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_7247941
_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         'C39 H49 I N8 O6 S2, 0.5(C4 H9 N O)'
_chemical_formula_sum            'C41 H53.5 I N8.5 O6.5 S2'
_chemical_formula_weight         959.94
_chemical_name_systematic        Phe(4I)_ASC
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.337(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7742(6)
_cell_length_b                   21.7130(16)
_cell_length_c                   15.1389(6)
_cell_measurement_reflns_used    8857
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5900
_cell_measurement_theta_min      3.5250
_cell_volume                     4526.5(4)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26294
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.920
_diffrn_source                   rotating-anode
_exptl_absorpt_coefficient_mu    6.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1982.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.104
_refine_diff_density_min         -2.411
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Flack x determined using 2754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         13407
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.1093
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2930
_refine_ls_wR_factor_ref         0.3125
_reflns_Friedel_coverage         0.572
_reflns_Friedel_fraction_full    0.609
_reflns_Friedel_fraction_max     0.606
_reflns_number_gt                9911
_reflns_number_total             13407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra07836a2.cif
_cod_data_source_block           phe4i
_cod_depositor_comments
;

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C82 H106 I2 N17 O13 S4'
_cod_original_formula_weight         1919.88
_cod_original_formula_moiety
'C39 H48 I N8 O6 S2, C39 H49 I N8 O6 S2, C4 H9 N O'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7247941
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              22383
_shelx_hkl_checksum              29508