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_4113132
_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 Cu N4 O2 S'
_chemical_formula_sum            'C23 H27 Cu N4 O2 S'
_chemical_formula_weight         487.09
_chemical_name_common            Cu(I)PETAEA
_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                 98.325(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2403(13)
_cell_length_b                   14.5902(10)
_cell_length_c                   13.2472(9)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      7.9
_cell_volume                     2149.6(3)
_computing_cell_refinement       'Siemens P3-PC'
_computing_data_collection       'Siemens P3-PC'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.1, XP (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      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3107
_diffrn_reflns_theta_full        56.10
_diffrn_reflns_theta_max         56.10
_diffrn_reflns_theta_min         4.53
_diffrn_standards_decay_%        14
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28 (1995)
53-56.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0537P)^2^+1.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                2114
_reflns_number_total             2804
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja045003gsi20040923_080942_1.cif
_cod_data_source_block           mn1499
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4113132