Synthesis, Characterization, and Cure Chemistry of High Performance Phosphate Cyanate Ester Resins
Harvey, Benjamin Grant; Chafin, Andrew; Garrison, Michael; Cambrea, Lee; Groshens, Thomas J.; RSC Adv.  (2015) –; doi:10.1039/C5RA16197E

data_7221890
_publ_section_title
;
 Synthesis, Characterization, and Cure Chemistry of High Performance
 Phosphate Cyanate Ester Resins
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA16197E
_journal_year                    2015
_chemical_formula_moiety         'C21 H12 N3 O7 P'
_chemical_formula_sum            'C21 H12 N3 O7 P'
_chemical_formula_weight         449.31
_chemical_name_common            PhosCy3
_chemical_name_systematic        'tris(4-cyanatophenyl) phosphate '
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   difmap
_audit_update_record
;
2015-06-11 deposited with the CCDC.
2015-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.5995(9)
_cell_length_b                   12.5995(9)
_cell_length_c                   7.5587(5)
_cell_measurement_reflns_used    6378
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      27.1518
_cell_measurement_theta_min      2.6947
_cell_volume                     1039.16(13)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       'profile data from omega scans'
_diffrn_radiation_type           'Mo k\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12418
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.108
_refine_ls_abs_structure_details
;
Flack x determined using 662 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1431
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0236P)^2^+0.2150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                1378
_reflns_number_total             1431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra16197e2.cif
_cod_data_source_block           I
_cod_original_cell_volume        1039.16(16)
_cod_database_code               7221890
_shelx_res_checksum              80085