Between porphyrins and phthalocyanines: 10,20-diaryl-5,15-tetrabenzodiazaporphyrins
D. S. Andrianov; V. B. Rybakov; A. V. Cheprakov; Chem.Commun. 50 (2014) 7953–; doi:10.1039/C4CC02405B

data_7115299
_publ_section_title
;
 Between porphyrins and phthalocyanines:
 10,20-diaryl-5,15-tetrabenzodiazaporphyrins
;
_journal_name_full               Chem.Commun.
_journal_page_first              7953
_journal_paper_doi               10.1039/C4CC02405B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C62 H60 N6'
_chemical_formula_sum            'C62 H60 N6'
_chemical_formula_weight         889.16
_chemical_melting_point_gt       623
_chemical_melting_point_lt       625
_chemical_name_systematic
; 
 5,15-Diazatetrabenzo-10,20-bis(3,5-tert-butylphenyl)-porhyrin 
;
_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           SHELXL97
_cell_angle_alpha                84.777(12)
_cell_angle_beta                 83.980(13)
_cell_angle_gamma                72.609(12)
_cell_formula_units_Z            1
_cell_length_a                   9.1332(15)
_cell_length_b                   11.8576(18)
_cell_length_c                   13.566(2)
_cell_measurement_reflns_used    8367
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      70.10
_cell_measurement_theta_min      3.92
_cell_volume                     1391.5(4)
_computing_cell_refinement       '<i>X--AREA</i>  (STOE & CIE, 2012)'
_computing_data_collection       '<i>X--AREA</i>  (STOE & CIE, 2012)'
_computing_data_reduction        '<i>X--RED</i>   (STOE & CIE, 2012)'
_computing_molecular_graphics    '<i>Ortep--3</i> (Farrugia,   1997)'
_computing_publication_material  '<i>WinGX</i>    (Farrugia,   1999)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick,  2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick,  2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details      '3493 frames, detector distance = 60 mm'
_diffrn_measurement_device_type  'Stoe STADI VARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4785
_diffrn_reflns_theta_full        70.09
_diffrn_reflns_theta_max         70.09
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2901
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
 Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             474
_exptl_crystal_preparation       Et~2~O/CH~2~Cl~2~
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                2788
_reflns_number_total             4785
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02405b2.cif
_cod_data_source_block           andr4
_cod_database_code               7115299
_exptl_absorpt_factor_mur        0.024