2,8-Dimethyl-1,9-dinitro-6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine
Bhuiyan, M. Delower H.; Jensen, Paul; Try, Andrew C.; Acta Crystallographica Section E 63 (2007) o908–o909; doi:10.1107/S1600536807002991

data_2212223
_publ_section_title
2,8-Dimethyl-1,9-dinitro-6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine
_journal_coeditor_code           HG2169
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o908
_journal_page_last               o909
_journal_paper_doi               10.1107/S1600536807002991
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C17 H16 N4 O4'
_chemical_formula_moiety         'C17 H16 N4 O4'
_chemical_formula_sum            'C17 H16 N4 O4'
_chemical_formula_weight         340.34
_chemical_melting_point          .515E-305
_chemical_name_common
;
2,8-Dimethyl-1,9-dinitro Tr\"oger's base
;
_chemical_name_systematic
;
2,8-Dimethyl-1,9-dinitro-6H,12H-5,11-methanodibenzo[b,f][1,5]diazocine
;
_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
_cell_angle_alpha                92.944(3)
_cell_angle_beta                 92.930(3)
_cell_angle_gamma                115.649(2)
_cell_formula_units_Z            2
_cell_length_a                   7.526(2)
_cell_length_b                   8.057(2)
_cell_length_c                   13.932(3)
_cell_measurement_reflns_used    6244
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2260
_cell_measurement_theta_min      2.8140
_cell_volume                     758.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'ModiCIFer (Guzei, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART CCD-1000 area-detector'
_diffrn_measurement_method       \w
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10018
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0557P)^2^+0.236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                3150
_reflns_number_total             3584
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2169.cif
_cod_data_source_block           I
_cod_database_code               2212223
_cod_database_fobs_code          2212223