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_4107072
_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 H37 Cl Cu N3 O2,C36 H30 N P2,5(C4 H8 O)'
_chemical_formula_sum            'C87 H75 Cl Cu N4 O7 P2'
_chemical_formula_weight         1449.44
_chemical_name_common            10173s
_chemical_name_systematic        PPN[CupyN2ipr2Cl]
_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                   15.0982(16)
_cell_length_b                   17.8967(19)
_cell_length_c                   30.531(3)
_cell_measurement_reflns_used    4008
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.21
_cell_volume                     8249.7(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            69464
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.9275
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             2836
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         18841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                13034
_reflns_number_total             18841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207882h_si_003_2.cif
_cod_data_source_block           PPN[CupyN2ipr2Cl]
_cod_original_cell_volume        8249.6(15)
_cod_database_code               4107072