Interfacial Ring-Opening Polymerization of Amino-Acid-Derived N-Thiocarboxyanhydrides Toward Well-Defined Polypeptides
Cao, Jinbao; Siefker, David; Chan, Brandon A.; Yu, Tianyi; Lu, Lu; Saputra, Mirza A.; Fronczek, Frank R.; Xie, Weiwei; Zhang, Donghui; ACS Macro Letters 6 (2017) 836–; doi:10.1021/acsmacrolett.7b00411

data_4516805
_publ_section_title
;
 Interfacial Ring-Opening Polymerization of Amino-Acid-Derived
 N-Thiocarboxyanhydrides Toward Well-Defined Polypeptides
;
_journal_issue                   8
_journal_name_full               'ACS Macro Letters'
_journal_page_first              836
_journal_paper_doi               10.1021/acsmacrolett.7b00411
_journal_volume                  6
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C7 H11 N O2 S'
_chemical_formula_sum            'C7 H11 N O2 S'
_chemical_formula_weight         173.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2424(9)
_cell_length_b                   23.4593(18)
_cell_length_c                   5.5565(4)
_cell_measurement_reflns_used    1428
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      22.70
_cell_measurement_theta_min      3.03
_cell_volume                     1726.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9114
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.710
_diffrn_reflns_theta_min         1.766
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 849 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0367P)^2^+0.1040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2527
_reflns_number_total             3290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz7b00411_si_004.cif
_cod_data_source_block           JCao3
_cod_database_code               4516805
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              45348
_shelx_hkl_checksum              28058