Effects of Electron-Deficient β-Diketiminate and Formazan Supporting Ligands on Copper(I)-Mediated Dioxygen Activation
Sungjun Hong; Lyndal M. R. Hill; Aalo K. Gupta; Benjamin D. Naab; Joe B. Gilroy; Robin G. Hicks; Christopher J. Cramer; William B. Tolman; Inorganic Chemistry 48 (2009) 4514–4523; doi:10.1021/ic9002466

data_4302138
_publ_section_title
;
Effects of Electron-Deficient \b-Diketiminate and Formazan Supporting
Ligands on Copper(I)-Mediated Dioxygen Activation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4514
_journal_page_last               4523
_journal_paper_doi               10.1021/ic9002466
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C54 H74 Cu2 N12 O4'
_chemical_formula_sum            'C27 H37 Cu N6 O2'
_chemical_formula_weight         541.16
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            8
_cell_length_a                   18.4379(15)
_cell_length_b                   18.0101(14)
_cell_length_c                   17.1820(14)
_cell_measurement_reflns_used    2825
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.37
_cell_volume                     5705.6(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36511
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.813768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,R.Blessing,1995
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.713
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10093
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1109P)^2^+1.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                6823
_reflns_number_total             10093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9002466_si_002_3.cif
_cod_data_source_block           08214b
_cod_database_code               4302138