Chiral spherical aromatic amides: one-step synthesis and their stereochemical/chiroptical properties.
Koike, Daiki; Masu, Hyuma; Kikkawa, Shoko; Chiba, Ayako; Kamohara, Kaho; Okuda, Arisa; Hikawa, Hidemasa; Azumaya, Isao; Organic & biomolecular chemistry 23 (2024) 145–150; doi:10.1039/d4ob01458h

data_7160224
_publ_section_title
;
 Chiral spherical aromatic amides: one-step synthesis and their
 stereochemical/chiroptical properties.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              145
_journal_page_last               150
_journal_paper_doi               10.1039/d4ob01458h
_journal_volume                  23
_journal_year                    2024
_chemical_formula_moiety         'C42 H42 N6 O6'
_chemical_formula_sum            'C42 H42 N6 O6'
_chemical_formula_weight         726.83
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-09-05 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.206(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.4033(5)
_cell_length_b                   9.78786(18)
_cell_length_c                   21.6095(7)
_cell_measurement_reflns_used    29184
_cell_measurement_temperature    93
_cell_measurement_theta_max      73.23
_cell_measurement_theta_min      2.62
_cell_volume                     3577.57(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55003
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.612
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1536.00
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1329P)^2^+1.0003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5023
_reflns_number_total             6489
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d4ob01458h2.cif
_cod_data_source_block           ach049_01_CF-THF_
_cod_depositor_comments
'Adding full bibliography for 7160223--7160224.cif.'
_cod_database_code               7160224
_shelx_res_checksum              14826