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_7708750
_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, F6 P'
_chemical_formula_sum            'C36 H34 Co F6 N2 O4 P'
_chemical_formula_weight         762.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-27
_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                84.468(2)
_cell_angle_beta                 75.530(3)
_cell_angle_gamma                61.275(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2535(4)
_cell_length_b                   12.3381(4)
_cell_length_c                   14.8997(4)
_cell_measurement_reflns_used    14705
_cell_measurement_temperature    175.00(10)
_cell_measurement_theta_max      77.2470
_cell_measurement_theta_min      3.0830
_cell_volume                     1911.99(12)
_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      175
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_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     98.00 171.00   0.50    1.09    --  107.75  45.00 -60.00  146
  2  \w     99.00 173.00   0.50    1.09    --  107.75  30.00 -30.00  148
  3  \w    108.00 177.00   0.50    1.09    --  107.75  45.00  30.00  138
  4  \w     95.00 166.00   0.50    1.09    --  107.75  30.00  60.00  142
  5  \w     95.00 177.00   0.50    1.09    --  107.75 125.00-150.00  164
  6  \w     97.00 138.00   0.50    1.09    --  107.75 144.00 -57.00   82
  7  \w     98.00 172.00   0.50    1.09    --  107.75 127.00 133.00  148
  8  \w     40.00  68.00   0.50    1.09    --  107.75 -61.00 120.00   56
  9  \w     45.00  70.00   0.50    1.09    --  107.75 -77.00 120.00   50
 10  \w     43.00  75.00   0.50    1.09    --  107.75 -77.00  60.00   64
 11  \w     49.00  95.00   0.50    1.09    --  107.75 -77.00  30.00   92
 12  \w     35.00  61.00   0.50    1.09    --  107.75 -61.00  90.00   52
 13  \w     42.00  69.00   0.50    1.09    --  107.75 -61.00 -60.00   54
 14  \w     35.00  63.00   0.50    1.09    --  107.75 -61.00 -90.00   56
 15  \w     40.00  67.00   0.50    1.09    --  107.75 -61.00-120.00   54
 16  \w     35.00  64.00   0.50    1.09    --  107.75 -61.00-180.00   58
 17  \w     35.00  71.00   0.50    1.09    --  107.75 -61.00-150.00   72
 18  \w    -26.00  17.00   0.50    0.27    --   47.57 -19.00 -30.00   86
 19  \w     36.00 106.00   0.50    1.09    --  107.75 -94.00   0.00  140
 20  \w     50.00  75.00   0.50    1.09    --  107.75-127.00  57.00   50
 21  \w     37.00  85.00   0.50    0.27    --   47.57-127.00  57.00   96
 22  \w     45.00  93.00   0.50    1.09    --  107.75-125.00 -60.00   96
 23  \w     95.00 126.00   0.50    1.09    --  107.75-144.00-111.00   62
 24  \w     46.00 110.00   0.50    1.09    --  107.75-125.00-150.00  128
 25  \w     45.00  70.00   0.50    1.09    --  107.75-125.00-180.00   50
 26  \w     78.00 110.00   0.50    1.09    --  107.75-125.00-180.00   64
 27  \w     48.00 103.00   0.50    1.09    --  107.75 -94.00-120.00  110
 28  \w     74.00 106.00   0.50    1.09    --  107.75 -94.00 -90.00   64
 29  \w     75.00 102.00   0.50    1.09    --  107.75 -94.00 -30.00   54
 30  \w     48.00  74.00   0.50    1.09    --  107.75 -94.00 -30.00   52
 31  \w     54.00 106.00   0.50    0.27    --   47.57-144.00-111.00  104
 32  \w    -50.00 -25.00   0.50    1.09    --  -86.25 127.00 133.00   50
 33  \w    -75.00 -50.00   0.50    0.27    --  -47.57 127.00 133.00   50
 34  \w    -76.00 -51.00   0.50    0.27    --  -47.57 144.00 -57.00   50
 35  \w    -62.00 -37.00   0.50    1.09    --  -86.25 144.00 -57.00   50
 36  \w    -43.00  24.00   0.50    0.27    --  -47.57  38.00-180.00  134
 37  \w    -30.00  26.00   0.50    0.27    --  -47.57  19.00-120.00  112
 38  \w    -37.00 -12.00   0.50    1.09    --  -86.25  30.00-120.00   50
 39  \w   -105.00 -80.00   0.50    0.27    --  -47.57-125.00-150.00   50
 40  \w    -98.00 -70.00   0.50    0.27    --  -47.57-144.00-111.00   56
 41  \w   -131.00-106.00   0.50    1.09    --  -86.25-144.00-111.00   50
 42  \w   -119.00 -75.00   0.50    0.27    --  -47.57-127.00  57.00   88
 43  \w   -140.00-115.00   0.50    1.09    --  -86.25-127.00  57.00   50
 44  \w   -118.00 -32.00   0.50    0.27    --  -47.57 -77.00  90.00  172
 45  \w   -157.00 -72.00   0.50    1.09    --  -86.25 -61.00 120.00  170
;
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.658
_diffrn_reflns_theta_min         3.064
_exptl_absorpt_coefficient_mu    4.507
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.592
_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_density_diffrn    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7860
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1558P)^2^+1.9175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7142
_reflns_number_total             7860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound5
_cod_database_code               7708750
_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. Restrained distances
 P1-F1A = P1-F2A = P1-F3A = P1-F4A = P1-F5A = P1-F6A = P1-F1B = P1-F2B = P1-
 F4B = P1-F5B = P1-F6B = P1-F3B
 1.65 with sigma of 0.02
 F2A-F5A \\sim F2A-F4A \\sim F2A-F3A \\sim F2A-F6A \\sim F5B-F1B \\sim F5B-F6B
\\sim F5B-F2B \\sim F5B-F4B
 \\sim F5A-F4A \\sim F5A-F6A \\sim F5A-F1A \\sim F4A-F3A \\sim F4A-F1A \\sim
F3A-F6A \\sim F3A-F1A \\sim F1B-
 F6B \\sim F1B-F3B \\sim F1B-F4B \\sim F6B-F3B \\sim F6B-F2B \\sim F3B-F2B
\\sim F3B-F4B \\sim F6A-F1A ~
 F2B-F4B
 with sigma of 0.04
 P1-F2A \\sim P1-F5B \\sim P1-F5A \\sim P1-F4A \\sim P1-F3A \\sim P1-F1B \\sim
P1-F6B \\sim P1-F3B \\sim P1-
 F6A \\sim P1-F2B \\sim P1-F4B \\sim P1-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1A) = Uanis(F2A) = Uanis(F4A) = Uanis(F5A) = Uanis(F6A)
Uanis(F1B) = Uanis(F2B) = Uanis(F4B) = Uanis(F5B) = Uanis(F6B)
Uanis(F3B) = Uanis(F3A)
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14A(H14A), C14B(H14B),
 C15A(H15A), C15B(H15B), C17A(H17A), C17B(H17B), C18A(H18A), C18B(H18B),
 C22B(H22B), C22A(H22A)
5.b Idealised Me refined as rotating group:
 C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C20B(H20A,H20B,H20C), C20A(H20D,
 H20E,H20F), C24B(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;