2,8-Dichloro-6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine
Faroughi, Masoud; Try, Andrew C.; Turner, Peter; Acta Crystallographica Section E 63 (2007) o2695–o2695; doi:10.1107/S1600536807019496

data_2213410
_publ_section_title
2,8-Dichloro-6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine
_journal_coeditor_code           HK2235
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2695
_journal_page_last               o2695
_journal_paper_doi               10.1107/S1600536807019496
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C15 H12 Cl2 N2'
_chemical_formula_moiety         'C15 H12 Cl2 N2'
_chemical_formula_sum            'C15 H12 Cl2 N2'
_chemical_formula_weight         291.17
_chemical_melting_point          402.49
_chemical_name_common
;
2,8-dichloro Tr\"oger's base
;
_chemical_name_systematic
;
2,8-Dichloro-6<i>H</i>,12<i>H</i>-5,11-
methanodibenzo[<i>b</i>,<i>f</i>][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                83.059(5)
_cell_angle_beta                 77.303(4)
_cell_angle_gamma                80.297(5)
_cell_formula_units_Z            2
_cell_length_a                   6.3017(18)
_cell_length_b                   10.203(3)
_cell_length_c                   10.685(3)
_cell_measurement_reflns_used    868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.299
_cell_measurement_theta_min      2.699
_cell_volume                     658.1(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT and XPREP (Siemens, 1995)'
_computing_molecular_graphics
;
TEXSAN for Windows (Molecular Structure Corporation, 1998),
Xtal3.6 (Hall <i>et al.</i>,  1999),
ORTEPII  (Johnson, 1976) and WinGX (Farrugia, 1999)
;
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6481
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
[GAUSSIAN (Coppens <i>et al.</i>,  1965) and XPREP (Siemens,
1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.246
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0296
_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^)+(0.03P)^2^+0.3P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                2845
_reflns_number_total             3041
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2235.cif
_cod_data_source_block           I
_cod_database_code               2213410
_cod_database_fobs_code          2213410