5,20-Diheterohexaphyrins: metal-template-free synthesis and aromaticity switching
Umetani, Masataka; Kim, Jinseok; Tanaka, Takayuki; Kim, Dongho; Osuka, Atsuhiro; Chemical Communications  (2019) –; doi:10.1039/C9CC05580K

data_7123963
_publ_section_title
;
 5,20-Diheterohexaphyrins: metal-template-free synthesis and aromaticity
 switching
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05580K
_journal_year                    2019
_chemical_formula_moiety         'C52 H34 N6 S2'
_chemical_formula_sum            'C52 H34 N6 S2'
_chemical_formula_weight         806.97
_chemical_name_systematic        5,20-dithiahexaphyrin
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-15 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.555(7)
_cell_length_b                   19.539(7)
_cell_length_c                   22.727(9)
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      30.3
_cell_volume                     7796(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1431
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            91194
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.998
_diffrn_reflns_theta_max         65.998
_diffrn_reflns_theta_min         6.756
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1970P)^2^+19.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.3486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3758
_reflns_number_total             6716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05580k2.cif
_cod_data_source_block           160601um
_cod_database_code               7123963
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              44447