Pseudopeptosomes: non-lipidated vesicular assemblies from bispidine-appended pseudopeptides.
Singh, Hanuman; Pragya, Pragya; Mittal, Aditya; Haridas, V.; Organic & biomolecular chemistry 21 (2023) 3557–3566; doi:10.1039/d3ob00201b

data_7159232
_publ_section_title
;
 Pseudopeptosomes: non-lipidated vesicular assemblies from
 bispidine-appended pseudopeptides.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3557
_journal_page_last               3566
_journal_paper_doi               10.1039/d3ob00201b
_journal_volume                  21
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H52 N4 O6'
_chemical_formula_sum            'C29 H52 N4 O6'
_chemical_formula_weight         552.760
_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'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.219(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6858(4)
_cell_length_b                   26.2740(17)
_cell_length_c                   11.3518(7)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.40
_cell_volume                     1948.9(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9976
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            64410
_diffrn_reflns_point_group_measured_fraction_full 0.9990
_diffrn_reflns_point_group_measured_fraction_max 0.9970
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.55
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6801
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1543 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.9120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.942
_exptl_crystal_description       needle
_exptl_crystal_F_000             604.288
_refine_diff_density_max         0.1646
_refine_diff_density_min         -0.1813
_refine_diff_density_rms         0.0408
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.8(4)
_refine_ls_d_res_high            0.7492
_refine_ls_d_res_low             13.1370
_refine_ls_extinction_coef       0.025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     363
_refine_ls_number_reflns         9644
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.9874
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          -0.0019
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.996
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              34
_reflns_limit_k_min              -34
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                4909
_reflns_number_total             9644
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ob00201b2.cif
_cod_data_source_block           BL2
_cod_depositor_comments
'Adding full bibliography for 7159232--7159233.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7159232
_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. Rigid body (RIGU) restrains
 C12, C17, C13, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, N4, H4, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C25, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12), C20(H20), C15(H15), C22(H22), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C21(H21a,H21b), C16(H16a,H16b), C18(H18a,H18b), C14(H14a,
 H14b), C13(H13a,H13b), C4(H4a,H4b)
3.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1)
3.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C29(H29a,H29b,H29c), C28(H28a,H28b,H28c), C3(H3a,H3b,
 H3c), C9(H9a,H9b,H9c), C27(H27a,H27b,H27c), C8(H8a,H8b,H8c), C23(H23a,H23b,
 H23c), C24(H24a,H24b,H24c), C1(H1a,H1b,H1c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'