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_7708751
_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 H34 Co N2 O4'
_chemical_formula_sum            'C36 H34 Co N2 O4'
_chemical_formula_weight         617.58
_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   mixed
_audit_creation_date             2021-08-09
_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                 93.6250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.63630(10)
_cell_length_b                   20.4317(2)
_cell_length_c                   12.93790(10)
_cell_measurement_reflns_used    12895
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      75.9880
_cell_measurement_theta_min      4.0380
_cell_volume                     3069.82(5)
_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 0.959
_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     98.00 123.00   0.50    0.97    --  105.86  30.00 -30.00   50
  2  \w    141.00 175.00   0.50    0.97    --  105.86  30.00 -30.00   68
  3  \w     95.00 178.00   0.50    0.97    --  105.86  15.00  60.00  166
  4  \w    115.00 159.00   0.50    0.97    --  105.86  45.00 150.00   88
  5  \w     38.00 105.00   0.50    0.97    --  105.86 -94.00 -30.00  134
  6  \w     65.00  91.00   0.50    0.97    --  105.86-114.00 -34.00   52
  7  \w    108.00 141.00   0.50    0.97    --  105.86-174.00-173.00   66
  8  \w     67.00 101.00   0.50    0.97    --  105.86-174.00-173.00   68
  9  \w     34.00  59.00   0.50    0.24    --   47.57-114.00 -34.00   50
 10  \w     43.00  71.00   0.50    0.97    --  105.86 -61.00   0.00   56
 11  \w     73.00  98.00   0.50    0.97    --  105.86 -77.00   0.00   50
 12  \w     35.00  61.00   0.50    0.97    --  105.86 -77.00   0.00   52
 13  \w     33.00  58.00   0.50    0.97    --  105.86 -61.00 -30.00   50
 14  \w     33.00  59.00   0.50    0.97    --  105.86 -77.00 -30.00   52
 15  \w     69.00  97.00   0.50    0.97    --  105.86 -77.00 -30.00   56
 16  \w     43.00  69.00   0.50    0.97    --  105.86 -61.00  30.00   52
 17  \w     89.00 114.00   0.50    0.97    --  105.86 174.00-165.00   50
 18  \w     68.00  93.00   0.50    0.24    --   47.57 174.00-165.00   50
 19  \w    -22.00   4.00   0.50    0.24    --  -47.57  19.00-180.00   52
 20  \w    -12.00  26.00   0.50    0.24    --  -47.57  19.00-120.00   76
 21  \w    -36.00 -11.00   0.50    0.97    --  -86.25  30.00-150.00   50
 22  \w    -37.00 -11.00   0.50    0.97    --  -86.25  30.00 -90.00   52
 23  \w    -29.00  14.00   0.50    0.24    --  -47.57  19.00 150.00   86
 24  \w    -72.00 -47.00   0.50    0.97    --  -86.25 114.00  55.00   50
 25  \w   -118.00 -75.00   0.50    0.24    --  -47.57-125.00  60.00   86
 26  \w   -113.00 -88.00   0.50    0.24    --  -47.57-125.00  30.00   50
 27  \w   -130.00 -45.00   0.50    0.97    --  -86.25-174.00-173.00  170
 28  \w    -86.00 -59.00   0.50    0.24    --  -47.57-174.00-173.00   54
 29  \w   -128.00 -81.00   0.50    0.97    --  -86.25-114.00 -34.00   94
 30  \w    -82.00 -32.00   0.50    0.24    --  -47.57 114.00  55.00  100
;
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.596
_diffrn_reflns_theta_min         4.050
_exptl_absorpt_coefficient_mu    4.720
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_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    1.336
_exptl_crystal_description       prism
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     385
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0346P)^2^+1.2547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5681
_reflns_number_total             6195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound4
_cod_database_code               7708751
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H20G)=Sof(H20H)=Sof(H20I)=1-FVAR(1)
 Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C15B(H15B), C14A(H14A), C18A(H18A), C14B(H14B), C17A(H17A), C9(H9), C5(H5),
 C6(H6), C8(H8), C15A(H15A), C18B(H18B), C17B(H17B), C22A(H22A), C10(H10),
 C22B(H22B), C4(H4)
4.b Idealised Me refined as rotating group:
 C20B(H20A,H20B,H20C), C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C20A(H20D,
 H20E,H20F), C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
;
_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
;