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_4038854
_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            'C85 H80 Cl2 N4 O4'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
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_cell_angle_alpha                90
_cell_angle_beta                 97.522(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.151(2)
_cell_length_b                   18.373(3)
_cell_length_c                   29.230(5)
_cell_measurement_reflns_used    3630
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.22
_cell_volume                     7002(2)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.1330
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25968
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.074
_diffrn_reflns_theta_min         1.312
_exptl_absorpt_coefficient_mu    0.148
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.626
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         11768
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1914
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1364P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             11768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01876_si_002.cif
_cod_data_source_block           Tanaka15
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4038854
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.996
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_shelx_fab_checksum              70741