Polymers from sugars and isothiocyanates: ring-opening copolymerization of a d-xylose anhydrosugar oxetane
Clark, Ella F.; Kociok-Köhn, Gabriele; Davidson, Matthew G.; Buchard, Antoine; Polymer Chemistry 14 (2023) 2838–2847; doi:10.1039/D3PY00443K

data_1569198
_publ_section_title
;
 Polymers from sugars and isothiocyanates: ring-opening copolymerization
 of a d-xylose anhydrosugar oxetane
;
_journal_issue                   23
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2838
_journal_page_last               2847
_journal_paper_doi               10.1039/D3PY00443K
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H15 F6 N O4 S'
_chemical_formula_sum            'C17 H15 F6 N O4 S'
_chemical_formula_weight         443.36
_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
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-31 deposited with the CCDC.	2023-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2334(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.47055(6)
_cell_length_b                   23.5365(3)
_cell_length_c                   14.44919(14)
_cell_measurement_reflns_used    15344
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.7930
_cell_measurement_theta_min      4.8330
_cell_volume                     1855.37(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1365)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29409
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.045
_diffrn_reflns_theta_min         3.597
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 2953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7096
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0318
_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^+0.3987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                6725
_reflns_number_total             7096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00443k2.cif
_cod_data_source_block           s22ab2
_cod_depositor_comments          'Adding full bibliography for 1569198.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1569198
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.677
_shelx_estimated_absorpt_t_max   0.892
_oxdiff_exptl_absorpt_empirical_full_min 0.850
_oxdiff_exptl_absorpt_empirical_full_max 1.309
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              33621