Cationic ring-opening polymerization of a five membered cyclic dithiocarbonate having a tertiary amine moiety
Krishnamurthy, Suvratha; Yoshida, Yoshiaki; Endo, Takeshi; Polymer Chemistry 13 (2022) 267–274; doi:10.1039/D1PY01230D

data_1565763
_publ_section_title
;
 Cationic ring-opening polymerization of a five membered cyclic
 dithiocarbonate having a tertiary amine moiety
;
_journal_issue                   2
_journal_name_full               'Polymer Chemistry'
_journal_page_first              267
_journal_page_last               274
_journal_paper_doi               10.1039/D1PY01230D
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H19 N O S2'
_chemical_formula_sum            'C18 H19 N O S2'
_chemical_formula_weight         329.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4425(4)
_cell_length_b                   10.2492(3)
_cell_length_c                   19.6013(8)
_cell_measurement_reflns_used    6167
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.0790
_cell_measurement_theta_min      4.8680
_cell_volume                     1696.08(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_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    -23.00  60.00   0.50    5.00    --   46.42 -56.00 176.00  166
  2  \w    -80.00 -55.00   0.50    5.00    -- -102.00  68.00 159.00   50
  3  \w   -107.00 -82.00   0.50    5.00    -- -102.00 109.00  40.00   50
  4  \w     48.00 107.00   0.50    5.00    --  104.15-109.00 -55.00  118
  5  \w    105.00 158.00   0.50    5.00    --  104.15  56.00 -40.00  106
  6  \w     -5.00  29.00   0.50    5.00    --  -46.42  19.00 120.00   68
  7  \w    -19.00  25.00   0.50    5.00    --  -46.42  19.00-120.00   88
  8  \w     26.00  61.00   0.50    5.00    --   46.42-125.00  60.00   70
  9  \w     69.00  94.00   0.50    5.00    --   46.42-125.00  60.00   50
 10  \w    -69.00 -44.00   0.50    5.00    -- -102.00  61.00 120.00   50
 11  \w    -66.00 -40.00   0.50    5.00    -- -102.00  61.00-120.00   52
 12  \w    -71.00 -29.00   0.50    5.00    -- -102.00 109.00  40.00   84
 13  \w    -70.00 -29.00   0.50    5.00    -- -102.00  61.00   0.00   82
 14  \w    -69.00 -31.00   0.50    5.00    -- -102.00  61.00  30.00   76
 15  \w     68.00 105.00   0.50    5.00    --  104.15 -94.00-150.00   74
 16  \w     32.00  93.00   0.50    5.00    --  104.15 -94.00 120.00  122
 17  \w     32.00 105.00   0.50    5.00    --  104.15 -94.00 -60.00  146
 18  \w     44.00 106.00   0.50    5.00    --  104.15 -94.00 150.00  124
;
_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      -0.1764548000
_diffrn_orient_matrix_UB_12      -0.0372513000
_diffrn_orient_matrix_UB_13      0.0030407000
_diffrn_orient_matrix_UB_21      0.0232817000
_diffrn_orient_matrix_UB_22      -0.0925849000
_diffrn_orient_matrix_UB_23      -0.0610192000
_diffrn_orient_matrix_UB_31      0.0397277000
_diffrn_orient_matrix_UB_32      -0.1124912000
_diffrn_orient_matrix_UB_33      0.0494619000
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9646
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.223
_diffrn_reflns_theta_min         4.512
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.114a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1294 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.056(6)
_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     199
_refine_ls_number_reflns         3384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0269P)^2^+0.5322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                3240
_reflns_number_total             3384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py01230d2.cif
_cod_data_source_block           bn-dtc3_auto
_cod_depositor_comments          'Adding full bibliography for 1565763.cif.'
_cod_database_code               1565763
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'block, colorless'
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.859
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C9(H9A,H9B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C5(H5), C12(H12), C4(H4), C15(H15), C3(H3), C14(H14),
 C13(H13), C2(H2)
;
_shelx_res_checksum              96334
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.794