Selective Convergence to Atropisomers of a Porphyrin Derivative Having Bulky Substituents at the Periphery.
Ishizuka, Tomoya; Tanaka, Shogo; Uchida, Sayaka; Wei, Lianyu; Kojima, Takahiko; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01876

data_4038857
_publ_section_title
;
 Selective Convergence to Atropisomers of a Porphyrin Derivative Having
 Bulky Substituents at the Periphery.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01876
_journal_year                    2020
_chemical_formula_sum            'C87.5 H83 Cl3 F6 N4 O10 S2'
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_cell_angle_beta                 90.434(2)
_cell_angle_gamma                99.096(2)
_cell_formula_units_Z            2
_cell_length_a                   15.715(2)
_cell_length_b                   15.840(2)
_cell_length_c                   16.452(2)
_cell_measurement_reflns_used    6182
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.63
_cell_volume                     4010.0(9)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.990
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.893
_diffrn_reflns_theta_min         1.248
_exptl_absorpt_coefficient_mu    0.243
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1706
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         17366
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.033
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_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.7545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             17366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01876_si_002.cif
_cod_data_source_block           Tanaka13
_cod_original_cell_volume        4010.0(10)
_cod_original_formula_sum        'C87.50 H83 Cl3 F6 N4 O10 S2'
_cod_database_code               4038857
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              62511
_shelx_hkl_checksum              83064