Insight into the synthesis of N-methylated polypeptides
Muhl, Christian; Zengerling, Lydia; Groß, Jonathan; Eckhardt, Paul; Opatz, Till; Besenius, Pol; Barz, Matthias; Polymer Chemistry 11 (2020) 6919–6927; doi:10.1039/D0PY01055C

data_1559293
_publ_section_title
;
 Insight into the synthesis of N-methylated polypeptides
;
_journal_issue                   43
_journal_name_full               'Polymer Chemistry'
_journal_page_first              6919
_journal_page_last               6927
_journal_paper_doi               10.1039/D0PY01055C
_journal_volume                  11
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C7 H11 N O3 S'
_chemical_formula_sum            'C7 H11 N O3 S'
_chemical_formula_weight         189.23
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.168(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9782(10)
_cell_length_b                   5.9102(5)
_cell_length_c                   9.3714(13)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      3.10
_cell_volume                     434.95(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      ' 211 frames, detector distance = 60 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3577
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.983
_diffrn_reflns_theta_min         3.096
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 574 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0783P)^2^+1.1204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                1637
_reflns_number_total             2055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py01055c2.cif
_cod_data_source_block           cmlz9-nca
_cod_depositor_comments
'Adding full bibliography for 1559292--1559293.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1559293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              88319