High-Tg PLA copolymers via base-catalyzed transesterification of PLA with 2,5,7-trioxabicyclo[2.2.2]octan-6-one
Zhou, Tong; Guo, Yu-Ting; Yang, Chun; Meng, Xian-Bin; Du, Fu-Sheng; Li, Zi-Chen; Polymer Chemistry 15 (2024) 156–165; doi:10.1039/D3PY01250F

data_1570474
_publ_section_title
;
 High-Tg PLA copolymers via base-catalyzed transesterification of PLA with
 2,5,7-trioxabicyclo[2.2.2]octan-6-one
;
_journal_issue                   3
_journal_name_full               'Polymer Chemistry'
_journal_page_first              156
_journal_page_last               165
_journal_paper_doi               10.1039/D3PY01250F
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C17 H20 O9'
_chemical_formula_sum            'C17 H20 O9'
_chemical_formula_weight         368.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-10-31 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.74180(10)
_cell_length_b                   34.0977(4)
_cell_length_c                   8.47780(10)
_cell_measurement_reflns_used    14056
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      74.8840
_cell_measurement_theta_min      2.5770
_cell_volume                     3394.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      170.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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     25.00 120.00   0.50    0.08    --   47.20  76.00 -36.00  190
  2  \w    -20.00  61.00   0.50    0.08    --   47.20 -56.00  51.00  162
  3  \w   -168.00 -91.00   0.50    0.20    --  -99.00 -56.00  51.00  154
  4  \w    -99.00 -56.00   0.50    0.20    --  -99.00  93.00  61.00   86
  5  \w     43.00  96.00   0.50    0.20    --  103.25 -76.00-163.00  106
  6  \w   -115.00 -89.00   0.50    0.08    --  -47.20-125.00-180.00   52
  7  \w   -112.00 -71.00   0.50    0.20    --  -99.00 125.00 120.00   82
  8  \w    -67.00 -26.00   0.50    0.20    --  -99.00  61.00 150.00   82
  9  \w    -61.00 -26.00   0.50    0.20    --  -99.00  56.00-165.00   70
 10  \w    -64.00 -38.00   0.50    0.20    --  -99.00  61.00  30.00   52
 11  \w    -55.00 -29.00   0.50    0.20    --  -99.00  61.00 -90.00   52
 12  \w     31.00 111.00   0.50    0.20    --  103.25-125.00   0.00  160
 13  \w     34.00  75.00   0.50    0.20    --  103.25 -61.00  30.00   82
 14  \w     93.00 163.00   0.50    0.20    --  103.25  45.00-120.00  140
 15  \w    138.00 169.00   0.50    0.20    --  103.25  77.00 -90.00   62
 16  \w     83.00 132.00   0.50    0.20    --  103.25  77.00 -90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0470376000
_diffrn_orient_matrix_UB_12      -0.0255688000
_diffrn_orient_matrix_UB_13      -0.0416780000
_diffrn_orient_matrix_UB_21      0.0740026000
_diffrn_orient_matrix_UB_22      -0.1490035000
_diffrn_orient_matrix_UB_23      -0.0042526000
_diffrn_orient_matrix_UB_31      -0.0976122000
_diffrn_orient_matrix_UB_32      -0.1007997000
_diffrn_orient_matrix_UB_33      0.0169149000
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19029
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.532
_diffrn_reflns_theta_min         2.592
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1942 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5758
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0640P)^2^+0.8559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.687
_reflns_Friedel_fraction_max     0.635
_reflns_number_gt                5557
_reflns_number_total             5758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01250f2.cif
_cod_data_source_block           tx5104
_cod_depositor_comments
'Adding full bibliography for 1570470--1570474.cif.'
_cod_database_code               1570474
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.97
_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
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9A), C11(H11), C14(H14), C16(H16), C9A(H9AB), C11A(H11A), C14A(H14A),
 C16A(H16A)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B), C15(H15A,H15B), C17(H17A,H17B),
 C7A(H7AA,H7AB), C10A(H10C,H10D), C12A(H12C,H12D), C15A(H15C,H15D), C17A(H17C,
 H17D)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2A(H2A), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O9A(H9AA)
;
_shelx_res_checksum              73970
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.691