Direct Synthesis of High-Valent Aryl-Cu(II) and Aryl-Cu(III) Compounds: Mechanistic Insight into Arene C-H Bond Metalation.
Zhang, Hu; Yao, Bo; Zhao, Liang; Wang, De-Xian; Xu, Bo-Qing; Wang, Mei-Xiang; Journal of the American Chemical Society 136 (2014) 6326–6332; doi:10.1021/ja412615h

data_4121731
_publ_section_title
;
 Direct Synthesis of High-Valent Aryl-Cu(II) and Aryl-Cu(III) Compounds:
 Mechanistic Insight into Arene C-H Bond Metalation.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6326
_journal_page_last               6332
_journal_paper_doi               10.1021/ja412615h
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C26 H26 Cl Cu N7 O5, Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C26 H27 Cl2 Cu N7 O9.5'
_chemical_formula_weight         723.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.860(11)
_cell_angle_beta                 78.930(12)
_cell_angle_gamma                74.040(9)
_cell_formula_units_Z            2
_cell_length_a                   10.334(2)
_cell_length_b                   11.469(3)
_cell_length_c                   12.422(3)
_cell_measurement_reflns_used    5005
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.86
_cell_volume                     1380.4(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 ver 1.1'
_computing_publication_material  'SHELX97 (Sheldrick, 2008)'
_computing_structure_refinement  'Olex2 ver 1.1'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17678
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6294
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0615P)^2^+1.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                5960
_reflns_number_total             6294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja412615h_si_002.cif
_cod_data_source_block           sa2889
_cod_depositor_comments
'Adding full bibliography for 4121731--4121733.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26 H27 Cl2 Cu N7 O9.50'
_cod_database_code               4121731