Redox-Innocent Metal-Assisted Cleavage of S-S Bond in a Disulfide-Containing Ligand.
Esmieu, Charlène; Orio, Maylis; Le Pape, Laurent; Lebrun, Colette; Pécaut, Jacques; Ménage, Stéphane; Torelli, Stéphane; Inorganic chemistry 55 (2016) 6208–6217; doi:10.1021/acs.inorgchem.6b00819

data_4347974
_publ_section_title
;
 Redox-Innocent Metal-Assisted Cleavage of S-S Bond in a
 Disulfide-Containing Ligand.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6208
_journal_page_last               6217
_journal_paper_doi               10.1021/acs.inorgchem.6b00819
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C37 H39 Cu2 N8 O2.58 S, 3(C F3 O3 S)'
_chemical_formula_sum            'C40 H39 Cu2 F9 N8 O11.58 S4'
_chemical_formula_weight         1243.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.188(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0878(10)
_cell_length_b                   18.9012(13)
_cell_length_c                   20.7938(14)
_cell_measurement_reflns_used    4748
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.5119
_cell_measurement_theta_min      3.5112
_cell_volume                     4987.0(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -6.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739  -99.0000   30.0000 74

  2 omega  -12.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739   19.0000 -150.0000 109

  3 omega   14.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739   57.0000  -30.0000 34

  4 omega  -72.00  -24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   19.0000  -90.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0012097000
_diffrn_orient_matrix_UB_12      0.0348983000
_diffrn_orient_matrix_UB_13      0.0122696000
_diffrn_orient_matrix_UB_21      -0.0206938000
_diffrn_orient_matrix_UB_22      0.0124355000
_diffrn_orient_matrix_UB_23      -0.0327952000
_diffrn_orient_matrix_UB_31      -0.0519494000
_diffrn_orient_matrix_UB_32      -0.0057797000
_diffrn_orient_matrix_UB_33      0.0035050000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22949
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             2522
_exptl_crystal_size_max          0.94
_exptl_crystal_size_mid          0.93
_exptl_crystal_size_min          0.594
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         10154
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0707P)^2^+11.0705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7029
_reflns_number_total             10154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00819_si_004.cif
_cod_data_source_block           st457_2
_cod_original_cell_volume        4986.9(6)
_cod_database_code               4347974
_chemical_oxdiff_formula         'C40 H39 Cu2 F9 N8 O11.50 S4'
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.419
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
2. Uiso/Uaniso restraints and constraints
C3S \\sim C3SB: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Sof(S13B)=Sof(F4S3)=Sof(O4S3)=Sof(O5S3)=Sof(C3SB)=1-FVAR(1)
 Sof(S13)=Sof(F3S3)=Sof(O2S3)=Sof(O3S3)=Sof(C3S)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C16(H16A,H16B), C23(H23A,H23B),
 C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
 C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'