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_1572723
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2527vc
_audit_creation_date             2019-12-09
_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                   4.65650(10)
_cell_length_b                   16.8753(3)
_cell_length_c                   22.9925(4)
_cell_measurement_reflns_used    4415
_cell_measurement_temperature    100.1(2)
_cell_measurement_theta_max      69.4620
_cell_measurement_theta_min      3.2530
_cell_volume                     1806.75(6)
_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 n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5001
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        60.993
_diffrn_reflns_theta_max         60.993
_diffrn_reflns_theta_min         3.249
_exptl_absorpt_coefficient_mu    15.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06292
_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    1.722
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details
;
 Flack x determined using 872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2638
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1210P)^2^+0.0961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.886
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                2549
_reflns_number_total             2638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02872d2.cif
_cod_data_source_block           exp_7551
_cod_depositor_comments
'Adding full bibliography for 1572720--1572724.cif.'
_cod_database_code               1572723
_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. Uiso/Uaniso restraints and constraints
I001 \\sim C009 \\sim C00I \\sim C00F \\sim C00H \\sim C00L \\sim C00B \\sim
C00J \\sim O004 \\sim N006 \\sim C00G \\sim C00D \\sim C00K \\sim O003 \\sim
N005 \\sim N007 \\sim C00E \\sim S002 \\sim N008 \\sim C00A \\sim C00C \\sim
C00M \\sim C00N \\sim C00P \\sim C00O: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00G(H00G)
3.b Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), N007(H007), N008(H008), C00C(H00C), C00F(H00F),
 C00H(H00H), C00I(H00I), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P)
3.c Idealised Me refined as rotating group:
 C00D(H00A,H00B,H00D)
;
_shelx_res_checksum              36585
_shelx_hkl_checksum              79638
_olex2_submission_special_instructions 'No special instructions were received'