2,9-Dimethyl-6<i>H</i>,13<i>H</i>-5:12,7:14-dimethanodibenzo[<i>d</i>,<i>i</i>][1,3,6,8]tetraazecine
Rivera, Augusto; Maldonado, Mauricio; Ríos-Motta, Jaime; González-Salas, Diego; Dacunha-Marinho, Bruno; Acta Crystallographica Section E 65 (2009) o2553–; doi:10.1107/S1600536809038380

data_2223367
_publ_section_title
2,9-Dimethyl-6<i>H</i>,13<i>H</i>-5:12,7:14-dimethanodibenzo[<i>d</i>,<i>i</i>][1,3,6,8]tetraazecine
_journal_coeditor_code           FB2167
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2553
_journal_paper_doi               10.1107/S1600536809038380
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C18 H20 N4'
_chemical_formula_moiety         'C18 H20 N4'
_chemical_formula_sum            'C18 H20 N4'
_chemical_formula_weight         292.38
_chemical_melting_point          465
_chemical_name_systematic
;
2,9-Dimethyl-6<i>H</i>,13<i>H</i>-5:12,7:14-
dimethanodibenzo[<i>d</i>,<i>i</i>][1,3,6,8]tetraazecine
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_type_scat_source           'International Tables Vol. IV Table 2.4.6B'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9777(3)
_cell_length_b                   18.8351(4)
_cell_length_c                   7.6963(2)
_cell_measurement_reflns_used    3533
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.97
_cell_volume                     1446.37(7)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10245
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     102
_refine_ls_number_reflns         807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0593P)^2^+0.5089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                737
_reflns_number_total             807
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fb2167.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               2223367
_cod_database_fobs_code          2223367