Mechanistic Insights into C-H Amination via Dicopper Nitrenes
Mae Joanne B. Aguila; Yosra M. Badiei; Timothy H. Warren; Journal of the American Chemical Society 135 (2013) 9399–9406; doi:10.1021/ja400879m

data_4119961
_publ_contact_author             'Timothy H. Warren'
_publ_contact_author_email       thw@georgetown.edu
_publ_section_title
;
 Mechanistic Insights into C-H Amination via Dicopper Nitrenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9399
_journal_page_last               9406
_journal_paper_doi               10.1021/ja400879m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C42.50 H43 Cl8 Cu2 N5'
_chemical_formula_sum            'C42.5 H43 Cl8 Cu2 N5'
_chemical_formula_weight         1034.50
_chemical_name_common            {Cl2NN]Cu}2(NC6H11)
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 94.2220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.290(2)
_cell_length_b                   10.9720(10)
_cell_length_c                   37.221(4)
_cell_measurement_reflns_used    9379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.188
_cell_measurement_theta_min      2.591
_cell_volume                     9078.3(15)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics
'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl.Cryst. 30, 565'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0943
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            38294
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta. Cryst. (1995) A51 33-38'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9875
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                5885
_reflns_number_total             9875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400879m_si_004.cif
_cod_data_source_block           '[{Cl2NN]Cu}2(NC6H11)'
_cod_original_cell_volume        9078.2(15)
_cod_original_formula_sum        'C42.50 H43 Cl8 Cu2 N5'
_cod_database_code               4119961