Simultaneous formation of helical and sheet-like assemblies from short azapeptides enables spontaneous resolution.
Yan, Xiaosheng; Weng, Peimin; Cao, Jinlian; Lin, Kexin; Qi, Yuanwei; Wu, Xin; Jiang, Yun-Bao; Nanoscale 16 (2024) 19221–19227; doi:10.1039/d4nr02872d

data_1572724
_publ_section_title
;
 Simultaneous formation of helical and sheet-like assemblies from short
 azapeptides enables spontaneous resolution.
;
_journal_issue                   41
_journal_name_full               Nanoscale
_journal_page_first              19221
_journal_page_last               19227
_journal_paper_doi               10.1039/d4nr02872d
_journal_volume                  16
_journal_year                    2024
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C17 H17 I N4 O2 S'
_chemical_formula_sum            'C17 H17 I N4 O2 S'
_chemical_formula_weight         468.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2527wd
_audit_creation_date             2020-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-21 deposited with the CCDC.	2024-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.65680(10)
_cell_length_b                   16.8731(4)
_cell_length_c                   22.9659(6)
_cell_measurement_reflns_used    3991
_cell_measurement_temperature    99.9(7)
_cell_measurement_theta_max      77.0270
_cell_measurement_theta_min      3.2390
_cell_volume                     1804.54(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.9(7)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6214
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.965
_diffrn_reflns_theta_min         3.250
_exptl_absorpt_coefficient_mu    15.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 944 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0410P)^2^+9.3880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.492
_reflns_Friedel_fraction_full    0.775
_reflns_Friedel_fraction_max     0.666
_reflns_number_gt                2978
_reflns_number_total             3149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02872d2.cif
_cod_data_source_block           exp_8447
_cod_depositor_comments
'Adding full bibliography for 1572720--1572724.cif.'
_cod_database_code               1572724
_shelx_shelxl_version_number     2014/8
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00D(H00D)
2.b Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), N007(H007), N008(H008), C00B(H00B), C00E(H00E),
 C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K), C00M(H00M), C00O(H00O),
 C00P(H00P)
2.c Idealised Me refined as rotating group:
 C00L(H00A,H00C,H00F)
;
_shelx_res_checksum              86236
_shelx_hkl_checksum              38586
_olex2_submission_special_instructions 'No special instructions were received'