β-Diketiminate Ligand Backbone Structural Effects on Cu(I)/O2 Reactivity: Unique Copper-Superoxo and Bis(μ-oxo) Complexes
Douglas J. E. Spencer; Nermeen W. Aboelella; Anne M. Reynolds; Patrick L. Holland; William B. Tolman; Journal of the American Chemical Society 124 (2002) 2108–2109; doi:10.1021/ja017820b

data_4114665
_publ_section_title
;
 \b-Diketiminate Ligand Backbone Structural Effects on Cu(I)/O2
 Reactivity: Unique Copper-Superoxo and Bis(\m-oxo) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2108
_journal_page_last               2109
_journal_paper_doi               10.1021/ja017820b
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        'Patrick Holland'
_chemical_formula_moiety         'C31 H44 Cu N3'
_chemical_formula_sum            'C31 H44 Cu N3'
_chemical_formula_weight         522.23
_chemical_name_common            00079
_chemical_name_systematic
;
 L(iPr)Cu(NCMe)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 126.494(1)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   31.3411(13)
_cell_length_b                   18.1396(7)
_cell_length_c                   22.9236(9)
_cell_measurement_reflns_used    7977
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     10477.0(7)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        XPREP
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26849
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             3678.2
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                6515
_reflns_number_total             9249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017820b_2.cif
_cod_data_source_block           79s
_cod_original_cell_volume        10477(1)
_cod_database_code               4114665