Elucidating substituent effects in magnetic properties of redox active cobalt complexes and testing them as potential catalysts for HER
Sundaresan, Sriram; Müller, Julia; Carrella, Luca M.; Rentschler, Eva; RSC Advances 15 (2025) 19287–19294; doi:10.1039/D5RA01958C

data_7250525
_publ_section_title
;
 Elucidating substituent effects in magnetic properties of redox active
 cobalt complexes and testing them as potential catalysts for HER
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              19287
_journal_page_last               19294
_journal_paper_doi               10.1039/D5RA01958C
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         '2(C31 H36 Co N2 O4), C2 H6 O'
_chemical_formula_sum            'C64 H78 Co2 N4 O9'
_chemical_formula_weight         1165.16
_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
_audit_creation_date             2023-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                92.046(5)
_cell_angle_beta                 99.904(5)
_cell_angle_gamma                102.261(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0407(6)
_cell_length_b                   11.0875(6)
_cell_length_c                   24.7624(15)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.00
_cell_volume                     2909.7(3)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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      120.0
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 2109 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33470
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'Axo Mo'
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.9560
_exptl_absorpt_correction_T_min  0.8433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.019
_exptl_crystal_size_rad          0.030
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0448P)^2^+2.0185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7381
_reflns_number_total             11409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra01958c2.cif
_cod_data_source_block           sus-jm-100_3d
_cod_database_code               7250525
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C41(H41A,H41B), C9(H9A,H9B), C8(H8A,H8B), C10(H10A,H10B),
 C40(H40A,H40B), C63(H63A,H63B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C38(H38), C42(H42), C19(H19), C47(H47), C5(H5), C11(H11),
 C52(H52), C44(H44), C46(H46), C4(H4), C3(H3), C2(H2), C45(H45), C15(H15),
 C33(H33), C36(H36), C16(H16), C14(H14), C50(H50), C13(H13), C35(H35), C34(H34)
2.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C26(H26A,H26B,H26C), C60(H60A,H60B,H60C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C61(H61A,H61B,H61C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C56(H56A,H56B,H56C), C64(H64A,H64B,H64C)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              65421
_olex2_submission_special_instructions 'No special instructions were received'