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_7708753
_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         '1.5(C34 H30 Co N2 O4), [+ solvents]'
_chemical_formula_sum            'C34 H30 Co N2 O4'
_chemical_formula_weight         589.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-26
_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                 133.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   30.221(6)
_cell_length_b                   19.317(4)
_cell_length_c                   21.459(4)
_cell_measurement_reflns_used    2231
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.658
_cell_measurement_theta_min      3.064
_cell_volume                     9159(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78316
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.269
_diffrn_reflns_theta_min         2.298
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.2010 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8809.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       prism
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0052(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         13257
_refine_ls_number_restraints     1003
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0820P)^2^+1.1259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10704
_reflns_number_total             13257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03327a2.cif
_cod_data_source_block           Compound3
_cod_database_code               7708753
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.982
_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 planarity
 C13B, C18C, C17C, C16B, C15C, C14C
 with sigma of 0.1
3. Rigid bond restraints
 C13B, C14B, C14C, C15B, C15C, C16B, C17B, C17C, C18B, C18C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19C, C19B, C20C, C20B, O1C, O1B, O2C, O2B, C22B, C22C, C21C, C21B, C23B, C23C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13B \\sim C14B \\sim C14C \\sim C15B \\sim C15C \\sim C16B \\sim C17B \\sim
C17C \\sim C18B \\sim C18C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C19C \\sim C19B \\sim C20C \\sim C20B \\sim O1C \\sim O1B \\sim O2C \\sim O2B
\\sim C22B \\sim C22C \\sim C21C \\sim C21B \\sim C23B \\sim C23C: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C14C) = Uanis(C14B)
Uanis(C15C) = Uanis(C15B)
Uanis(C19B) = Uanis(C19C)
5. 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
6. Others
 Sof(O2C)=Sof(O1C)=Sof(C23C)=Sof(H23G)=Sof(H23H)=Sof(H23I)=Sof(C21C)=Sof(H21C)=
 Sof(C19C)=Sof(H19G)=Sof(H19H)=Sof(H19I)=Sof(C22C)=Sof(C20C)=1-FVAR(1)
 Sof(O2B)=Sof(O1B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20B)=FVAR(1)
 Sof(C17C)=Sof(H17C)=Sof(C14C)=Sof(H14C)=Sof(C18C)=Sof(H18C)=Sof(C15C)=
 Sof(H15C)=1-FVAR(2)
 Sof(C14B)=Sof(H14B)=Sof(C18B)=Sof(H18B)=Sof(C17B)=Sof(H17B)=Sof(C15B)=
 Sof(H15B)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C21A(H21A), C15A(H15A), C17A(H17A), C8(H8), C5(H5), C10(H10), C16A(H16A),
 C14A(H14A), C4(H4), C18A(H18A), C9(H9), C6(H6), C21B(H21B), C14B(H14B),
 C18B(H18B), C17B(H17B), C15B(H15B), C17C(H17C), C21C(H21C), C14C(H14C),
 C18C(H18C), C15C(H15C), C28(H28), C32(H32), C39(H39), C26(H26), C36(H36),
 C33(H33), C27(H27), C34(H34), C35(H35)
7.b Idealised Me refined as rotating group:
 C19A(H19A,H19B,H19C), C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F), C19B(H19D,
 H19E,H19F), C23C(H23G,H23H,H23I), C19C(H19G,H19H,H19I), C41(H41A,H41B,H41C),
 C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'