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_4110179
_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         'C35 H37 Cu N2 O3'
_chemical_formula_sum            'C35 H37 Cu N2 O3'
_chemical_formula_weight         597.21
_chemical_name_common            '[(N2XY)Cu(BF)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.812(10)
_cell_length_b                   14.651(9)
_cell_length_c                   15.986(9)
_cell_measurement_reflns_used    3725
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.19
_cell_volume                     3056(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28455
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,R.Blessing,1995
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5404
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+1.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                4529
_reflns_number_total             5404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0760426si20070810_064222.cif
_cod_data_source_block           07051b
_cod_database_code               4110179