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_7708752
_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 Cl2 Co N2 O4, H2 O'
_chemical_formula_sum            'C34 H30 Cl2 Co N2 O5'
_chemical_formula_weight         676.43
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-13
_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                 107.2720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.19180(10)
_cell_length_b                   19.02700(10)
_cell_length_c                   13.23210(10)
_cell_measurement_reflns_used    23299
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5220
_cell_measurement_theta_min      4.2120
_cell_volume                     3171.49(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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    -62.00  25.00   0.50    0.38    --  -47.57  55.00 -64.00  174
  2  \w   -119.00 -34.00   0.50    0.38    --  -47.57 -55.00 152.00  170
  3  \w     -1.00  58.00   0.50    0.38    --   47.57 -55.00 152.00  118
  4  \w     83.00 109.00   0.50    0.38    --   47.57  55.00 -64.00   52
  5  \w   -158.00 -77.00   0.50    1.53    --  -86.25 -55.00 152.00  162
  6  \w    -41.00 -15.00   0.50    1.53    --  -86.25  55.00 -64.00   52
  7  \w     92.00 177.00   0.50    1.53    --  105.86  55.00 -64.00  170
  8  \w     34.00  59.00   0.50    1.53    --  105.86 -55.00 152.00   50
  9  \w   -118.00 -91.00   0.50    0.38    --  -47.57-125.00  90.00   54
 10  \w    -61.00  20.00   0.50    0.38    --  -47.57  57.00-150.00  162
 11  \w   -117.00 -82.00   0.50    0.38    --  -47.57-125.00 -90.00   70
 12  \w   -117.00 -82.00   0.50    0.38    --  -47.57-125.00 120.00   70
 13  \w     49.00  95.00   0.50    0.38    --   47.57-125.00   0.00   92
 14  \w    -37.00 -12.00   0.50    1.53    --  -86.25  30.00 150.00   50
 15  \w   -151.00-125.00   0.50    1.53    --  -86.25 -30.00-120.00   52
 16  \w    -37.00 -12.00   0.50    1.53    --  -86.25  30.00-150.00   50
 17  \w    -37.00 -11.00   0.50    1.53    --  -86.25  30.00  60.00   52
 18  \w    -45.00 -13.00   0.50    1.53    --  -86.25  61.00  90.00   64
 19  \w    103.00 158.00   0.50    1.53    --  105.86  45.00-150.00  110
 20  \w     34.00 101.00   0.50    1.53    --  105.86 -77.00 120.00  134
 21  \w     33.00  63.00   0.50    1.53    --  105.86 -94.00 -60.00   60
 22  \w     35.00  64.00   0.50    1.53    --  105.86 -94.00 -30.00   58
 23  \w     34.00 105.00   0.50    1.53    --  105.86 -94.00  30.00  142
 24  \w     35.00 105.00   0.50    1.53    --  105.86 -94.00  60.00  140
 25  \w     41.00 174.00   0.50    1.53    --  105.86   0.00  90.00  266
 26  \w     82.00 112.00   0.50    1.53    --  105.86-125.00 -60.00   60
 27  \w     33.00 104.00   0.50    1.53    --  105.86 -94.00 -90.00  142
 28  \w     55.00 122.00   0.50    1.53    --  105.86-139.00 -62.47  134
 29  \w     92.00 118.00   0.50    1.53    --  105.86  15.00 150.00   52
 30  \w    141.00 178.00   0.50    1.53    --  105.86  15.00 150.00   74
 31  \w     38.00  83.00   0.50    1.53    --  105.86 -77.00  60.00   90
 32  \w     35.00  90.00   0.50    1.53    --  105.86 -94.00 120.00  110
 33  \w     49.00  94.00   0.50    1.53    --  105.86 -77.00-180.00   90
 34  \w    113.00 177.00   0.50    1.53    --  105.86  30.00-120.00  128
 35  \w     95.00 124.00   0.50    1.53    --  105.86-142.00-152.71   58
 36  \w     67.00  93.00   0.50    1.53    --  105.86 -94.00 -30.00   52
 37  \w     81.00 106.00   0.50    1.53    --  105.86 -94.00 -60.00   50
 38  \w     68.00 105.00   0.50    1.53    --  105.86 -94.00   0.00   74
 39  \w     35.00  64.00   0.50    1.53    --  105.86 -61.00 -30.00   58
 40  \w     38.00  71.00   0.50    1.53    --  105.86 -61.00 -60.00   66
;
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.679
_diffrn_reflns_theta_min         4.155
_exptl_absorpt_coefficient_mu    6.158
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6576
_refine_ls_number_restraints     436
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0426P)^2^+1.4617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6133
_reflns_number_total             6576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound2H2O
_cod_database_code               7708752
_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(Cl1)=Sof(C18)=Sof(H18)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(C17)=Sof(H17)=1-FVAR(1)
 Sof(Cl1B)=Sof(C17B)=Sof(H17B)=Sof(C16B)=Sof(C15B)=Sof(H15B)=Sof(C14B)=
 Sof(H14B)=Sof(C18B)=Sof(H18B)=FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=1-FVAR(2)
 Sof(O2)=Sof(H2A)=Sof(H2B)=FVAR(2)
 Sof(C23)=Sof(H23G)=Sof(H23H)=Sof(H23I)=1-FVAR(3)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=FVAR(3)
4.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C21B(H21B), C6(H6), C15A(H15A), C18A(H18A), C14A(H14A), C17A(H17A),
 C8(H8), C21A(H21A), C4(H4), C10(H10), C9(H9), C17B(H17B), C15B(H15B),
 C14B(H14B), C18B(H18B), C18(H18), C14(H14), C15(H15), C17(H17)
4.c Fitted hexagon refined as free rotating group:
 C18(C13B,C14,C15,C16,C17)
4.d Idealised Me refined as rotating group:
 C19B(H19A,H19B,H19C), C23B(H23A,H23B,H23C), C19A(H19D,H19E,H19F), C23A(H23D,
 H23E,H23F), C23(H23G,H23H,H23I)
;
_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
;