Rich redox-activity and solvatochromism in a family of heteroleptic cobalt complexes
Nadurata, Vincent L.; Hay, Moya A.; Janetzki, Jett T.; Gransbury, Gemma K.; Boskovic, Colette; Dalton Transactions  (2021) –; doi:10.1039/D1DT03327A

data_7708748
_publ_section_title
;
 Rich redox-activity and solvatochromism in a family of heteroleptic
 cobalt complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03327A
_journal_year                    2021
_chemical_formula_moiety         'C36 H28 Co F6 N2 O4'
_chemical_formula_sum            'C36 H28 Co F6 N2 O4'
_chemical_formula_weight         725.53
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-29 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3831(2)
_cell_length_b                   16.40050(10)
_cell_length_c                   15.1624(2)
_cell_measurement_reflns_used    14199
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5380
_cell_measurement_theta_min      3.5490
_cell_volume                     3257.69(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_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     94.00 120.00   0.50    0.49    --  105.86  45.00 -60.00   52
  2  \w    143.00 178.00   0.50    0.49    --  105.86  45.00 -60.00   70
  3  \w    101.00 176.00   0.50    0.49    --  105.86  30.00 120.00  150
  4  \w     94.00 176.00   0.50    0.49    --  105.86  30.00-120.00  164
  5  \w     93.00 152.00   0.50    0.49    --  105.86  16.00-141.00  118
  6  \w     71.00 102.00   0.50    0.12    --   47.57  16.00-141.00   62
  7  \w     35.00  65.00   0.50    0.12    --   47.57  16.00-141.00   60
  8  \w     39.00 106.00   0.50    0.49    --  105.86 -94.00-120.00  134
  9  \w    -28.00  27.00   0.50    0.12    --  -47.57  16.00-141.00  110
 10  \w    -37.00 -12.00   0.50    0.49    --  -86.25  30.00 -30.00   50
 11  \w    -71.00 -44.00   0.50    0.49    --  -86.25  61.00   0.00   54
 12  \w    -41.00   6.00   0.50    0.12    --  -47.57  38.00   0.00   94
 13  \w    -44.00  22.00   0.50    0.12    --  -47.57  38.00  90.00  132
 14  \w   -141.00 -89.00   0.50    0.49    --  -86.25 -16.00  48.00  104
 15  \w   -108.00 -41.00   0.50    0.12    --  -47.57 -16.00  48.00  134
 16  \w    -67.00 -41.00   0.50    0.12    --  -47.57 125.00-120.00   52
 17  \w     36.00 101.00   0.50    0.49    --  105.86 -77.00-120.00  130
 18  \w     62.00  94.00   0.50    0.49    --  105.86 -77.00 -60.00   64
 19  \w     40.00  69.00   0.50    0.49    --  105.86 -61.00-120.00   58
 20  \w     33.00  69.00   0.50    0.49    --  105.86 -61.00 -60.00   72
 21  \w     33.00  65.00   0.50    0.49    --  105.86 -61.00 -30.00   64
 22  \w     39.00  70.00   0.50    0.49    --  105.86 -61.00  90.00   62
 23  \w    142.00 175.00   0.50    0.49    --  105.86 125.00 120.00   66
 24  \w    113.00 138.00   0.50    0.49    --  105.86 125.00 120.00   50
 25  \w    -23.00   2.00   0.50    0.12    --   47.57 -16.00  48.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.571
_diffrn_reflns_theta_min         3.565
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0386P)^2^+1.2646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6114
_reflns_number_total             6622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound1
_cod_database_code               7708748
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
3. Others
 Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(1)
 Sof(F3A)=Sof(F1A)=Sof(F2A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C22B(H22B), C14A(H14A), C14B(H14B), C4(H4), C15B(H15B), C18A(H18A),
 C22A(H22A), C5(H5), C10(H10), C15A(H15A), C17A(H17A), C6(H6), C9(H9),
 C18B(H18B), C17B(H17B), C8(H8)
4.b Idealised Me refined as rotating group:
 C20A(H20A,H20B,H20C), C24B(H24A,H24B,H24C), C24A(H24D,H24E,H24F), C20B(H20D,
 H20E,H20F)
;
_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
;