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_4115125
_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        'Elizabeth Lewis'
_chemical_formula_moiety         'C36 H59 N4 O2 Cu2, C S O3 F3'
_chemical_formula_sum            'C37 H59 Cu2 F3 N4 O5 S'
_chemical_formula_weight         856.02
_chemical_name_common            02148
_chemical_name_systematic        L1Cu(O)2CuL2
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.0198(19)
_cell_length_b                   26.0198(19)
_cell_length_c                   40.147(6)
_cell_measurement_reflns_used    2770
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      47.195
_cell_measurement_theta_min      4.366
_cell_volume                     23539(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
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            40462
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.819587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       block
_exptl_crystal_F_000             8100
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                6449
_reflns_number_total             9230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027164v_s2_1.cif
_cod_data_source_block           02148
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115125