Copper-based homometallic and heterometallic binuclear complexes for electrocatalytic CO<sub>2</sub> reduction.
Xie, Xin-Ling; Chen, Feng; Wang, Wen-Wen; Lyu, Lei-Yan; Sun, Meng-Jiao; Zhang, Teng; Cao, Rong; Chemical communications (Cambridge, England) 61 (2025) 13485–13488; doi:10.1039/d5cc04378f

data_7134901
_publ_section_title
;
 Copper-based homometallic and heterometallic binuclear complexes for
 electrocatalytic CO<sub>2</sub> reduction.
;
_journal_issue                   71
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13485
_journal_page_last               13488
_journal_paper_doi               10.1039/d5cc04378f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C25 H32 Co Cu N4 O4, 2(Cl O4)'
_chemical_formula_sum            'C25 H32 Cl2 Co Cu N4 O12'
_chemical_formula_weight         773.91
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-07-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                79.812(2)
_cell_angle_beta                 85.501(2)
_cell_angle_gamma                84.317(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6012(3)
_cell_length_b                   11.2838(4)
_cell_length_c                   14.0602(3)
_cell_measurement_reflns_used    10759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1700
_cell_measurement_theta_min      2.1460
_cell_volume                     1488.98(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_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      100.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19334
_diffrn_reflns_point_group_measured_fraction_full 0.818
_diffrn_reflns_point_group_measured_fraction_max 0.612
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.543
_diffrn_reflns_theta_min         1.841
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 3110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         11168
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0437P)^2^+0.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.506
_reflns_Friedel_fraction_full    0.635
_reflns_Friedel_fraction_max     0.411
_reflns_number_gt                9973
_reflns_number_total             11168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04378f2.cif
_cod_data_source_block           trialsolve
_cod_depositor_comments
'Adding full bibliography for 7134898--7134901.cif.'
_cod_database_code               7134901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.658
_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, All O(H,H) groups
2. Restrained distances
 O4-H4 = O7-H7A = O7-H7B = O8-H8 = O9-H9A = O9-H9B
 0.87 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C24(H24A,
 H24B), C25(H25A,H25B), C29(H29A,H29B), C34(H34A,H34B), C36(H36A,H36B),
 C37(H37A,H37B), C40(H40A,H40B), C41(H41A,H41B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C17(H17), C18(H18),
 C26(H26), C31(H31), C32(H32), C35(H35), C38(H38), C42(H42), C45(H45), C47(H47)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C46(H46A,H46B,
 H46C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              37537
_shelx_hkl_checksum              34158
_olex2_submission_special_instructions 'No special instructions were received'