Bio-inspired copper complexes with Cu<sub>2</sub>S cores: (solvent) effects on oxygen reduction reactions.
Mangue, Jordan; Wehrung, Iris; Pécaut, Jacques; Ménage, Stéphane; Orio, Maylis; Torelli, Stéphane; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15576–15582; doi:10.1039/d4dt01629g

data_7716862
_publ_section_title
;
 Bio-inspired copper complexes with Cu<sub>2</sub>S cores: (solvent)
 effects on oxygen reduction reactions.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15576
_journal_page_last               15582
_journal_paper_doi               10.1039/d4dt01629g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H35 Cu2 F3 N4 O3 S2, C F3 O3 S, C3 H6 O'
_chemical_formula_sum            'C40 H41 Cu2 F6 N4 O7 S3'
_chemical_formula_weight         1027.03
_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   mixed
_audit_creation_date             2023-11-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                71.825(3)
_cell_angle_beta                 89.191(3)
_cell_angle_gamma                79.823(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0301(4)
_cell_length_b                   13.4863(5)
_cell_length_c                   15.6024(5)
_cell_measurement_reflns_used    6711
_cell_measurement_temperature    150.1(5)
_cell_measurement_theta_max      31.3520
_cell_measurement_theta_min      2.2740
_cell_volume                     2168.36(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.1(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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     35.00 102.00   1.00   10.00    --   25.72 178.00 120.00   67
  2  \w    -11.00  77.00   1.00   10.00    --   25.72-116.00 -18.00   88
  3  \w    -79.00  11.00   1.00   10.00    --  -26.97 116.00  70.00   90
  4  \w    -53.00  45.00   1.00   10.00    --  -26.97  37.00-120.00   98
  5  \w    -99.00  -1.00   1.00   10.00    --  -26.97 -37.00  60.00   98
  6  \w    -97.00 -48.00   1.00   10.00    --  -26.97 -77.00-120.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0209371000
_diffrn_orient_matrix_UB_12      -0.0274066000
_diffrn_orient_matrix_UB_13      0.0425304000
_diffrn_orient_matrix_UB_21      0.0304659000
_diffrn_orient_matrix_UB_22      0.0292420000
_diffrn_orient_matrix_UB_23      0.0207706000
_diffrn_orient_matrix_UB_31      -0.0539462000
_diffrn_orient_matrix_UB_32      0.0395255000
_diffrn_orient_matrix_UB_33      -0.0073217000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26420
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'lustrous black'
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         13107
_refine_ls_number_restraints     422
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0593P)^2^+3.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9406
_reflns_number_total             13107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01629g2.cif
_cod_data_source_block           mj157
_cod_depositor_comments
'Adding full bibliography for 7716861--7716862.cif.'
_cod_original_cell_volume        2168.37(14)
_cod_database_code               7716862
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H37 Cu2 F6 N4 O7 S3'
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5S-S5
 1.83 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F3S4 \\sim S4 \\sim O1S4 \\sim O2S4 \\sim O3S4 \\sim C4S \\sim F1S4 \\sim F2S4
\\sim O2S5 \\sim S5 \\sim O1S5 \\sim O3S5 \\sim C5S \\sim F1S5 \\sim F2S5 \\sim
F3S5 \\sim O3S3 \\sim S3 \\sim O1S3 \\sim O2S3 \\sim C3S \\sim F1S3 \\sim F2S3
\\sim F3S3: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.005 within 1.7A
4. Others
 1*[Sof(S3)+Sof(F1S3)+Sof(F2S3)+Sof(F3S3)+Sof(O1S3)+Sof(O2S3)+Sof(O3S3)+
 Sof(C3S)]+1*[Sof(S4)+Sof(F1S4)+Sof(F2S4)+Sof(F3S4)+Sof(O1S4)+Sof(O2S4)+
 Sof(O3S4)+Sof(C4S)]+1*[Sof(S5)+Sof(F1S5)+Sof(F2S5)+Sof(F3S5)+Sof(O1S5)+
 Sof(O2S5)+Sof(O3S5)+Sof(C5S)]=1 with esd of 0.000001
 Sof(S3)=Sof(F1S3)=Sof(F2S3)=Sof(F3S3)=Sof(O1S3)=Sof(O2S3)=Sof(O3S3)=Sof(C3S)=
 FVAR(1)
 Sof(S4)=Sof(F1S4)=Sof(F2S4)=Sof(F3S4)=Sof(O1S4)=Sof(O2S4)=Sof(O3S4)=Sof(C4S)=
 FVAR(2)
 Sof(S5)=Sof(F1S5)=Sof(F2S5)=Sof(F3S5)=Sof(O1S5)=Sof(O2S5)=Sof(O3S5)=Sof(C5S)=
 FVAR(3)
5.a :
 S3(F1S3,F2S3,F3S3,O1S3,O2S3,O3S3,C3S), S4(F1S4,F2S4,F3S4,O1S4,O2S4,O3S4,C4S),
 S5(F1S5,F2S5,F3S5,O1S5,O2S5,O3S5,C5S)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              77193
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.950