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_7059686
_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         'F6 P, C23 H16 N7 O'
_chemical_formula_sum            'C23 H16 F6 N7 O P'
_chemical_formula_weight         551.40
_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
_audit_block_doi                 10.5517/ccdc.csd.cc23w6bk
_audit_creation_date             2020-05-18
_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                90
_cell_angle_beta                 87.874(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.036(2)
_cell_length_b                   19.412(9)
_cell_length_c                   23.741(10)
_cell_measurement_reflns_used    1711
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      2.27
_cell_measurement_theta_min      27.94
_cell_volume                     2319.3(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.1288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.355
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0697P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2007
_reflns_number_total             4044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02028a2.cif
_cod_data_source_block           compound12+
_cod_depositor_comments
;Adding full bibliography for 7059685--7059686.cif.

 Adding full bibliography for 7059685--7059686.cif.
;
_cod_original_cell_volume        2319.2(18)
_cod_database_code               7059686
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C6(H6), C4(H4), C16(H16), C11(H11), C14(H14), C15(H15),
 C22(H22), C18(H18), C20(H20), C12(H12), C13(H13), C21(H21), C10(H10), C23(H23)
;
_shelx_res_checksum              17800
_olex2_submission_special_instructions 'No special instructions were received'