Synthesis and chiroptical properties of cylindrical macrocycles comprising two calix[3]aramide moieties.
Saito, Yuuki; Satake, Misa; Mori, Ryuichi; Okayasu, Misaki; Masu, Hyuma; Tominaga, Masahide; Katagiri, Kosuke; Yamaguchi, Kentaro; Kikkawa, Shoko; Hikawa, Hidemasa; Azumaya, Isao; Organic & biomolecular chemistry 18 (2020) 230–236; doi:10.1039/c9ob02022e

data_7157161
_publ_section_title
;
 Synthesis and chiroptical properties of cylindrical macrocycles
 comprising two calix[3]aramide moieties.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              230
_journal_page_last               236
_journal_paper_doi               10.1039/c9ob02022e
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C45 H39 N3 O3'
_chemical_formula_sum            'C45 H39 N3 O3'
_chemical_formula_weight         669.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-09-10 deposited with the CCDC.    2019-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.6839(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.47394(8)
_cell_length_b                   19.77494(10)
_cell_length_c                   19.02693(13)
_cell_measurement_reflns_used    23816
_cell_measurement_temperature    93
_cell_measurement_theta_max      73.08
_cell_measurement_theta_min      3.23
_cell_volume                     3490.77(4)
_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 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (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 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45193
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.259
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.819
_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    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416.00
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.2085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5691
_reflns_number_total             6325
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9ob02022e2.cif
_cod_data_source_block           ysa166-02_dcm-nHex
_cod_depositor_comments
'Adding full bibliography for 7157160--7157161.cif.'
_cod_database_code               7157161
_shelx_res_checksum              41994