Increasing the Functional Group Diversity in Helical β-Peptoids: Achievement of Solvent- and pH-Dependent Folding
Wellhöfer, Isabelle; Beck, Janina; Frydenvang, Karla; Bräse, Stefan; Olsen, Christian A.; The Journal of Organic Chemistry  (2020) –; doi:10.1021/acs.joc.0c00780

data_4038685
_publ_contact_author
;
Karla Frydenvang
;
_publ_section_title
;
 Increasing the Functional Group Diversity in Helical \b-Peptoids:
 Achievement of Solvent- and pH-Dependent Folding
;
_journal_name_full               'The Journal of Organic Chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00780
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C17 H23 N O2 S'
_chemical_formula_weight         305.42
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 115.585(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6686(15)
_cell_length_b                   6.3122(4)
_cell_length_c                   11.3113(6)
_cell_measurement_reflns_used    21351
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      72.077
_cell_measurement_theta_min      3.818
_cell_volume                     1653.01(18)
_computing_cell_refinement       'APEX2 v2016 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21351
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.077
_diffrn_reflns_theta_min         3.818
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS-2016-2. Reference: Krause et al. J.Appl.Cryst. 48 (2015) 3-10.
Part of Apex2 Suite 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3090
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0430P)^2^+0.5952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.902
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                2741
_reflns_number_total             3090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c00780_si_004.cif
_cod_data_source_block           jbc-71f2
_cod_original_cell_volume        1653.01(17)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4038685
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.926