Ring-opening terpolymerisation of phthalic thioanhydride with carbon dioxide and epoxides
Stühler, Merlin R.; Gallizioli, Cesare; Rupf, Susanne M.; Plajer, Alex J.; Polymer Chemistry 14 (2023) 4848–4855; doi:10.1039/D3PY01022H

data_1570093
_publ_section_title
;
 Ring-opening terpolymerisation of phthalic thioanhydride with carbon
 dioxide and epoxides
;
_journal_issue                   42
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4848
_journal_page_last               4855
_journal_paper_doi               10.1039/D3PY01022H
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C24 H23 Cr N2 O7, C H4 O'
_chemical_formula_sum            'C25 H27 Cr N2 O8'
_chemical_formula_weight         535.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-29
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-08-29 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                98.341(3)
_cell_angle_beta                 100.448(3)
_cell_angle_gamma                115.303(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7338(8)
_cell_length_b                   10.8127(8)
_cell_length_c                   11.6585(9)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.45
_cell_volume                     1164.70(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38482
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.449
_diffrn_reflns_theta_min         2.152
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.8773.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0706P)^2^+2.4682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3663
_reflns_number_total             4276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01022h2.cif
_cod_data_source_block           p-1
_cod_depositor_comments          'Adding full bibliography for 1570093.cif.'
_cod_original_cell_volume        1164.70(15)
_cod_database_code               1570093
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C16(H16),
 C22(H22), C23(H23), C24(H24), C26(H26)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C70(H70A,H70B,
 H70C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              27327
_olex2_submission_special_instructions 'No special instructions were received'