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_4129871
_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         'C67 H73 N5 O Zn, 0.5(C4 H8 O)'
_chemical_formula_sum            'C69 H77 N5 O1.5 Zn'
_chemical_formula_weight         1065.75
_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                93.09(3)
_cell_angle_beta                 104.28(4)
_cell_angle_gamma                116.22(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2483(7)
_cell_length_b                   14.6134(10)
_cell_length_c                   18.0800(18)
_cell_measurement_reflns_used    2097
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      25.8
_cell_volume                     2989.3(11)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35041
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         6.58
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1.36
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         9284
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1315P)^2^+10.8257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2458
_reflns_number_gt                6932
_reflns_number_total             9284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b11223_si_005.cif
_cod_data_source_block           50313ds
_cod_original_cell_volume        2989.4(4)
_cod_database_code               4129871