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_7708749
_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         'C34 H28.23 Cl2 Co N2 O4.12'
_chemical_formula_sum            'C34 H28.23 Cl2 Co N2 O4.12'
_chemical_formula_weight         660.53
_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   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                 100.6520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.32350(10)
_cell_length_b                   20.2915(2)
_cell_length_c                   12.52390(10)
_cell_measurement_reflns_used    13248
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0410
_cell_measurement_theta_min      4.2180
_cell_volume                     3077.79(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 0.958
_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     79.00 104.00   0.50    0.08    --   47.57  23.00 -81.00   50
  2  \w    139.00 173.00   0.50    0.33    --  105.86 125.00 -30.00   68
  3  \w     99.00 128.00   0.50    0.33    --  105.86 125.00 -30.00   58
  4  \w     93.00 178.00   0.50    0.33    --  105.86  23.00 -81.00  170
  5  \w     81.00 107.00   0.50    0.33    --  105.86-125.00-180.00   52
  6  \w     50.00  76.00   0.50    0.33    --  105.86-125.00-180.00   52
  7  \w     36.00  61.00   0.50    0.33    --  105.86-125.00  30.00   50
  8  \w     37.00  62.00   0.50    0.33    --  105.86-125.00  90.00   50
  9  \w     68.00 111.00   0.50    0.33    --  105.86-125.00  30.00   86
 10  \w     33.00 101.00   0.50    0.33    --  105.86 -77.00   0.00  136
 11  \w     33.00  68.00   0.50    0.33    --  105.86 -61.00  60.00   70
 12  \w     33.00  67.00   0.50    0.33    --  105.86 -61.00 120.00   68
 13  \w     37.00  63.00   0.50    0.33    --  105.86 -61.00 150.00   52
 14  \w      0.00  28.00   0.50    0.08    --   47.57 -23.00 113.00   56
 15  \w     37.00  64.00   0.50    0.33    --  105.86 -61.00 -60.00   54
 16  \w     33.00  71.00   0.50    0.33    --  105.86 -61.00 -90.00   76
 17  \w     33.00  71.00   0.50    0.33    --  105.86 -61.00-180.00   76
 18  \w    -29.00  21.00   0.50    0.08    --  -47.57  23.00 -81.00  100
 19  \w    -51.00 -15.00   0.50    0.33    --  -86.25  45.00 -90.00   72
 20  \w    -30.00  28.00   0.50    0.08    --  -47.57  19.00 -30.00  116
 21  \w    -37.00 -12.00   0.50    0.33    --  -86.25  30.00-150.00   50
 22  \w    -71.00 -13.00   0.50    0.33    --  -86.25  61.00  60.00  116
 23  \w    -48.00 -23.00   0.50    0.33    --  -86.25  45.00 120.00   50
 24  \w    -37.00 -12.00   0.50    0.33    --  -86.25  30.00  60.00   50
 25  \w    -29.00  17.00   0.50    0.08    --  -47.57  19.00  60.00   92
 26  \w   -100.00 -38.00   0.50    0.08    --  -47.57 -23.00 113.00  124
 27  \w   -123.00 -81.00   0.50    0.33    --  -86.25 -23.00 113.00   84
;
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.550
_diffrn_reflns_theta_min         4.201
_exptl_absorpt_coefficient_mu    6.310
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.454
_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    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1361
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6207
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0411P)^2^+1.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5730
_reflns_number_total             6207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound2
_cod_database_code               7708749
_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, All O(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(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
4.a Free rotating group:
 O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C21B(H21B), C9(H9), C15B(H15B), C21A(H21A), C8(H8), C6(H6), C15A(H15A),
 C5(H5), C17A(H17A), C17B(H17B), C18B(H18B), C18A(H18A), C10(H10), C14B(H14B),
 C14A(H14A), C4(H4)
4.c Idealised Me refined as rotating group:
 C19A(H19A,H19B,H19C), C23B(H23A,H23B,H23C), C19B(H19D,H19E,H19F), C23A(H23D,
 H23E,H23F)
;
_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
;