Cooperative Intramolecular Hydrogen Bonding Strongly Enforces cis-Peptoid Folding
Wijaya, Andrew W.; Nguyen, Andy I.; Roe, Leah T.; Butterfoss, Glenn L.; Spencer, Ryan K.; Li, Nan K.; Zuckermann, Ronald N.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10497

data_4132345
_publ_section_title
;
 Cooperative Intramolecular Hydrogen Bonding Strongly Enforces cis-Peptoid
 Folding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10497
_journal_year                    2019
_chemical_formula_sum            'C42.5 H54 B N3 O2'
_chemical_formula_weight         649.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.7610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4964(2)
_cell_length_b                   19.2489(2)
_cell_length_c                   16.72120(10)
_cell_measurement_reflns_used    48671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.7310
_cell_measurement_theta_min      3.5480
_cell_volume                     7546.37(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            98025
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        74.000
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         15400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0474P)^2^+2.1757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13239
_reflns_number_total             15400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10497_si_002.cif
_cod_data_source_block           AIN_3_56
_cod_original_cell_volume        7546.38(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C42.50 H54 B N3 O2'
_cod_database_code               4132345
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              99355
_shelx_hkl_checksum              52099