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_4347972
_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         'C35 H38 Cu2 N7 O3 S, 3(C F3 O3 S), C4 H8 O'
_chemical_formula_sum            'C42 H46 Cu2 F9 N7 O13 S4'
_chemical_formula_weight         1283.18
_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             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                 101.161(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1289(3)
_cell_length_b                   19.7968(14)
_cell_length_c                   22.2550(11)
_cell_measurement_reflns_used    7342
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.3707
_cell_measurement_theta_min      3.3639
_cell_volume                     5242.7(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   34.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000  -30.0000 54

  2 omega  -66.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   19.0000   30.0000 110

  3 omega  -91.00  -47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239 -179.0000   60.0000 44

  4 omega   -5.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000  -90.0000 49
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0054982000
_diffrn_orient_matrix_UB_12      0.0289215000
_diffrn_orient_matrix_UB_13      0.0191700000
_diffrn_orient_matrix_UB_21      0.0567895000
_diffrn_orient_matrix_UB_22      0.0035689000
_diffrn_orient_matrix_UB_23      -0.0032083000
_diffrn_orient_matrix_UB_31      -0.0173573000
_diffrn_orient_matrix_UB_32      0.0208604000
_diffrn_orient_matrix_UB_33      -0.0260520000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99014
_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_colour_primary    blue
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       octaedra
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.215
_refine_diff_density_max         2.025
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         15849
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0638P)^2^+2.5865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10176
_reflns_number_total             15849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00819_si_003.cif
_cod_data_source_block           st440
_cod_database_code               4347972
_chemical_oxdiff_formula         'Cu S2 N2 O2 C30 H30'
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.668
_reflns_odcompleteness_completeness 98.90
_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, All O(H,H) groups
2. Restrained distances
 S4B-O34 = S4B-O35 = S4B-O36
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O51 \\sim C54 \\sim C53 \\sim C52 \\sim C51: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S4B)=Sof(O34)=Sof(O35)=Sof(O36)=1-FVAR(1)
 Sof(S4)=Sof(O31)=Sof(O32)=Sof(O33)=FVAR(1)
5.a Rotating group:
 O3(H3A,H3B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C16(H16A,H16B), C22(H22A,H22B),
 C28(H28A,H28B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
5.c 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), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C42(H42A,H42B,H42C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'