Comparing electrocatalytic and chemical oxygen reduction reaction by a molecular copper complex
Dutta, Lesa; Das, Avijit; Hasan, Babar; Paria, Sayantan; Mondal, Dhrubajyoti; Chemical Communications 61 (2025) 10158–10161; doi:10.1039/D5CC01491C

data_7134637
_publ_section_title
;
 Comparing electrocatalytic and chemical oxygen reduction reaction by a
 molecular copper complex
;
_journal_issue                   55
_journal_name_full               'Chemical Communications'
_journal_page_first              10158
_journal_page_last               10161
_journal_paper_doi               10.1039/D5CC01491C
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C26 H23 Cl Cu N3 O2, C26 H26 Cl Cu N3 O2, 4(Cl O4), H2 O, O'
_chemical_formula_sum            'C52 H51 Cl6 Cu2 N6 O22'
_chemical_formula_weight         1451.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-28 deposited with the CCDC.	2025-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8921(13)
_cell_length_b                   16.3316(17)
_cell_length_c                   29.441(3)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.35
_cell_volume                     6160.1(11)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'BRUKER APEX-II'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26747
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        24.333
_diffrn_reflns_theta_max         24.333
_diffrn_reflns_theta_min         1.392
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.275(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         9654
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                8293
_reflns_number_total             9654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01491c2.cif
_cod_data_source_block           Complex_2
_cod_depositor_comments
'Adding full bibliography for 7134636--7134637.cif.'
_cod_database_code               7134637
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.725(18)
 0.275(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 Cu2-H4B \\sim Cu2-H4A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O13A \\sim O13 \\sim O14 \\sim O16A \\sim O14A \\sim O15 \\sim O15A \\sim O16:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O18 \\sim O18A \\sim O19 \\sim O19A \\sim O20A \\sim O20 \\sim O17A \\sim O17:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Cl5) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(Cl5A) \\sim Ueq, Uanis(O13A) \\sim Ueq,
Uanis(O16A) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(O15A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl5A) = Uanis(Cl5)
Uanis(O13A) = Uanis(O13)
Uanis(O16) = Uanis(O16A)
Uanis(O14) = Uanis(O14A)
Uanis(O15A) = Uanis(O15)
Uanis(Cl6) = Uanis(Cl6A)
Uanis(O20) = Uanis(O20A)
Uanis(O18) = Uanis(O18A)
Uanis(O17A) = Uanis(O17)
Uanis(O19) = Uanis(O19A)
Uanis(O22C) = Uanis(O22B) = Uanis(O22A)
5. Others
 Sof(Cl5A)=Sof(O13A)=Sof(O16A)=Sof(O14A)=Sof(O15A)=1-FVAR(1)
 Sof(Cl5)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=FVAR(1)
 Sof(Cl6A)=Sof(O17A)=Sof(O18A)=Sof(O19A)=Sof(O20A)=1-FVAR(2)
 Sof(Cl6)=Sof(O17)=Sof(O18)=Sof(O19)=Sof(O20)=FVAR(2)
 Fixed Sof: O22B(0.26028) O22C(0.26924) O22A(0.47048)
6.a Riding coordinates:
 O4(H4A,H4B), O2(H2A,H2B)
6.b Free rotating group:
 O21(H21A,H21B), Cl5(O13,O14,O15,O16), Cl5A(O13A,O16A,O14A,O15A), Cl6(O17,O18,
 O19,O20), Cl6A(O17A,O18A,O19A,O20A)
6.c Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C40(H40A,H40B), C33(H33A,H33B), C20(H20A,H20B), C14(H14A,
 H14B), C8(H8A,H8B), C7(H7A,H7B)
6.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C39(H39), C37(H37), C38(H38), C29(H29), C31(H31), C13(H13),
 C11(H11), C10(H10), C12(H12), C5(H5), C26(H26), C22(H22), C25(H25), C19(H19),
 C18(H18), C24(H24), C3(H3), C49(H49), C50(H50), C42(H42), C45(H45), C43(H43),
 C44(H44), C48(H48), C51(H51), C16(H16), C17(H17), C23(H23)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3A)
;
_olex2_submission_special_instructions 'No special instructions were received'