Seeding Crystals, Harvesting Polypeptides: Preparing Long Chiral-Sequence Controlled Polypeptides by Interlocked Polymerization in Cocrystals (iPiC) of N-Thiocarboxyanhydride (NTA) at Room Temperature
Bai, Tianwen; Zhou, Peng; Li, Zixian; Zheng, Botuo; Ling, Jun; Macromolecules  (2021) –; doi:10.1021/acs.macromol.1c00371

data_1564145
_publ_section_title
;
 Seeding Crystals, Harvesting Polypeptides: Preparing Long Chiral-Sequence
 Controlled Polypeptides by Interlocked Polymerization in Cocrystals
 (iPiC) of N-Thiocarboxyanhydride (NTA) at Room Temperature
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.1c00371
_journal_year                    2021
_chemical_formula_moiety         'C6 H9 N O2 S2'
_chemical_formula_sum            'C6 H9 N O2 S2'
_chemical_formula_weight         191.26
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-30
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Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
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_cell_angle_alpha                90
_cell_angle_beta                 101.719(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1451(16)
_cell_length_b                   7.7606(7)
_cell_length_c                   9.2513(10)
_cell_measurement_reflns_used    1239
_cell_measurement_temperature    170.9
_cell_measurement_theta_max      29.4032
_cell_measurement_theta_min      3.1281
_cell_volume                     853.79(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.9
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -21.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       10.8433   77.0000   90.0000 103

  2 omega  -21.00   49.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183   38.0000  -30.0000 70
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0329318000
_diffrn_orient_matrix_UB_12      0.0564116000
_diffrn_orient_matrix_UB_13      -0.0339946000
_diffrn_orient_matrix_UB_21      -0.0258829000
_diffrn_orient_matrix_UB_22      0.0720184000
_diffrn_orient_matrix_UB_23      0.0267398000
_diffrn_orient_matrix_UB_31      0.0423964000
_diffrn_orient_matrix_UB_32      -0.0000457000
_diffrn_orient_matrix_UB_33      0.0653013000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.134
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0490P)^2^+1.8685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1296
_reflns_number_total             1563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00371_si_002.cif
_cod_data_source_block           161229_sc_metdl
_cod_original_cell_volume        853.78(17)
_cod_database_code               1564145
_chemical_oxdiff_formula         'c10 h10 n2 o8 S1'
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.770
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              51332
_shelx_hkl_checksum              43595
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'