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_4330941
_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         'C54 H45 Cu P3, C24 H20 B, C18 H15 P, C3 H6 O'
_chemical_formula_sum            'C99 H86 B Cu O P4'
_chemical_formula_weight         1489.91
_chemical_name_common            '[Cu(PPh3)3(PPh3)][BPh4]'
_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                91.395(2)
_cell_angle_beta                 91.568(3)
_cell_angle_gamma                90.929(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8893(6)
_cell_length_b                   15.7278(6)
_cell_length_c                   16.8133(6)
_cell_measurement_reflns_used    3789
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.22
_cell_volume                     3934.1(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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            113420
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_correction_T_min  0.8680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         18431
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0328P)^2^+1.4833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                16000
_reflns_number_total             18431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3018198_si_002_4.cif
_cod_data_source_block           '[Cu(PPh3)(PPh3)][BPh4]'
_cod_database_code               4330941