Cu(I)-Amido Complexes in the Ullmann Reaction: Reactions of Cu(I)-Amido Complexes with Iodoarenes with and without Autocatalysis by CuI
Ramesh Giri; John F. Hartwig; Journal of the American Chemical Society 132 (2010) 15860–15863; doi:10.1021/ja105695s

data_4103491
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Cu(I)-Amido Complexes in the Ullmann Reaction: Reactions of Cu(I)-Amido
 Complexes with Iodoarenes with and without Autocatalysis by CuI
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15860
_journal_page_last               15863
_journal_paper_doi               10.1021/ja105695s
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C24 H20 Cu N2, C24 H16 Cu N4'
_chemical_formula_sum            'C48 H36 Cu2 N6'
_chemical_formula_weight         823.91
_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
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.185(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7968(12)
_cell_length_b                   13.1593(7)
_cell_length_c                   13.3171(7)
_cell_measurement_reflns_used    6225
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.48
_cell_volume                     3770.8(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba84has
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29784
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.7421
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_id                ba84has
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         3501
_refine_ls_number_restraints     1174
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.8411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                2673
_reflns_number_total             3501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105695s_si_002.cif
_cod_data_source_block           test
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4103491