Crystal structures of 2,3,8,9,14,15-hexamethyl-5,6,11,12,17,18-hexaazatrinaphthylene and 2,3,8,9,14,15-hexaphenyl-5,6,11,12,17,18-hexazatrinaphthylene dichloromethane disolvate
Fangmann, Pia; Schmidtmann, Marc; Beckhaus, Rüdiger; Acta Crystallographica Section E 74 (2018) 167–171; doi:10.1107/S2056989018000725

data_2242327
_publ_section_title
;
 Crystal structures of
 2,3,8,9,14,15-hexamethyl-5,6,11,12,17,18-hexaazatrinaphthylene and
 2,3,8,9,14,15-hexaphenyl-5,6,11,12,17,18-hexazatrinaphthylene
 dichloromethane disolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              167
_journal_page_last               171
_journal_paper_doi               10.1107/S2056989018000725
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C60 H36 N6, 2C H2 Cl2'
_chemical_formula_moiety         'C60 H36 N6, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H40 Cl4 N6'
_chemical_formula_weight         1010.80
_chemical_name_systematic
;
2,3,8,9,14,15-Hexaphenyl-5,6,11,12,17,18-hexazatrinaphthylene dichloromethane
disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                64.2659(13)
_cell_angle_beta                 78.2616(15)
_cell_angle_gamma                88.3530(17)
_cell_formula_units_Z            2
_cell_length_a                   9.2629(4)
_cell_length_b                   16.3829(6)
_cell_length_c                   18.4366(6)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.25
_cell_volume                     2461.97(16)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS-2013/1 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87137
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.383
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.839
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0500P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                11804
_reflns_number_total             14377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5431sup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        2461.98(16)
_cod_database_code               2242327
_cod_database_fobs_code          2242327
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.972
_shelx_hkl_checksum              59136
_shelx_res_checksum              59485