Sulfur Donor Atom Effects on Copper(I)/O2 Chemistry with Thioanisole Containing Tetradentate N3S Ligand Leading to μ-1,2-Peroxo-Dicopper(II) Species
Yunho Lee; Dong-Heon Lee; Ga Young Park; Heather R. Lucas; Amy A. Narducci Sarjeant; Matthew T. Kieber-Emmons; Michael A. Vance; Ashley E. Milligan; Edward I. Solomon; Kenneth D. Karlin; Inorganic Chemistry 49 (2010) 8873–8885; doi:10.1021/ic101041m

data_4316598
_publ_section_title
;
 Sulfur Donor Atom Effects on Copper(I)/O2 Chemistry with Thioanisole
 Containing Tetradentate N3S Ligand Leading to \m-1,2-Peroxo-Dicopper(II)
 Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8873
_journal_page_last               8885
_journal_paper_doi               10.1021/ic101041m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C20 H21 Cl Cu N3 O, C24 B F20, C4 H8 O'
_chemical_formula_sum            'C44 H29 B Cl Cu F20 N3 O2'
_chemical_formula_weight         1121.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu May 31 09:20:25 2007'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0065(2)
_cell_length_b                   21.9340(3)
_cell_length_c                   16.2954(2)
_cell_measurement_reflns_used    21400
_cell_measurement_theta_max      27.4992
_cell_measurement_theta_min      3.8580
_cell_volume                     4287.10(11)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_publication_material  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega phi scans'
_diffrn_orient_matrix_UB_11      0.0172001297
_diffrn_orient_matrix_UB_12      -0.0274248807
_diffrn_orient_matrix_UB_13      -0.0186418886
_diffrn_orient_matrix_UB_21      -0.0222525003
_diffrn_orient_matrix_UB_22      -0.0169828172
_diffrn_orient_matrix_UB_23      0.0324568822
_diffrn_orient_matrix_UB_31      -0.0519895004
_diffrn_orient_matrix_UB_32      -0.0017907606
_diffrn_orient_matrix_UB_33      -0.0222528293
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39965
_diffrn_reflns_resolution_max    0.77
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.87
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_voltage           50
_diffrn_standards_interval_count 2
_diffrn_standards_interval_time  50
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
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    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.7712
_exptl_crystal_size_mid          0.4026
_exptl_crystal_size_min          0.3108
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9882
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0532P)^2^+4.1083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                7270
_reflns_number_total             9882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101041m_si_001_1.cif
_cod_data_source_block           x0364
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4316598
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_cell_measurement_resolution_max 0.77
_jhu_your_name_here              'Dr. Amy A Sarjeant'
_jhu_your_lab_here               'NCB 240'
_jhu_your_phone_number_here      x6-8569
_jhu_your_email_here             xray@jhu.edu
_jhu_institutional_source        'Karlin Lab'
_jhu_submitting_scientist        'GaYoung Park'
_jhu_scientist_phone             x6-6161
_jhu_scientist_email             gpark8@jhu.edu
_jhu_identifying_number          x0364
_jhu_xray_labbook                II-69
_jhu_crystalization_labbook      GY-EOE
_jhu_crystalization_solvent      'Tetrahydrofuran, Ether'
_jhu_crystalization_method
;
;
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              2