The base-free multicomponent polymerization of elemental sulfur, difluoromethylene phosphobetaine and amines toward electron-deficient aromatic polythioureas
Yu, Yongjiang; Chen, Wang; Hu, Rongrong; Tang, Ben Zhong; Polymer Chemistry 16 (2025) 1509–1518; doi:10.1039/D4PY01387E

data_1573897
_publ_section_title
;
 The base-free multicomponent polymerization of elemental sulfur,
 difluoromethylene phosphobetaine and amines toward electron-deficient
 aromatic polythioureas
;
_journal_issue                   13
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1509
_journal_page_last               1518
_journal_paper_doi               10.1039/D4PY01387E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C17 H20 N2 S'
_chemical_formula_sum            'C17 H20 N2 S'
_chemical_formula_weight         284.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-03 deposited with the CCDC.	2025-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7780(2)
_cell_length_b                   9.33460(10)
_cell_length_c                   30.4546(4)
_cell_measurement_reflns_used    10677
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      76.8550
_cell_measurement_theta_min      2.8670
_cell_volume                     3063.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00  69.00   0.50    0.06    --  107.18 -57.00 150.00   68
  2  \w     35.00  69.00   0.50    0.06    --  107.18 -57.00 120.00   68
  3  \w     35.00  69.00   0.50    0.06    --  107.18 -57.00 -60.00   68
  4  \w     35.00  69.00   0.50    0.06    --  107.18 -57.00 -90.00   68
  5  \w     35.00  67.00   0.50    0.06    --  107.18 -56.00-134.00   64
  6  \w    -27.00  29.00   0.50    0.05    --   47.13 -19.00-150.00  112
  7  \w     90.00 178.00   0.50    0.06    --  107.18  95.00-123.00  176
  8  \w     94.00 178.00   0.50    0.06    --  107.18  38.00  30.00  168
  9  \w    -27.00  29.00   0.50    0.05    --   47.13 -19.00 120.00  112
 10  \w    -23.00  28.00   0.50    0.05    --  -47.13  19.00 150.00  102
 11  \w    -23.00  28.00   0.50    0.05    --  -47.13  19.00  30.00  102
 12  \w    -63.00 -30.00   0.50    0.06    -- -103.00  57.00  90.00   66
 13  \w   -119.00 -60.00   0.50    0.05    --  -47.13 -57.00 120.00  118
 14  \w   -174.00 -81.00   0.50    0.06    -- -103.00 -75.00  12.00  186
 15  \w   -119.00 -32.00   0.50    0.05    --  -47.13 -56.00-134.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0434060000
_diffrn_orient_matrix_UB_12      -0.0332862000
_diffrn_orient_matrix_UB_13      -0.0470989000
_diffrn_orient_matrix_UB_21      -0.0855216000
_diffrn_orient_matrix_UB_22      -0.1322807000
_diffrn_orient_matrix_UB_23      -0.0010733000
_diffrn_orient_matrix_UB_31      -0.1059437000
_diffrn_orient_matrix_UB_32      0.0930559000
_diffrn_orient_matrix_UB_33      -0.0183803000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            15574
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.285
_diffrn_reflns_theta_min         2.902
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
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    1.233
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0528P)^2^+1.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2818
_reflns_number_total             3129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py01387e2.cif
_cod_data_source_block           chns_auto
_cod_depositor_comments
'Adding full bibliography for 1573892--1573897.cif.'
_cod_database_code               1573897
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNS
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.814
_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 Secondary CH2 refined with riding coordinates:
 C006(H00a,H00b), C00C(H00d,H00e)
2.b Aromatic/amide H refined with riding coordinates:
 N002(H002), N003(H003), C008(H008), C009(H009), C00B(H00c), C00D(H00f),
 C00E(H00g), C00G(H00h), C00H(H00i), C00I(H00j)
2.c Idealised Me refined as rotating group:
 C00J(H00k,H00l,H00m), C00K(H00n,H00o,H00p)
;
_shelx_res_checksum              57674
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.178
_oxdiff_exptl_absorpt_empirical_full_min 0.461