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_4121891
_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
'C56 H74 Cu2 N6 O4 S2, 2(C24 B F20), 1.29(C4 H8 O)'
_chemical_formula_sum            'C109.14 H84.29 B2 Cu2 F40 N6 O5.29 S2'
_chemical_formula_weight         2537.25
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                112.681(2)
_cell_angle_beta                 99.1365(17)
_cell_angle_gamma                108.1586(19)
_cell_formula_units_Z            1
_cell_length_a                   14.1218(3)
_cell_length_b                   15.1886(3)
_cell_length_c                   15.4437(3)
_cell_measurement_reflns_used    23910
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.96
_cell_measurement_theta_min      3.46
_cell_volume                     2753.21(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43222
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.899
_diffrn_reflns_theta_min         3.271
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.530
_exptl_crystal_description       'small needle'
_exptl_crystal_F_000             1283.4
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         10705
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0581P)^2^+1.6279P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9596
_reflns_number_total             10705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502974c_si_006.cif
_cod_data_source_block           3_sub2
_cod_depositor_comments
'Adding full bibliography for 4121890--4121895.cif.'
_cod_original_cell_volume        2753.20(11)
_cod_database_code               4121891
_shelxl_version_number           2013-2
_shelx_res_checksum              4699
_shelx_hkl_checksum              90763
_shelx_fab_checksum              82788