Identification and Characterization of Monoanionic Tripodal Tetradentate Ligand Complexes of Copper(I) and Copper(II) Involved in Halogen Atom Transfer Reactions
Jocelyn M. Goodwin; Marilyn M. Olmstead; Timothy E. Patten; Journal of the American Chemical Society 126 (2004) 14352–14353; doi:10.1021/ja045003g

data_4113133
_publ_section_title
;
 Identification and Characterization of Monoanionic Tripodal Tetradentate
 Ligand Complexes of Copper(I) and Copper(II) Involved in Halogen Atom
 Transfer Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14352
_journal_page_last               14353
_journal_paper_doi               10.1021/ja045003g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C23 H27 Br Cu N4 O2 S,C4 H8 O'
_chemical_formula_sum            'C27 H35 Br Cu N4 O3 S'
_chemical_formula_weight         639.10
_chemical_name_common            BrCu(PETAEA)^.^THF
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.566(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.156(2)
_cell_length_b                   10.049(3)
_cell_length_c                   30.571(8)
_cell_measurement_reflns_used    454
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.7
_cell_volume                     2794.3(13)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.35 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.152
_diffrn_reflns_av_sigmaI/netI    0.225
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            18282
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                2402
_reflns_number_total             5316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja045003gsi20040923_080942_2.cif
_cod_data_source_block           mn1509
_cod_original_cell_volume        2794.4(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4113133