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_7250524
_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         'C23 H16 Cl4 Co N2 O4, C6 H16 N'
_chemical_formula_sum            'C29 H32 Cl4 Co N3 O4'
_chemical_formula_weight         687.30
_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
_audit_creation_date             2023-10-16
_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                90
_cell_angle_beta                 97.922(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.235(5)
_cell_length_b                   19.690(2)
_cell_length_c                   14.657(3)
_cell_measurement_reflns_used    22969
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.50
_cell_volume                     6070(2)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.25.0 (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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
 152 frames, detector distance = 70 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.948
_diffrn_reflns_theta_min         2.500
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.6601
_exptl_absorpt_correction_T_min  0.3038
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.150
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0574P)^2^+16.3270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1322
_reflns_d_resolution_high        0.757
_reflns_d_resolution_low         8.152
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              25
_reflns_limit_k_min              -24
_reflns_limit_l_max              17
_reflns_limit_l_min              -19
_reflns_number_gt                5673
_reflns_number_total             7216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra01958c2.cif
_cod_data_source_block           sus-jm-059
_cod_original_cell_volume        6070.0(18)
_cod_database_code               7250524
_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
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C24(H24A,H24B), C26(H26A,H26B), C8(H8A,H8B),
 C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C2(H2), C3(H3), C16(H16), C11(H11), C15(H15), C14(H14),
 C4(H4), C5(H5)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              6621
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '70.0 mm'
_stoe_detector_pixelsize_x       '0.150 mm'
_stoe_detector_pixelsize_y       '0.150 mm'
_stoe_detector_size_x            '21.6 cm'
_stoe_detector_size_y            '21.6 cm'
_stoe_evaluation_integration_a   8.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 98.1
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 56.1
_stoe_evaluation_lana_max_2theta_desired 56.1
_stoe_evaluation_lana_mean_redundancy 2.2
_stoe_evaluation_lana_number_refls_after_or 16683
_stoe_evaluation_lana_number_refls_outliers 5027
_stoe_evaluation_lana_number_refls_total 21710
_stoe_evaluation_lana_number_refls_unique 7419
_stoe_evaluation_lana_number_refls_written 16683
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           7.3   13.1   18.9   24.7   30.5   36.3   42.1   47.9   53.7
<Resolution>    4.88   3.00   2.12   1.64   1.34   1.14   0.99   0.87   0.79
N(total)         131    459    905   1531   2248   3066   3910   4762   4698
<Redundancy>     2.2    2.2    2.3    2.3    2.3    2.3    2.2    2.2    2.2
Complet. [%%]    92.2   98.1   99.0   99.6  100.0  100.0  100.0  100.0   92.8
<I/sigma>      299.9  143.3  103.2   67.2   44.9   26.6   14.2    9.3    5.3
R(int)         0.019  0.020  0.021  0.023  0.026  0.030  0.045  0.063  0.097
;
_stoe_measurement_identifier     SUS-JM-059
_stoe_measurement_max_exposure_per_frame '30.0 s'
_stoe_measurement_mean_exposure_per_frame '30.0 s'
_stoe_measurement_min_exposure_per_frame '30.0 s'
_stoe_measurement_total_exposure_time '76 min'
_stoe_measurement_total_frame_number 152
_stoe_measurement_total_run_number 1
_stoe_measurement_tube_power     '2.0 kW'