Toluene and Ethylbenzene Aliphatic C-H Bond Oxidations Initiated by a Dicopper(II)-μ-1,2-Peroxo Complex
Heather R. Lucas; Lei Li; Amy A. Narducci Sarjeant; Michael A. Vance; Edward I. Solomon; Kenneth D. Karlin; Journal of the American Chemical Society 131 (2009) 3230–3245; doi:10.1021/ja807081d

data_4104259
_publ_section_title
;
 Toluene and Ethylbenzene Aliphatic C-H Bond Oxidations Initiated by a
 Dicopper(II)-\m-1,2-Peroxo Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3230
_journal_page_last               3245
_journal_paper_doi               10.1021/ja807081d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'C46 H54 Cl2 Cu2 N6 O2, 2(C24 B F20), C0.94 H1.88 Cl1.88'
_chemical_formula_sum            'C47.47 H27.94 B Cl1.94 Cu F20 N3 O'
_chemical_formula_weight         1179.43
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Jun 10 10:47:06 2005'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.056(4)
_cell_angle_beta                 82.456(4)
_cell_angle_gamma                85.222(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1990(5)
_cell_length_b                   12.4156(5)
_cell_length_c                   16.1018(7)
_cell_measurement_reflns_used    16690
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.4990
_cell_measurement_theta_min      3.9861
_cell_volume                     2310.08(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega scans'
_diffrn_orient_matrix_UB_11      0.0274506841
_diffrn_orient_matrix_UB_12      -0.0532214975
_diffrn_orient_matrix_UB_13      0.0020706737
_diffrn_orient_matrix_UB_21      -0.0372697816
_diffrn_orient_matrix_UB_22      -0.0102619343
_diffrn_orient_matrix_UB_23      -0.0268432507
_diffrn_orient_matrix_UB_31      0.0361274677
_diffrn_orient_matrix_UB_32      0.0252384672
_diffrn_orient_matrix_UB_33      -0.0377202774
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43084
_diffrn_reflns_resolution_max    0.74
_diffrn_reflns_theta_full        28.56
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         3.99
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.93976
_exptl_absorpt_correction_T_min  0.82561
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET)
(compiled Mar  2 2005,09:02:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1177.5
_exptl_crystal_size_max          0.15545
_exptl_crystal_size_mid          0.08767
_exptl_crystal_size_min          0.03647
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         11737
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+1.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                9297
_reflns_number_total             11737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807081d_si_002.cif
_cod_data_source_block           x0123
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4104259
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET)
(compiled Mar  2 2005,09:02:11)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET)
(compiled Mar  2 2005,09:02:11)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET)
(compiled Mar  2 2005,09:02:11)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET)
(compiled Mar  2 2005,09:02:11)
;
_cell_measurement_resolution_max 0.74
_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        'Lei Li'
_jhu_scientist_phone             x6-6557
_jhu_scientist_email             lli1@jhu.edu
_jhu_identifying_number          x0123
_jhu_xray_labbook                88
_jhu_crystalization_labbook      n%2Fa
_jhu_crystalization_solvent      'Methylene Chloride'
_jhu_crystalization_method
;
;
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              2