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_7159233
_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         'C39 H50 N6 O6, H2 O'
_chemical_formula_sum            'C39 H52 N6 O7'
_chemical_formula_weight         716.884
_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                 112.53(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.650(13)
_cell_length_b                   9.887(10)
_cell_length_c                   15.827(16)
_cell_measurement_reflns_used    1445
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      19.783
_cell_measurement_theta_min      2.490
_cell_volume                     1973(3)
_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 0.9778
_diffrn_measured_fraction_theta_max 0.9778
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.1647
_diffrn_reflns_Laue_measured_fraction_full 0.9778
_diffrn_reflns_Laue_measured_fraction_max 0.9778
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11416
_diffrn_reflns_point_group_measured_fraction_full 0.8516
_diffrn_reflns_point_group_measured_fraction_max 0.8516
_diffrn_reflns_theta_full        24.9995
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5222
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1527 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.7003.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       needle
_exptl_crystal_F_000             768.368
_refine_diff_density_max         0.2870
_refine_diff_density_min         -0.2954
_refine_diff_density_rms         0.0714
_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   -2.3(18)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             12.1166
_refine_ls_extinction_coef       0.022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0396
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     470
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.0368
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.708
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              11
_reflns_limit_k_min              -10
_reflns_limit_l_max              18
_reflns_limit_l_min              -16
_reflns_number_gt                3069
_reflns_number_total             5912
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ob00201b2.cif
_cod_data_source_block           BW2
_cod_depositor_comments
'Adding full bibliography for 7159232--7159233.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7159233
_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, All O(H,H) groups
2. Rigid body (RIGU) restrains
 O6, C2, C1, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Riding coordinates:
 O7(H7c,H7d)
3.b Ternary CH refined with riding coordinates:
 C18(H18), C25(H25), C6(H6a), C21(H21)
3.c Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b), C20(H20a,H20b), C17(H17a,H17b), C19(H19a,H19b), C22(H22a,
 H22b), C23(H23a,H23b), C7(H7a,H7b)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N5(H5), N6(H6), C33(H33), C36(H36), C37(H37), C9(H9),
 C15(H15), C39(H39), C38(H38), C12(H12), C14(H14), C13(H13)
3.e Idealised Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C28(H28a,H28b,H28c),
 C29(H29a,H29b,H29c), C30(H30a,H30b,H30c)
;
_olex2_submission_special_instructions 'No special instructions were received'