2,9-Dichloro-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; Fejfarová, Karla; Dušek, Michal; Acta Crystallographica Section E 67 (2011) o2395–; doi:10.1107/S1600536811033721

data_2231446
_publ_section_title
;
 2,9-Dichloro-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           BX2366
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2395
_journal_paper_doi               10.1107/S1600536811033721
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H14 Cl2 N4'
_chemical_formula_moiety         'C16 H14 Cl2 N4'
_chemical_formula_sum            'C16 H14 Cl2 N4'
_chemical_formula_weight         333.2
_chemical_name_common
;
2,9-Dichloro-6<i>H</i>,13<i>H</i>-5:12,7:14-
dimethanodibenzo[<i>d</i>,<i>i</i>][1,3,6,8]tetraazecine
;
_chemical_name_systematic
;
4,13-dichloro-1,8,10,17-tetraazapentacyclo[8.8.1.1^8,17^.0^2,7^.0^11,16^]icosa-
2,4,6,11(16),12,14-hexaene
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8633(6)
_cell_length_b                   19.0429(14)
_cell_length_c                   7.6720(7)
_cell_measurement_reflns_used    3667
_cell_measurement_temperature    119.7
_cell_measurement_theta_max      66.75
_cell_measurement_theta_min      4.48
_cell_volume                     1441.00(19)
_computing_cell_refinement       'CrysalisPro (Agilent Technologies, 2010)'
_computing_data_collection
;
CrysAlisPro (Agilent Technologies, 2010)
;
_computing_data_reduction        'CrysalisPro (Agilent Technologies, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>,  2006)'
_computing_structure_refinement
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>,  2006)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Agilent Xcalibur diffractometer with an Atlas (Gemini ultra Cu) detector'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7379
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Agilent Technologies, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        66.83
_diffrn_reflns_theta_max         66.83
_diffrn_reflns_theta_min         6.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent Technologies, 2010);
analytical numeric absorption correction using a multifaceted crystal
 model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.5355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_details
;
(Flack, 1983), 569 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.33
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    37
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0035
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                1174
_reflns_number_total             1265
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bx2366.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               2231446
_cod_database_fobs_code          2231446