Effect of a <i>cis</i>-4-aminopiperidine-3-carboxylic acid (<i>cis</i>-APiC) residue on mixed-helical folding of unnatural peptides.
Choi, Sunglim; Shim, Jihyun; Kang, Philjae; Choi, Soo Hyuk; Organic & biomolecular chemistry 20 (2022) 613–618; doi:10.1039/d1ob02223g

data_7158453
_publ_section_title
;
 Effect of a <i>cis</i>-4-aminopiperidine-3-carboxylic acid
 (<i>cis</i>-APiC) residue on mixed-helical folding of unnatural peptides.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              613
_journal_page_last               618
_journal_paper_doi               10.1039/d1ob02223g
_journal_volume                  20
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C48 H73 N7 O9'
_chemical_formula_sum            'C48 H73 N7 O9'
_chemical_formula_weight         892.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-06 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.685(9)
_cell_length_b                   10.180(2)
_cell_length_c                   12.884(3)
_cell_measurement_reflns_used    60124
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.868
_cell_measurement_theta_min      2.290
_cell_volume                     5571(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_number            12496
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         1.625
_diffrn_source                   'Fixed gap multiple wiggler beamline'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12496
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0885P)^2^+1.6423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                11687
_reflns_number_total             12496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob02223g2.cif
_cod_data_source_block           SLIX004
_cod_depositor_comments
'Adding full bibliography for 7158451--7158453.cif.'
_cod_database_code               7158453
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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:
 C5(H5), C10(H10), C14(H14), C19(H19), C23(H23), C28(H28), C39(H39), C44(H44),
 C48(H48), C53(H53)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C24(H24A,H24B), C26(H26A,H26B),
 C27(H27A,H27B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C58(H58A,H58B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N11(H11), N20(H20), N36(H36), N45(H45), N54(H54), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              35322
_shelx_hkl_checksum              99178
_shelx_fab_checksum              10637
_olex2_submission_special_instructions 'No special instructions were received'