Dimethyl 6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-2,8-diacetate
Faroughi, Masoud; Jensen, Paul; Try, Andrew C.; Acta Crystallographica Section E 64 (2008) o500–o500; doi:10.1107/S1600536808001918

data_2217550
_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-diacetate
;
_journal_coeditor_code           HK2419
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o500
_journal_page_last               o500
_journal_paper_doi               10.1107/S1600536808001918
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C21 H22 N2 O4'
_chemical_formula_moiety         'C21 H22 N2 O4'
_chemical_formula_sum            'C21 H22 N2 O4'
_chemical_formula_weight         366.41
_chemical_melting_point          395
_chemical_name_systematic
;
Dimethyl 5,6,11,12-tetrahydro-5,11-
methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-2,8-diacetate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.0800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5590(10)
_cell_length_b                   10.9570(10)
_cell_length_c                   28.976(3)
_cell_measurement_reflns_used    7374
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2673
_cell_measurement_theta_min      2.3439
_cell_volume                     3613.2(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
;
X-SEED (Barbour, 2001) and SHELXTL (Sheldrick, 2008)
;
_computing_publication_material  'modiCIFer (Guzei, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD 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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            35113
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.12
_diffrn_standards_number         148
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0601P)^2^+1.5095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                5732
_reflns_number_total             8689
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2419.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217550
_cod_database_fobs_code          2217550