Rapid C-H Bond Activation by a Monocopper(III)-Hydroxide Complex
Patrick J. Donoghue; Jacqui Tehranchi; Christopher J. Cramer; Ritimukta Sarangi; Edward I. Solomon; William B. Tolman; Journal of the American Chemical Society 133 (2011) 17602–17605; doi:10.1021/ja207882h

data_4107071
_publ_section_title
;
 Rapid C-H Bond Activation by a Monocopper(III)-Hydroxide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17602
_journal_page_last               17605
_journal_paper_doi               10.1021/ja207882h
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C31 H38 Cu N3 O3,C36 H30 N P2, 6(C4 H8 O)'
_chemical_formula_sum            'C91 H83 Cu N4 O9 P2'
_chemical_formula_weight         1502.09
_chemical_name_common            10129
_chemical_name_systematic        PPN[CupyN2ipr2OH]
_chemical_properties_physical    air-sensitive
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   15.023(3)
_cell_length_b                   17.813(3)
_cell_length_c                   30.480(5)
_cell_measurement_reflns_used    4051
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.38
_cell_volume                     8157(3)
_computing_cell_refinement       'SMART, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_publication_material  '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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            52255
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_correction_T_min  0.8380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_recrystallization_method 'diethyl ether, tetrahydrofuran'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         18417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                12157
_reflns_number_total             18417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207882h_si_003_1.cif
_cod_data_source_block           PPN[CupyN2ipr2OH]
_cod_original_cell_volume        8156(3)
_cod_database_code               4107071