Poly(bridged bicycle)s synthesized via cyclopolymerization of cyclic diacrylates
Kohsaka, Yasuhiro; Yoshida, Taichi; Nishiie, Natsumi; Polymer Chemistry 16 (2025) 4009–4012; doi:10.1039/D5PY00631G

data_1575518
_publ_section_title
;
 Poly(bridged bicycle)s synthesized via cyclopolymerization of cyclic
 diacrylates
;
_journal_issue                   36
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4009
_journal_page_last               4012
_journal_paper_doi               10.1039/D5PY00631G
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C8 H10 O4'
_chemical_formula_sum            'C8 H8 O4'
_chemical_formula_weight         168.14
_chemical_properties_physical    Heat-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2ntfxv
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_audit_update_record
;
2025-06-25 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.622(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1668(5)
_cell_length_b                   6.0924(3)
_cell_length_c                   11.7374(6)
_cell_measurement_reflns_used    5202
_cell_measurement_temperature    97
_cell_measurement_theta_max      30.4040
_cell_measurement_theta_min      2.4740
_cell_volume                     798.21(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      97
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_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      9.00  57.00   0.50    7.48    --   20.00  54.00  90.00   96
  2  \w    -72.00 -47.00   0.50    7.48    --   20.00  54.00-150.00   50
  3  \w     -7.00  70.00   0.50    7.48    --   20.00  54.00-150.00  154
  4  \w    -74.00 110.00   0.50    7.48    --   20.00  54.00 -33.60  368
  5  \w    -74.00  42.00   0.50    7.48    --   20.00  54.00 -90.00  232
  6  \w     60.00 110.00   0.50    7.48    --   20.00  54.00 -90.00  100
  7  \w    -73.00 -11.00   0.50    7.48    --   20.00  54.00   0.00  124
  8  \w    -67.00 -35.00   0.50    7.48    --   20.00  54.00  90.00   64
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0421579000
_diffrn_orient_matrix_UB_12      -0.0803220000
_diffrn_orient_matrix_UB_13      0.0186187000
_diffrn_orient_matrix_UB_21      -0.0418052000
_diffrn_orient_matrix_UB_22      -0.0842378000
_diffrn_orient_matrix_UB_23      -0.0138173000
_diffrn_orient_matrix_UB_31      0.0224966000
_diffrn_orient_matrix_UB_32      -0.0059212000
_diffrn_orient_matrix_UB_33      -0.0558183000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5875
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         3.473
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (Rigaku Oxford Diffraction, 2023)
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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.913
_exptl_crystal_size_mid          0.665
_exptl_crystal_size_min          0.306
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0390P)^2^+0.3016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1366
_reflns_number_total             1454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00631g2.cif
_cod_data_source_block           20231211_auto
_cod_depositor_comments
'Adding full bibliography for 1575518--1575520.cif.'
_cod_database_code               1575518
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              30709
_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 1.697
_oxdiff_exptl_absorpt_empirical_full_min 0.650