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_1543840
_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         'C46 H14 F20 N4 O, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C47.5 H17 Cl3 F20 N4 O'
_chemical_formula_weight         1146.00
_space_group_IT_number           2
_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                65.355(14)
_cell_angle_beta                 88.006(11)
_cell_angle_gamma                86.758(12)
_cell_formula_units_Z            2
_cell_length_a                   10.2204(18)
_cell_length_b                   14.8005(13)
_cell_length_c                   15.9075(12)
_cell_measurement_reflns_used    1835
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      26.11
_cell_volume                     2183.4(5)
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25930
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         6.59
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.4872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         6787
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[s^2^(Fo^2^)+(0.1622P)^2^+4.7167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2377
_refine_ls_wR_factor_ref         0.2480
_reflns_number_gt                5396
_reflns_number_total             6787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01377_si_002.cif
_cod_data_source_block           41020m2'
_cod_original_formula_sum        'C47.50 H17 Cl3 F20 N4 O'
_cod_database_code               1543840