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_7134898
_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         '2(C12 H15 Cu N2 O2), 2(Cl O4)'
_chemical_formula_sum            'C24 H30 Cl2 Cu2 N4 O12'
_chemical_formula_weight         764.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-07-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-29 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.507(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4287(2)
_cell_length_b                   12.34880(10)
_cell_length_c                   14.3680(2)
_cell_measurement_reflns_used    17368
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      60.4740
_cell_measurement_theta_min      2.4190
_cell_volume                     2808.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     60.00 146.00   0.50    0.88    --   73.43  38.00-150.00  172
  2  \w     59.00 145.00   0.50    0.88    --   73.43  57.00   0.00  172
  3  \w     61.00 145.00   0.50    0.88    --   73.43  37.00 111.00  168
  4  \w     79.00 105.00   0.50    0.88    --   73.43-125.00 150.00   52
  5  \w     21.00 110.00   0.50    0.88    --   73.43-125.00  90.00  178
  6  \w     20.00 109.00   0.50    0.88    --   73.43-125.00 -60.00  178
  7  \w      2.00 105.00   0.50    0.88    --   73.43 -99.00 -60.00  206
  8  \w     60.00  88.00   0.50    0.88    --   73.43 -77.00 -30.00   56
  9  \w      2.00  36.00   0.50    0.88    --   73.43 -77.00 -30.00   68
 10  \w     21.00  47.00   0.50    0.88    --   73.43 -37.00 -44.00   52
 11  \w     13.00  66.00   0.50    0.88    --   73.43 -38.00-180.00  106
 12  \w    -16.00  72.00   0.50    0.11    --   -0.94  37.00 111.00  176
 13  \w     26.00  70.00   0.50    0.11    --   -0.94  38.00-150.00   88
 14  \w    -17.00  36.00   0.50    0.11    --   -0.94  57.00-180.00  106
 15  \w    -81.00 -16.00   0.50    0.88    --  -75.30  77.00-180.00  130
 16  \w    -91.00 -16.00   0.50    0.88    --  -75.30  57.00-180.00  150
 17  \w    -58.00 -32.00   0.50    0.88    --  -75.30  37.00 111.00   52
 18  \w    -90.00 -13.00   0.50    0.88    --  -75.30  57.00 120.00  154
 19  \w    -74.00 -17.00   0.50    0.11    --   -0.94 -37.00 -44.00  114
 20  \w   -126.00 -95.00   0.50    0.88    --  -75.30 -99.00  90.00   62
 21  \w   -149.00 -60.00   0.50    0.88    --  -75.30 -37.00 -44.00  178
 22  \w    -94.00 -43.00   0.50    0.88    --  -75.30 125.00-180.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.710
_diffrn_reflns_theta_min         2.427
_exptl_absorpt_coefficient_mu    9.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6370
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0811
_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^)+(0.0316P)^2^+27.5394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5027
_reflns_number_total             6370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04378f2.cif
_cod_data_source_block           sd-re-cu-co-1
_cod_depositor_comments
'Adding full bibliography for 7134898--7134901.cif.'
_cod_original_cell_volume        2808.79(6)
_cod_database_code               7134898
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.442
_shelx_estimated_absorpt_t_min   0.096
_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,H) groups
2. Restrained distances
 O11-H11A = O11-H11B
 0.9 with sigma of 0.02
 O12-H12A = O12-H12B
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14), C16(H16), C17(H17)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              59128
_shelx_hkl_checksum              96981
_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
;