Triarylporphyrin meso-Oxy Radicals: Remarkable Chemical Stabilities and Oxidation to Oxophlorin π-Cations.
Shimizu, Daiki; Oh, Juwon; Furukawa, Ko; Kim, Dongho; Osuka, Atsuhiro; Journal of the American Chemical Society 137 (2015) 15584–15594; doi:10.1021/jacs.5b11223

data_4129874
_publ_section_title
;
 Triarylporphyrin meso-Oxy Radicals: Remarkable Chemical Stabilities and
 Oxidation to Oxophlorin \p-Cations.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15584
_journal_page_last               15594
_journal_paper_doi               10.1021/jacs.5b11223
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C62 H72 N4 Ni O, C H3 O H'
_chemical_formula_sum            'C63 H76 N4 Ni O2'
_chemical_formula_weight         979.97
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                70.31(4)
_cell_angle_beta                 86.42(5)
_cell_angle_gamma                87.73(5)
_cell_formula_units_Z            2
_cell_length_a                   9.011(6)
_cell_length_b                   15.824(8)
_cell_length_c                   20.375(8)
_cell_measurement_reflns_used    1032
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      25.5
_cell_volume                     2730(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1463
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32121
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         6.51
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.600
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         8507
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_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+2.2212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2466
_refine_ls_wR_factor_ref         0.3013
_reflns_number_gt                4523
_reflns_number_total             8507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b11223_si_002.cif
_cod_data_source_block           50227ds
_cod_original_cell_volume        2730(2)
_cod_database_code               4129874