Copper(I)-α-Ketocarboxylate Complexes: Characterization and O2 Reactions That Yield Copper-Oxygen Intermediates Capable of Hydroxylating Arenes
Sungjun Hong; Stefan M. Huber; Laura Gagliardi; Christopher C. Cramer; William B. Tolman; Journal of the American Chemical Society 129 (2007) 14190–14192; doi:10.1021/ja0760426

data_4110181
_publ_section_title
;
 Copper(I)-\a-Ketocarboxylate Complexes: Characterization and O2 Reactions
 That Yield Copper-Oxygen Intermediates Capable of Hydroxylating Arenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14190
_journal_page_last               14192
_journal_paper_doi               10.1021/ja0760426
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C28 H32 Cu F3 N2 O3 S'
_chemical_formula_sum            'C28 H32 Cu F3 N2 O3 S'
_chemical_formula_weight         597.16
_chemical_name_common            '[(N2-XY)Cu(OTf)]'
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.702(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4571(11)
_cell_length_b                   13.8773(10)
_cell_length_c                   15.4330(12)
_cell_measurement_reflns_used    3263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.37
_cell_volume                     2840.9(4)
_computing_cell_refinement       SAINT,Bruker
_computing_data_collection       SMART,Bruker
_computing_data_reduction        SAINT,Bruker
_computing_molecular_graphics    SHELXTL,Bruker
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector,omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18007
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.845885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,R.Blessing 1995'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.744
_refine_diff_density_min         -1.724
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+5.5519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                4477
_reflns_number_total             5015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0760426si20070810_064252.cif
_cod_data_source_block           06264b
_cod_database_code               4110181