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_7048707
_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         'C30 H28 Co F4 N4 O2, C3 H7 N O, Cl'
_chemical_formula_sum            'C33 H35 Cl Co F4 N5 O3'
_chemical_formula_weight         720.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-09
_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                 100.046(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9482(2)
_cell_length_b                   22.6458(5)
_cell_length_c                   13.1929(3)
_cell_measurement_reflns_used    18820
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      30.9000
_cell_measurement_theta_min      2.3660
_cell_volume                     3220.78(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -54.00  -7.00   0.50   10.50    --   -4.80 -37.00 -60.00   94
  2  \w     -8.00  26.00   0.50   10.50    --   -4.80 -99.00 -30.00   68
  3  \w      5.00  36.00   0.50   10.50    --    3.71 -99.00  30.00   62
  4  \w    -25.00  36.00   0.50   10.50    --    3.71 -99.00 150.00  122
  5  \w    -26.00  25.00   0.50   10.50    --   -4.80 -99.00  90.00  102
  6  \w      2.00  38.00   0.50   10.50    --    3.71-102.00-146.00   72
  7  \w    -17.00   8.00   0.50   10.50    --   -4.80-102.00-146.00   50
  8  \w    -23.00   5.00   0.50   10.50    --   -4.80  98.00 -22.67   56
;
_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      -0.0486351000
_diffrn_orient_matrix_UB_12      0.0025361000
_diffrn_orient_matrix_UB_13      0.0289208000
_diffrn_orient_matrix_UB_21      0.0164647000
_diffrn_orient_matrix_UB_22      0.0298919000
_diffrn_orient_matrix_UB_23      0.0110133000
_diffrn_orient_matrix_UB_31      -0.0411601000
_diffrn_orient_matrix_UB_32      0.0089761000
_diffrn_orient_matrix_UB_33      -0.0449875000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.092
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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 red'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0363P)^2^+1.4717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6026
_reflns_number_total             6588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04606a2.cif
_cod_data_source_block           '[Co(3F-salen)(3F-BnNH2)2]+'
_cod_depositor_comments
'Adding full bibliography for 7048707--7048709.cif.'
_cod_database_code               7048707
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C33H31ClCoF4N5O3
_chemical_oxdiff_usercomment     'Crystallized from DMF/Ether'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3A
 0.86 with sigma of 0.02
 H3B-N3
 0.86 with sigma of 0.02
 N4-H4B
 0.86 with sigma of 0.02
 H4A-N4
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3A \\sim O3B \\sim C31B \\sim C31A \\sim C33B \\sim N5A \\sim N5B \\sim C33A
\\sim C32B \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O3A, O3B, C31B, C31A, C33B, N5A, N5B, C33A, C32B, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3B)=Sof(H20)=1-FVAR(1)
 Sof(F3A)=Sof(H22)=FVAR(1)
 Sof(O3B)=Sof(N5B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=
 Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(2)
 Sof(O3A)=Sof(N5A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C29(H29),
  C30(H30), C31A(H31A), C31B(H31B)
6.c Idealised Me refined as rotating group:
 C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C32B(H32D,H32E,H32F), C33B(H33D,
 H33E,H33F)
;
_shelx_res_checksum              53280
_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 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.898