Doubly N-Methylated Porphyrinoids.
Naito, Wakana; Yasuda, Nobuhiro; Morimoto, Tatsuki; Shigeta, Yasuteru; Takaya, Hikaru; Hisaki, Ichiro; Maeda, Hiromitsu; Organic letters 18 (2016) 3006–3009; doi:10.1021/acs.orglett.6b01377

data_1543835
_publ_section_title
;
 Doubly N-Methylated Porphyrinoids.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              3006
_journal_page_last               3009
_journal_paper_doi               10.1021/acs.orglett.6b01377
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C31 H11 F15 N2 O2'
_chemical_formula_sum            'C31 H11 F15 N2 O2'
_chemical_formula_weight         728.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 116.512(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   29.637(7)
_cell_length_b                   11.513(2)
_cell_length_c                   36.067(7)
_cell_measurement_reflns_used    5958
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      25.2
_cell_volume                     11012(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            132734
_diffrn_reflns_theta_full        68.48
_diffrn_reflns_theta_max         68.48
_diffrn_reflns_theta_min         6.68
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.8039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1801
_refine_ls_number_reflns         20133
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0773
_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^)+(0.1650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2329
_reflns_number_gt                11555
_reflns_number_total             20133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01377_si_002.cif
_cod_data_source_block           50319m3
_cod_depositor_comments
;

2019-01-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_moiety     '4(C31 H11 F15 N2 O2) '
_cod_original_formula_sum        'C124 H44 F60 N8 O8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2913.67
_cod_database_code               1543835