Parent and trisubstituted triazacoronenes: synthesis, crystal structure and physicochemical properties
Qitao Tan; Huanhuan Chen; Huaida Xia; Bingxin Liu; Bin Xu; Chem.Commun. 52 (2016) 537–; doi:

data_7118416
_publ_section_title
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 Parent and trisubstituted triazacoronenes: synthesis, crystal structure
 and physicochemical properties
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_journal_name_full               Chem.Commun.
_journal_page_first              537
_journal_volume                  52
_journal_year                    2016
_chemical_compound_source        No
_chemical_formula_moiety         C33H33N3
_chemical_formula_sum            'C33 H33 N3'
_chemical_formula_weight         471.62
_chemical_melting_point_gt       523
_chemical_name_common
2,6,10-tributylbenzo[lmn]phenanthridino[2,1,10,9-defgh][2,8]phenanthroline
_chemical_name_systematic        '2, 6,10-tributyl-1,5,9-triazacoronene'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
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2014-12-25 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
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_cell_angle_alpha                76.13(2)
_cell_angle_beta                 87.13(3)
_cell_angle_gamma                87.08(3)
_cell_formula_units_Z            2
_cell_length_a                   8.299(16)
_cell_length_b                   12.11(2)
_cell_length_c                   13.39(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1304(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6410
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9972
_exptl_absorpt_correction_T_min  0.9867
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'THF-CH3CN diffusion'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     842
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2619
_refine_ls_wR_factor_ref         0.3043
_reflns_number_gt                2560
_reflns_number_total             4478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc08853d2.cif
_cod_data_source_block           chh
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>523 K' was changed to
'523' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 4093 2015-10-18 17:28:56Z antanas 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118416