Latency control of chemical reactions in polymerization of epoxy resins using a hydrogen bonding network
Haneda, Tsuyoshi; Matsuno, Shinya; Yamamoto, Hisanao; Ohtsu, Hiroyoshi; Kawano, Masaki; CrystEngComm 23 (2021) 7717–7719; doi:10.1039/D1CE01163D

data_7243839
_publ_section_title
;
 Latency control of chemical reactions in polymerization of epoxy resins
 using a hydrogen bonding network
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7717
_journal_page_last               7719
_journal_paper_doi               10.1039/D1CE01163D
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '2(C16 H36 P), C10 H4 O8'
_chemical_formula_sum            'C42 H76 O8 P2'
_chemical_formula_weight         770.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-28 deposited with the CCDC.	2021-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1921(7)
_cell_length_b                   20.0035(8)
_cell_length_c                   11.7616(4)
_cell_measurement_reflns_used    3634
_cell_measurement_temperature    223
_cell_measurement_theta_max      74.5440
_cell_measurement_theta_min      4.4230
_cell_volume                     4515.4(3)
_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_temperature      223
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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  67.00   0.50   11.00    --   47.00 -71.00 -37.00  184
  2  \w   -106.00 -29.00   0.50   38.00    -- -102.00  96.00-171.00  154
  3  \w    -93.00 -29.00   0.50   38.00    -- -102.00  71.00  93.00  128
  4  \w    -69.00 -29.00   0.50   38.00    -- -102.00  59.00 -43.00   80
  5  \w     40.00  91.00   0.50   38.00    --  104.75 -71.00 -37.00  102
  6  \w    -12.00  14.00   0.50   11.00    --  -47.00  19.00-120.00   52
  7  \w   -109.00 -81.00   0.50   11.00    --  -47.00-125.00 120.00   56
  8  \w      2.00  27.00   0.50   11.00    --  -47.00  19.00  90.00   50
  9  \w    -63.00 -37.00   0.50   38.00    -- -102.00  61.00  60.00   52
 10  \w     32.00  74.00   0.50   38.00    --  104.75 -61.00 -90.00   84
 11  \w     32.00  57.00   0.50   38.00    --  104.75 -61.00  30.00   50
 12  \w    113.00 165.00   0.50   38.00    --  104.75  45.00-120.00  104
 13  \w     32.00  63.00   0.50   38.00    --  104.75 -61.00 150.00   62
 14  \w     37.00  65.00   0.50   38.00    --  104.75 -61.00 120.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0564600000
_diffrn_orient_matrix_UB_12      0.0504090000
_diffrn_orient_matrix_UB_13      0.0362262000
_diffrn_orient_matrix_UB_21      -0.0297423000
_diffrn_orient_matrix_UB_22      -0.0515893000
_diffrn_orient_matrix_UB_23      0.0842296000
_diffrn_orient_matrix_UB_31      0.0487109000
_diffrn_orient_matrix_UB_32      0.0269201000
_diffrn_orient_matrix_UB_33      0.0935760000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9289
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.063
_diffrn_reflns_theta_min         4.421
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77903
_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    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0698P)^2^+2.1465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1668
_reflns_number_total             2301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01163d2.cif
_cod_data_source_block           han_pym-50
_cod_depositor_comments
'Adding full bibliography for 7243835--7243841.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               7243839
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H78 O8 P2'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All O(H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C2(H2A,H2B), C6(H6A,H6B), C3(H3A,H3B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              73096
_shelx_hkl_checksum              88708
_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 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.620