Cyclic arylopeptoid oligomers: synthesis and conformational propensities of peptide-mimetic aromatic macrocycles.
Hayakawa, Masahide; Ohsawa, Ayaka; Takeda, Kumi; Torii, Ryo; Kitamura, Yoshiaki; Katagiri, Hiroshi; Ikeda, Masato; Organic & biomolecular chemistry 16 (2018) 8505–8512; doi:10.1039/c8ob01962b

data_7156415
_publ_section_title
;
 Cyclic arylopeptoid oligomers: synthesis and conformational propensities
 of peptide-mimetic aromatic macrocycles.
;
_journal_issue                   44
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8505
_journal_page_last               8512
_journal_paper_doi               10.1039/c8ob01962b
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C56 H60 N4 O6, 3(C H Cl3)'
_chemical_formula_sum            'C59 H63 Cl9 N4 O6'
_chemical_formula_weight         1243.18
_chemical_name_common            C[4]pAP(iBt-mBzl-iBt-mBzl)
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-06 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.526(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   5.74900(10)
_cell_length_c                   26.1364(7)
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_cell_measurement_temperature    93
_cell_measurement_theta_max      30.2970
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_cell_volume                     5870.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31702
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.673
_diffrn_source                   'Rotating Anode'
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_exptl_absorpt_correction_T_min  0.94488
_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    1.407
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5145
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0865
_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^)+(0.1525P)^2^+42.4736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2679
_refine_ls_wR_factor_ref         0.2767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4417
_reflns_number_total             5145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob01962b2.cif
_cod_data_source_block           160725_ikeda_cyclic_b
_cod_depositor_comments
'Adding full bibliography for 7156414--7156415.cif.'
_cod_database_code               7156415
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.962
_oxdiff_exptl_absorpt_empirical_full_min 0.932
_oxdiff_exptl_absorpt_empirical_full_max 1.056
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              3718