Serendipitous isolation of a triazinone-based air stable organic radical: synthesis, crystal structure, and computation
Madhu, Vedichi; Kanakati, Arun Kumar; Das, Samar K.; New Journal of Chemistry 44 (2020) 10781–10785; doi:10.1039/D0NJ02028A

data_7059685
_publ_section_title
;
 Serendipitous isolation of a triazinone-based air stable organic radical:
 synthesis, crystal structure, and computation
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10781
_journal_page_last               10785
_journal_paper_doi               10.1039/D0NJ02028A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(F6 P), C23 H16 N7 O, 2(O)'
_chemical_formula_sum            'C23 H16 F12 N7 O3 P2'
_chemical_formula_weight         728.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc23w68h
_audit_creation_date             2020-05-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2020-05-26 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                87.328(8)
_cell_angle_beta                 89.110(7)
_cell_angle_gamma                79.874(8)
_cell_formula_units_Z            2
_cell_length_a                   8.633(4)
_cell_length_b                   12.422(6)
_cell_length_c                   13.653(6)
_cell_measurement_reflns_used    1817
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.27
_cell_volume                     1439.7(12)
_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      273.15
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.1208
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9540
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        22.497
_diffrn_reflns_theta_max         22.497
_diffrn_reflns_theta_min         2.833
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1198P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1817
_reflns_number_total             3377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02028a2.cif
_cod_data_source_block           compound1+
_cod_depositor_comments
;Adding full bibliography for 7059685--7059686.cif.

 Adding full bibliography for 7059685--7059686.cif.
;
_cod_original_cell_volume        1439.9(12)
_cod_database_code               7059685
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C16(H16), C8(H8), C10(H10), C3(H3), C17(H17), C15(H15),
 C4(H4), C14(H14), C1(H1), C20(H20), C23(H23), C2(H2), C21(H21), C22(H22)
;
_shelx_res_checksum              38425
_olex2_submission_special_instructions 'No special instructions were received'