Recyclable Sulfone-Containing Polymers via Ring-Opening Polymerization of Macroheterocyclic Siloxane Monomers: Synthesis, Properties and Recyclability
Guo, Mengdong; Huang, Yue; Cao, Jinfeng; Sun, Guibao; Zhao, Xia; Zhang, Jie; Feng, Shengyu; Polymer Chemistry  (2019) –; doi:10.1039/C9PY01363F

data_1552455
_publ_section_title
;
 Recyclable Sulfone-Containing Polymers via Ring-Opening Polymerization of
 Macroheterocyclic Siloxane Monomers: Synthesis, Properties and
 Recyclability
;
_journal_name_full               'Polymer Chemistry'
_journal_paper_doi               10.1039/C9PY01363F
_journal_year                    2019
_chemical_formula_moiety         'C16 H28 O5 S2 Si2'
_chemical_formula_sum            'C16 H28 O5 S2 Si2'
_chemical_formula_weight         420.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                78.460(3)
_cell_angle_beta                 84.048(3)
_cell_angle_gamma                78.306(3)
_cell_formula_units_Z            2
_cell_length_a                   6.2499(2)
_cell_length_b                   9.4654(3)
_cell_length_c                   19.2084(5)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0950
_cell_measurement_theta_min      4.9460
_cell_volume                     1087.88(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.988
_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    -93.00 -67.00   1.00    0.10    --  -48.45 141.00 -19.00   26
  2  \w    -97.00 -54.00   1.00    0.10    --  -48.45 128.00 168.00   43
  3  \w    -79.00 -54.00   1.00    1.20    --  -86.25 128.00 168.00   25
  4  \w    -96.00 -45.00   1.00    1.20    --  -86.25 141.00 -19.00   51
  5  \w     92.00 134.00   1.00    1.20    --  107.75  77.00 150.00   42
  6  \w    143.00 169.00   1.00    1.20    --  107.75  77.00 150.00   26
  7  \w     90.00 150.00   1.00    1.20    --  107.75 128.00 168.00   60
  8  \w     93.00 176.00   1.00    1.20    --  107.75 125.00 120.00   83
  9  \w     82.00 113.00   1.00    1.20    --  107.75 141.00 -19.00   31
 10  \w     96.00 177.00   1.00    1.20    --  107.75  37.00-120.00   81
 11  \w     53.00  78.00   1.00    0.10    --   48.45-128.00  94.00   25
 12  \w     82.00 115.00   1.00    1.20    --  107.75-125.00 -60.00   33
 13  \w     35.00  61.00   1.00    1.20    --  107.75-125.00 -60.00   26
 14  \w     59.00 107.00   1.00    1.20    --  107.75 -99.00  90.00   48
 15  \w     82.00 121.00   1.00    1.20    --  107.75-128.00  94.00   39
 16  \w     64.00 128.00   1.00    1.20    --  107.75-141.00 -77.00   64
 17  \w     41.00 104.00   1.00    0.10    --   48.45-141.00 -77.00   63
 18  \w   -120.00 -26.00   1.00    0.10    --  -48.45 -77.00  90.00   94
 19  \w   -159.00-115.00   1.00    1.20    --  -86.25 -57.00 150.00   44
 20  \w   -110.00 -72.00   1.00    1.20    --  -86.25 -57.00 150.00   38
 21  \w   -137.00-112.00   1.00    1.20    --  -86.25-128.00  94.00   25
 22  \w   -110.00 -69.00   1.00    0.10    --  -48.45-128.00  94.00   41
 23  \w   -117.00 -75.00   1.00    0.10    --  -48.45-125.00  60.00   42
 24  \w   -119.00 -62.00   1.00    0.10    --  -48.45-141.00 -77.00   57
 25  \w     37.00  63.00   1.00    1.20    --  107.75 -57.00  90.00   26
 26  \w     75.00 122.00   1.00    1.20    --  107.75 -57.00  90.00   47
 27  \w     36.00 116.00   1.00    1.20    --  107.75 -37.00  30.00   80
 28  \w     47.00 105.00   1.00    1.20    --  107.75 -57.00-120.00   58
 29  \w     45.00 119.00   1.00    1.20    --  107.75 -37.00-150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1770986000
_diffrn_orient_matrix_UB_12      0.0584714000
_diffrn_orient_matrix_UB_13      0.0545699000
_diffrn_orient_matrix_UB_21      -0.1401191000
_diffrn_orient_matrix_UB_22      0.0885566000
_diffrn_orient_matrix_UB_23      -0.0612039000
_diffrn_orient_matrix_UB_31      -0.1124268000
_diffrn_orient_matrix_UB_32      -0.1316413000
_diffrn_orient_matrix_UB_33      0.0024344000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10149
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         4.991
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
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    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0694P)^2^+1.2918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3180
_reflns_number_total             3858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py01363f2.cif
_cod_data_source_block           180305b
_cod_original_cell_volume        1087.90(6)
_cod_database_code               1552455
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         SiOSCH
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 98.85
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              12285
_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 3.190
_oxdiff_exptl_absorpt_empirical_full_min 0.584