Snapshots of Dioxygen Activation by Copper: The Structure of a 1:1 Cu/O2 Adduct and Its Use in Syntheses of Asymmetric Bis(μ-oxo) Complexes
Nermeen W. Aboelella; Elizabeth A. Lewis; Anne M. Reynolds; William W. Brennessel; Christopher J. Cramer; William B. Tolman; Journal of the American Chemical Society 124 (2002) 10660–10661; doi:10.1021/ja027164v

data_4115126
_publ_section_title
;
 Snapshots of Dioxygen Activation by Copper: The Structure of a 1:1 Cu/O2
 Adduct and Its Use in Syntheses of Asymmetric Bis(\m-oxo) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10660
_journal_page_last               10661
_journal_paper_doi               10.1021/ja027164v
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        'Nermeen W. Aboelella'
_chemical_formula_moiety         '3(C4 H8 O), C35 H53 Cu N2 O2'
_chemical_formula_sum            'C47 H77 Cu N2 O5'
_chemical_formula_weight         813.65
_chemical_name_common            02073
_chemical_name_systematic        (tbu)2LiPrCu(O2)
_space_group_IT_number           44
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2'
_symmetry_space_group_name_H-M   'I m m 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.464(4)
_cell_length_b                   17.324(4)
_cell_length_c                   8.763(2)
_cell_measurement_reflns_used    1242
_cell_measurement_temperature    173(2)
_cell_volume                     2347.6(10)
_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
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5614
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.677149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'bright green'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       needle
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2024
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0980P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                1523
_reflns_number_total             2024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027164v_s2_2.cif
_cod_data_source_block           02073
_cod_original_cell_volume        2348(1)
_cod_database_code               4115126