Tuning of the Copper-Thioether Bond in Tetradentate N3S(thioether) Ligands; O-O Bond Reductive Cleavage via a [Cu(II)2(μ-1,2-peroxo)](2+)/[Cu(III)2(μ-oxo)2](2+) Equilibrium.
Kim, Sunghee; Ginsbach, Jake W.; Billah, A. Imtiaz; Siegler, Maxime A.; Moore, Cathy D.; Solomon, Edward I.; Karlin, Kenneth D.; Journal of the American Chemical Society 136 (2014) 8063–; doi:10.1021/ja502974c

data_4121890
_publ_section_title
;
 Tuning of the Copper-Thioether Bond in Tetradentate N3S(thioether)
 Ligands; O-O Bond Reductive Cleavage via a
 [Cu(II)2(\m-1,2-peroxo)](2+)/[Cu(III)2(\m-oxo)2](2+) Equilibrium.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8063
_journal_paper_doi               10.1021/ja502974c
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C52 H66 Cu2 N6 O4 S2, 2(C24 B F20), 2(C5 H12)'
_chemical_formula_sum            'C110 H90 B2 Cu2 F40 N6 O4 S2'
_chemical_formula_weight         2532.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.739(3)
_cell_angle_beta                 88.928(3)
_cell_angle_gamma                65.891(3)
_cell_formula_units_Z            1
_cell_length_a                   14.5520(5)
_cell_length_b                   14.6344(5)
_cell_length_c                   15.0327(6)
_cell_measurement_reflns_used    17137
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.89
_cell_measurement_theta_min      3.60
_cell_volume                     2669.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3875
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31449
_diffrn_reflns_theta_full        71.90
_diffrn_reflns_theta_max         71.90
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         10473
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.4385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                9658
_reflns_number_total             10473
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja502974c_si_004.cif
_cod_data_source_block           2_sub2
_cod_depositor_comments
'Adding full bibliography for 4121890--4121895.cif.'
_cod_original_cell_volume        2669.02(17)
_cod_database_code               4121890