Kinetic and Mechanistic Aspects of Atom Transfer Radical Addition (ATRA) Catalyzed by Copper Complexes with Tris(2-pyridylmethyl)amine
William T. Eckenhoff; Ashley B. Biernesser; Tomislav Pintauer; Inorganic Chemistry 51 (2012) 11917–11929; doi:10.1021/ic3018198

data_4330940
_publ_section_title
;
 Kinetic and Mechanistic Aspects of Atom Transfer Radical Addition (ATRA)
 Catalyzed by Copper Complexes with Tris(2-pyridylmethyl)amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11917
_journal_page_last               11929
_journal_paper_doi               10.1021/ic3018198
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C56 H48 Cu N P3, C3 H6 O, Cl O4'
_chemical_formula_sum            'C59 H54 Cl Cu N O5 P3'
_chemical_formula_weight         1048.93
_chemical_name_common            '[Cu(PPh3)3(CH3CN)][ClO4]'
_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                102.7740(10)
_cell_angle_beta                 104.3170(10)
_cell_angle_gamma                95.2620(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5153(8)
_cell_length_b                   13.4234(10)
_cell_length_c                   19.3711(14)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.126
_cell_measurement_theta_min      2.1515
_cell_volume                     2552.6(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'ORTEP-3 for Windows (Faruggia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       '\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_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29164
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.12
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         26054
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.8297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         14156
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0598P)^2^+0.7676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                11813
_reflns_number_total             14156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3018198_si_002_3.cif
_cod_data_source_block           '[Cu(PPh3)3(CH3CN)][ClO4]'
_cod_database_code               4330940