Controlled O<sub>2</sub> reduction at a mixed-valent (II,I) Cu<sub>2</sub>S core.
Mangue, Jordan; Gondre, Clément; Pécaut, Jacques; Duboc, Carole; Ménage, Stéphane; Torelli, Stéphane; Chemical communications (Cambridge, England) 56 (2020) 9636–9639; doi:10.1039/d0cc03987j

data_7126925
_publ_section_title
;
 Controlled O<sub>2</sub> reduction at a mixed-valent (II,I)
 Cu<sub>2</sub>S core.
;
_journal_issue                   67
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9636
_journal_page_last               9639
_journal_paper_doi               10.1039/d0cc03987j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C33 H34 Cu2 N6 O S, 3(C H2 Cl2), H2 O, 2(C F3 O3 S)'
_chemical_formula_sum            'C38 H42 Cl6 Cu2 F6 N6 O8 S3'
_chemical_formula_weight         1260.73
_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             2020-07-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2020-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                74.072(3)
_cell_angle_beta                 66.275(3)
_cell_angle_gamma                86.862(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9903(4)
_cell_length_b                   14.2793(5)
_cell_length_c                   15.5742(6)
_cell_measurement_reflns_used    10960
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4522
_cell_measurement_theta_min      2.9692
_cell_volume                     2538.12(17)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -3.00   26.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   88.0000 -109.0000 29

  2 omega  -43.00   54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -77.0000   60.0000 97

  3 omega   -5.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000 -180.0000 96

  4 omega   59.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000    0.0000 32

  5 omega  -38.00   -1.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -88.0000  -70.0000 37

  6 omega  -24.00    8.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -88.0000  -45.0000 32

  7 omega  -93.00   39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239    0.0000 -150.0000 132

  8 omega   -5.00   96.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000   30.0000 101

  9 omega   34.00  102.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000  -90.0000 68

 10 omega    0.00   25.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000 -180.0000 25

 11 omega  -39.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -88.0000  -70.0000 101
;
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0026042580
_diffrn_orient_matrix_UB_12      -0.0217288767
_diffrn_orient_matrix_UB_13      0.0458325253
_diffrn_orient_matrix_UB_21      -0.0392535392
_diffrn_orient_matrix_UB_22      -0.0380178147
_diffrn_orient_matrix_UB_23      0.0094017461
_diffrn_orient_matrix_UB_31      0.0449944780
_diffrn_orient_matrix_UB_32      -0.0275916278
_diffrn_orient_matrix_UB_33      -0.0222017095
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34311
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.973
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.96191
_exptl_absorpt_correction_T_min  0.8995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
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    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         10358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6676
_reflns_number_total             10358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03987j2.cif
_cod_data_source_block           st125
_cod_depositor_comments          'Adding full bibliography for 7126925.cif.'
_cod_database_code               7126925
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 H10 S O2'
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.774
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(Cl5B)=Sof(Cl6B)=1-FVAR(1)
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(Cl5)=Sof(Cl6)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(Cl4B)=Sof(Cl3B)=1-FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(Cl3)=Sof(Cl4)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C42(H42C,H42D), C43A(H43A,H43B), C43B(H43C,H43D)
;
_olex2_submission_special_instructions 'No special instructions were received'