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_7247945
_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_formula_moiety         'C39 H49 Cl N8 O6 S2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C40 H50.5 Cl N8.5 O6 S2'
_chemical_formula_weight         845.96
_chemical_name_systematic        Phe(4Cl)_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-2016/4
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6272(2)
_cell_length_b                   16.6962(2)
_cell_length_c                   16.1368(2)
_cell_measurement_reflns_used    33823
_cell_measurement_temperature    90
_cell_measurement_theta_max      74.1060
_cell_measurement_theta_min      2.7580
_cell_volume                     4191.37(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 5.881
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46819
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.452
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 7283 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         16582
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+12.0171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                16132
_reflns_number_total             16582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra07836a2.cif
_cod_data_source_block           phe4c
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C40 H50.50 Cl N8.50 O6 S2'
_cod_database_code               7247945
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              30725
_shelx_hkl_checksum              84010