Control of Cu(II) and Cu(III) States in N-Confused Porphyrin by Protonation/Deprotonation at the Peripheral Nitrogen
Hiromitsu Maeda; Yuichi Ishikawa; Tomoyuki Matsuda; Atsuhiro Osuka; Hiroyuki Furuta; Journal of the American Chemical Society 125 (2003) 11822–11823; doi:10.1021/ja0356075

data_4114206
_publ_section_title
;
 Control of Cu(II) and Cu(III) States in N-Confused Porphyrin by
 Protonation/Deprotonation at the Peripheral Nitrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11822
_journal_page_last               11823
_journal_paper_doi               10.1021/ja0356075
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C44 H8 Cu F20 N4'
_chemical_formula_weight         1036.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   20.0878(10)
_cell_length_b                   20.0878(10)
_cell_length_c                   23.882(3)
_cell_measurement_reflns_used    2351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.86
_cell_measurement_theta_min      2.49
_cell_volume                     8345.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10503
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9437
_exptl_absorpt_correction_T_min  0.8210
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             4581
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         1942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+88.6209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2006
_reflns_number_gt                1398
_reflns_number_total             1942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0356075si20030729_035811.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        8345.7(11)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4114206