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_4038855
_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'
_chemical_formula_weight         1292.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 110.677(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.701(2)
_cell_length_b                   38.079(6)
_cell_length_c                   14.624(2)
_cell_measurement_reflns_used    7062
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      2.33
_cell_volume                     7659.2(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43291
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.898
_diffrn_reflns_theta_min         1.069
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.135
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         17481
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+4.1670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8919
_reflns_number_total             17481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01876_si_002.cif
_cod_data_source_block           Tanaka1
_cod_original_cell_volume        7659(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4038855
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              93786
_shelx_hkl_checksum              31375
_shelx_fab_checksum              68460