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_4121893
_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         'C22 H33 Cl Cu N3 O6 S, Cl O4'
_chemical_formula_sum            'C22 H33 Cl2 Cu N3 O10 S'
_chemical_formula_weight         666.01
_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                93.826(3)
_cell_angle_beta                 95.153(2)
_cell_angle_gamma                99.590(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5031(2)
_cell_length_b                   9.9656(3)
_cell_length_c                   16.9854(5)
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.08
_cell_volume                     1408.57(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      150(2)
_diffrn_detector_area_resol_mean 15.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19209
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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            blue
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.8853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                5847
_reflns_number_total             6467
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja502974c_si_003.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4121890--4121895.cif.'
_cod_database_code               4121893