Electronic substituent effect on the conformation of a phenylalanine-incorporated cyclic peptide
Asano, Akiko; Kawanami, Yukiko; Fujita, Mao; Yano, Yuta; Ide, Rio; Minoura, Katsuhiko; Kato, Takuma; Doi, Mitsunobu; RSC Advances 14 (2024) 1062–1071; doi:10.1039/D3RA07836A

data_7247942
_publ_section_title
;
 Electronic substituent effect on the conformation of a
 phenylalanine-incorporated cyclic peptide
;
_journal_issue                   2
_journal_name_full               'RSC Advances'
_journal_page_first              1062
_journal_page_last               1071
_journal_paper_doi               10.1039/D3RA07836A
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C40 H47 F3 N8 O6 S2, C3 H6 O'
_chemical_formula_sum            'C43 H53 F3 N8 O7 S2'
_chemical_formula_weight         915.05
_chemical_name_systematic        Phe(4cf3)_ASC
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.097(4)
_cell_angle_beta                 80.867(4)
_cell_angle_gamma                84.776(4)
_cell_formula_units_Z            1
_cell_length_a                   9.4424(4)
_cell_length_b                   9.8919(4)
_cell_length_c                   12.9370(6)
_cell_measurement_reflns_used    4809
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.0320
_cell_measurement_theta_min      5.4560
_cell_volume                     1172.74(9)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single & P200K'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17517
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        63.685
_diffrn_reflns_theta_max         63.685
_diffrn_reflns_theta_min         4.547
_diffrn_source                   rotating-anode
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             482
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1688 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.500
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.567
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1268
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3550
_refine_ls_wR_factor_ref         0.3792
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                4779
_reflns_number_total             6940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra07836a2.cif
_cod_data_source_block           201219_Phecf3
_cod_database_code               7247942
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              86032
_shelx_hkl_checksum              78414