Diethyl 6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-1,7-dicarboxylate
Bhuiyan, M. Delower H.; Clegg, Jack K.; Try, Andrew C.; Acta Crystallographica Section E 65 (2009) o187–; doi:10.1107/S1600536808042967

data_2220669
_publ_section_title
;Diethyl
 6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-1,7-dicarboxylate
;
_journal_coeditor_code           ZL2169
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o187
_journal_paper_doi               10.1107/S1600536808042967
_journal_volume                  65
_journal_year                    2009
_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          441
_chemical_name_common
;
1,7-Diethyl ester Tr\"oger's base
;
_chemical_name_systematic
;
Diethyl
6<i>H</i>,12<i>H</i>-5,11-methanodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-
1,7-dicarboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.149(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.306(3)
_cell_length_b                   9.251(2)
_cell_length_c                   15.081(4)
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.73
_cell_volume                     1759.8(7)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT and XPREP (Siemens, 1995)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and WINGX-32 (Farrugia, 1999)'
_computing_publication_material  'enCIFer (Allen <i>et al.</i>,  2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0.33
_diffrn_standards_number         111
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.98000
_exptl_absorpt_correction_T_min  0.855822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0513P)^2^+1.1460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                1925
_reflns_number_total             2135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zl2169.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2220669
_cod_database_fobs_code          2220669