Pseudodiproline (Pro-Cyp) Oligomers Fold into Helical Polyproline Type secondary structures
Garsi, Jean-Baptiste; Aguiar, Pedro M.; Berger, Gilles; Maris, Thierry; Hanessian, Stephen; Journal of Organic Chemistry 89 (2024) 4283–4293; doi:10.1021/acs.joc.3c02840

data_4039027
_publ_section_title
;
 Pseudodiproline (Pro-Cyp) Oligomers Fold into Helical Polyproline Type
 secondary structures
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4283
_journal_page_last               4293
_journal_paper_doi               10.1021/acs.joc.3c02840
_journal_volume                  89
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H46 N2 O7'
_chemical_formula_sum            'C28 H46 N2 O7'
_chemical_formula_weight         522.67
_chemical_name_systematic
;
tert-Butyl (S)-2-((S)-hydroxy((1R,2R)-2-((S)-2-((S)-hydroxy-
((1R,2R)-2-(methoxycarbonyl)cyclopentyl)methyl)pyrrolidine-1-
carbonyl)cyclopentyl)methyl)pyrrolidine-1-carboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-15
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_cell_angle_alpha                90
_cell_angle_beta                 100.471(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8992(4)
_cell_length_b                   6.1645(2)
_cell_length_c                   35.2338(11)
_cell_measurement_reflns_used    4801
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.053
_cell_measurement_theta_min      2.550
_cell_volume                     2755.03(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Quazar MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18561
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.176
_diffrn_reflns_theta_min         2.550
_diffrn_source                   'Microfocus Source'
_diffrn_source_current           0.65
_diffrn_source_power             0.02912
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_diffrn_source_voltage           44.8
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.4027
_exptl_absorpt_correction_T_min  0.2893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1618 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.7184.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4899
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0514P)^2^+0.2943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.853
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                4588
_reflns_number_total             4899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            han588.cif
_cod_data_source_block           han588
_cod_database_code               4039027
_cod_database_fobs_code 4039027