Tandem Incorporation of Enantiomeric Residues Engenders Discrete Peptoid Structures.
Gorske, Benjamin C.; Mumford, Emily M.; Conry, Rebecca R.; Organic letters 18 (2016) 2780–2783; doi:10.1021/acs.orglett.6b01283

data_1555584
_publ_section_title
;
 Tandem Incorporation of Enantiomeric Residues Engenders Discrete Peptoid
 Structures.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2780
_journal_page_last               2783
_journal_paper_doi               10.1021/acs.orglett.6b01283
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C49 H55 N3 O6'
_chemical_formula_weight         781.96
_chemical_name_common            bcg1-109a
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.2970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9668(15)
_cell_length_b                   13.1573(15)
_cell_length_c                   13.5181(15)
_cell_measurement_reflns_used    2320
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      21.8435
_cell_measurement_theta_min      1.6172
_cell_volume                     2176.7(4)
_computing_cell_refinement       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 v2015.9-0 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20186
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.245
_refine_ls_abs_structure_details
;

Flack x determined using 3466 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         10204
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0442P)^2^+0.3092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                8883
_reflns_number_total             10204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01283_si_001.cif
_cod_data_source_block           BG01
_cod_database_code               1555584
_shelx_res_checksum              81643
_shelx_hkl_checksum              60411