_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    1.440
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 1318 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1045P)^2^+2.3307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3389
_reflns_number_total             3800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04606a2.cif
_cod_data_source_block           '[Co(tfacen)(3F-BnNH2)2]+'
_cod_depositor_comments
'Adding full bibliography for 7048707--7048709.cif.'
_cod_original_cell_volume        3454.67(18)
_cod_database_code               7048709
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C30H38ClCoF8N4O3
_chemical_oxdiff_usercomment     MeOH/Ether
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C7B \\sim N2-C7A
 with sigma of 0.02
 C8A-C7A \\sim C8B-C7B
 with sigma of 0.02
 F4B-C10B \\sim F4A-C10A
 with sigma of 0.02
3. Restrained planarity
 C8B, C9B, C10B, C11B, C12A, C13B, F4B
 with sigma of 0.1
 C8A, C9A, C10A, C11A, C12B, C13A, F4A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(F4B) = Uanis(F4A)
Uanis(C8A) = Uanis(C8B) = Uanis(C9A) = Uanis(C9B) = Uanis(C10A) = Uanis(C10B) =
Uanis(C11A) = Uanis(C11B) = Uanis(C12B) = Uanis(C12A) = Uanis(C13A) =
Uanis(C13B)
5. Rigid body (RIGU) restrains
 N2, F4A, C7A, C8A, C9A, C10A, C11A, C12B, C13A, F4B, C7B, C8B, C9B, C10B,
 C11B, C12A, C13B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{F4A, C7A, C8A, C9A, C10A, C11A, C12A, C13A} sigma for 1-2: 0.02, 1-3: 0.04
as
{F4B, C7B, C8B, C9B, C10B, C11B, C12B, C13B}
7. Others
 Sof(H2BC)=Sof(H2BD)=Sof(F4B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(C9B)=
 Sof(H9B)=Sof(C10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13B)=
 1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(F4A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=
 FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 N2(H2AA,H2AB), N2(H2BC,H2BD), C5(H5A,H5B), C7A(H7AA,H7AB), C7B(H7BA,H7BB),
 C14(H14A,H14B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C9B(H9B), C11B(H11B),
 C12B(H12B), C13B(H13B)
8.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C15(H15A,H15B,H15C)
;
_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 1.042
_oxdiff_exptl_absorpt_empirical_full_min 0.952