Dimethyl 6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-2,8-dicarboxylate
Faroughi, Masoud; Try, Andrew C.; Turner, Peter; Acta Crystallographica Section E 62 (2006) o3479–o3480; doi:10.1107/S1600536806028388

data_2209891
_publ_section_title
;Dimethyl
 6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-2,8-dicarboxylate
;
_journal_coeditor_code           HK2086
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3479
_journal_page_last               o3480
_journal_paper_doi               10.1107/S1600536806028388
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C19 H18 N2 O4'
_chemical_formula_moiety         'C19 H18 N2 O4'
_chemical_formula_sum            'C19 H18 N2 O4'
_chemical_formula_weight         338.35
_chemical_melting_point          503.18
_chemical_name_common
;
dimethyl ester Tr\"oger's base
;
_chemical_name_systematic
;
Dimethyl 6H,12H-5,11-methanodibenzo[b,f][1,5]diazocine-2,8-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.500(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.941(3)
_cell_length_b                   8.1336(19)
_cell_length_c                   15.260(4)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.47
_cell_volume                     1584.2(7)
_computing_cell_refinement       SAINT
_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) and
ORTEPII (Johnson, 1976)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker 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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15205
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.352
_exptl_crystal_size_min          0.269
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0368
_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^+0.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                3286
_reflns_number_total             3826
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2086.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2209891
_cod_database_fobs_code          2209891