Toward an Air-Stable Triradical with Strong Spin Coupling: Synthesis of Substituted Truxene-5,10,15-triyl.
Yang, Xiao; Zhang, Di; Liao, Yinhui; Zhao, Dahui; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03077

data_4038265
_publ_section_title
;
 Toward an Air-Stable Triradical with Strong Spin Coupling: Synthesis of
 Substituted Truxene-5,10,15-triyl.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03077
_journal_year                    2020
_chemical_formula_moiety         'C52 H35 Cl9 O3'
_chemical_formula_sum            'C52 H35 Cl9 O3'
_chemical_formula_weight         1026.85
_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_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 111.906(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.913(4)
_cell_length_b                   15.005(3)
_cell_length_c                   20.527(5)
_cell_measurement_reflns_used    13205
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.4852
_cell_measurement_theta_min      1.3571
_cell_volume                     4547.4(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35686
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         1.728
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+9.5026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8928
_reflns_number_total             10393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03077_si_002.cif
_cod_data_source_block           mx6700
_cod_original_cell_volume        4547.5(18)
_cod_database_code               4038265
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.857
_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
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C21(H21), C23(H23), C26(H26), C27(H27),
 C28(H28), C29(H29), C35(H35), C37(H37), C41(H41), C42(H42), C43(H43), C44(H44),
  C49(H49), C51(H51)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C32(H32A,H32B,
 H32C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              15888
_shelx_hkl_checksum              51922
_olex2_submission_special_instructions 'No special instructions were received'