Double helices of dissymmetrical α,α'-disubstituted tripyrrins.
Fukuda, Yui; Akamatsu, Yuki; Umetani, Masataka; Kise, Koki; Kato, Kenichi; Osuka, Atsuhiro; Tanaka, Takayuki; Organic & biomolecular chemistry 21 (2023) 1158–1162; doi:10.1039/d2ob02125k

data_7159076
_publ_section_title
;
 Double helices of dissymmetrical &#x3b1;,&#x3b1;'-disubstituted
 tripyrrins.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1158
_journal_page_last               1162
_journal_paper_doi               10.1039/d2ob02125k
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C41 H29 F6 N5 O, C H2 Cl2'
_chemical_formula_sum            'C42 H31 Cl2 F6 N5 O'
_chemical_formula_weight         806.62
_chemical_name_systematic
1-(4-methoxyphenylamino)-14-(3,5-bis(trifluoromethyl)phenylamino)tripyrrin
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.6554(4)
_cell_length_b                   15.7158(2)
_cell_length_c                   16.5684(2)
_cell_measurement_reflns_used    18151
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.7210
_cell_measurement_theta_min      3.1070
_cell_volume                     7458.73(17)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Hybrid Pixel Array Detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23156
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.000
_diffrn_reflns_theta_min         3.085
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         6615
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1245P)^2^+14.7822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6089
_reflns_number_total             6615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob02125k2.cif
_cod_data_source_block           191223fukuda_a
_cod_depositor_comments
'Adding full bibliography for 7159075--7159076.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7159076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              34774