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_7157160
_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         'C87 H79 N6 O7'
_chemical_formula_sum            'C87 H79 N6 O7'
_chemical_formula_weight         1320.62
_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                 98.1145(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.89204(7)
_cell_length_b                   17.25623(10)
_cell_length_c                   28.41877(13)
_cell_measurement_reflns_used    64579
_cell_measurement_temperature    103
_cell_measurement_theta_max      73.08
_cell_measurement_theta_min      2.99
_cell_volume                     7229.95(6)
_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      103
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            142071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.004
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.741
_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    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2796.00
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         13221
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1048P)^2^+5.7324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11552
_reflns_number_total             13221
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9ob02022e2.cif
_cod_data_source_block           ysa084_hplc2_02-2_TL-Me
_cod_depositor_comments
'Adding full bibliography for 7157160--7157161.cif.'
_cod_database_code               7157160
_shelx_res_checksum              60152