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_4103492
_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         'C36 H24 K N6, C24 H20 Cu N2'
_chemical_formula_sum            'C60 H44 Cu K N8'
_chemical_formula_weight         979.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.536(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4811(9)
_cell_length_b                   25.167(2)
_cell_length_c                   18.0748(14)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.29
_cell_volume                     4687.3(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  ba45i2as
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73918
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.9213
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_id                ba45i2as
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 0 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+3.0686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                6802
_reflns_number_total             8608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105695s_si_003.cif
_cod_data_source_block           ba45i2as
_cod_depositor_comments
;

2021-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_moiety     'C72 H48 K2 N12, 2(C24 H20 Cu N2)'
_cod_original_formula_sum        'C120 H88 Cu2 K2 N16'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1959.34
_cod_database_code               4103492