Solvent-induced changes in the reactivity of tricyanate esters undergoing thermal polymerization
Galukhin, Andrey; Nikolaev, Ilya; Nosov, Roman; Islamov, Daut; Vyazovkin, Sergey; Polymer Chemistry 12 (2021) 6179–6187; doi:10.1039/D1PY01088C

data_1564903
_publ_section_title
;
 Solvent-induced changes in the reactivity of tricyanate esters undergoing
 thermal polymerization
;
_journal_issue                   42
_journal_name_full               'Polymer Chemistry'
_journal_page_first              6179
_journal_page_last               6187
_journal_paper_doi               10.1039/D1PY01088C
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C23 H15 N3 O3'
_chemical_formula_sum            'C23 H15 N3 O3'
_chemical_formula_weight         381.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-07-26 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6119(2)
_cell_length_b                   13.3664(2)
_cell_length_c                   8.87420(10)
_cell_measurement_reflns_used    7449
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.9530
_cell_measurement_theta_min      2.8660
_cell_volume                     1832.78(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_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    -27.00  28.00   0.50    0.05    --  -47.45  19.00 -90.00  110
  2  \w    -25.00  28.00   0.50    0.05    --  -47.45  19.00 -30.00  106
  3  \w     57.00  89.00   0.50    0.05    --   47.45 149.00 -60.00   64
  4  \w     76.00 119.00   0.50    0.05    --   47.45 125.00 -90.00   86
  5  \w     93.00 176.00   0.50    0.06    --  105.86  45.00 -30.00  166
  6  \w     58.00  84.00   0.50    0.05    --   47.45-122.00  56.00   52
  7  \w     58.00 104.00   0.50    0.06    --  105.86 -94.00  90.00   92
  8  \w     35.00  93.00   0.50    0.06    --  105.86 -77.00  60.00  116
  9  \w     41.00  67.00   0.50    0.06    --  105.86 -61.00 -60.00   52
 10  \w     40.00  66.00   0.50    0.06    --  105.86 -61.00-120.00   52
 11  \w     40.00  66.00   0.50    0.06    --  105.86 -61.00-150.00   52
 12  \w    -91.00 -23.00   0.50    0.05    --  -47.45 122.00 137.00  136
 13  \w    -58.00 -33.00   0.50    0.06    -- -105.86  77.00 -60.00   50
 14  \w   -106.00 -79.00   0.50    0.06    -- -105.86  77.00 -60.00   54
 15  \w   -126.00 -41.00   0.50    0.06    -- -105.86 149.00 -60.00  170
 16  \w    -70.00 -37.00   0.50    0.06    -- -105.86  61.00 120.00   66
 17  \w   -106.00 -37.00   0.50    0.06    -- -105.86 122.00 137.00  138
 18  \w   -169.00-143.00   0.50    0.06    -- -105.86 -61.00 -30.00   52
 19  \w   -129.00 -94.00   0.50    0.06    -- -105.86 -61.00 -30.00   70
 20  \w   -130.00-105.00   0.50    0.06    -- -105.86-122.00  56.00   50
 21  \w   -113.00 -62.00   0.50    0.05    --  -47.45-149.00-106.00  102
 22  \w   -110.00 -83.00   0.50    0.05    --  -47.45-125.00-180.00   54
 23  \w   -176.00-103.00   0.50    0.06    -- -105.86 -45.00 150.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0985928000
_diffrn_orient_matrix_UB_12      0.0134801000
_diffrn_orient_matrix_UB_13      0.0407322000
_diffrn_orient_matrix_UB_21      0.0124773000
_diffrn_orient_matrix_UB_22      -0.1139403000
_diffrn_orient_matrix_UB_23      -0.0117532000
_diffrn_orient_matrix_UB_31      0.0080045000
_diffrn_orient_matrix_UB_32      0.0111129000
_diffrn_orient_matrix_UB_33      -0.1701933000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.674
_diffrn_reflns_theta_min         2.860
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0395
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3337
_reflns_number_total             3697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py01088c1.cif
_cod_data_source_block           galukh336_corr
_cod_depositor_comments          'Adding full bibliography for 1564903.cif.'
_cod_database_code               1564903
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C23H15N3O3
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C7(H7), C4(H4), C14(H14), C26(H26), C5(H5), C17(H17),
 C25(H25), C23(H23), C22(H22), C16(H16)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              78931
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.744