Acid-Base Properties of a Freebase Form of a Quadruply Ring-Fused Porphyrin-Stepwise Protonation Induced by Rigid Ring-Fused Structure.
Saegusa, Yuta; Ishizuka, Tomoya; Shiota, Yoshihito; Yoshizawa, Kazunari; Kojima, Takahiko; The Journal of organic chemistry 82 (2017) 322–330; doi:10.1021/acs.joc.6b02419

data_4032106
_publ_section_title
;
 Acid-Base Properties of a Freebase Form of a Quadruply Ring-Fused
 Porphyrin-Stepwise Protonation Induced by Rigid Ring-Fused Structure.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              322
_journal_page_last               330
_journal_paper_doi               10.1021/acs.joc.6b02419
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C60 H54 N4'
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_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.120(4)
_cell_angle_gamma                90
_cell_formula_units_Z            14
_cell_length_a                   20.774(5)
_cell_length_b                   29.800(8)
_cell_length_c                   30.233(8)
_cell_measurement_temperature    120(2)
_cell_volume                     17788(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.472
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.472
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97443
_diffrn_reflns_point_group_measured_fraction_full 0.472
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.404
_diffrn_reflns_theta_min         0.984
_exptl_absorpt_coefficient_mu    0.063
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       Plate
_exptl_crystal_F_000             6188
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2059
_refine_ls_number_reflns         15178
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0911
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+90.0894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2331
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_reflns_number_gt                10460
_reflns_number_total             15178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02419_si_002.cif
_cod_data_source_block           gusa41
_cod_depositor_comments          'Adding full bibliography for 4032106.cif.'
_cod_database_code               4032106
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2013-4
_shelx_res_checksum              91327
_shelx_hkl_checksum              37425