(11b<i>R</i>,11c<i>S</i>)-<i>rel</i>-Diethyl 6-bromo-9-methoxy-4,11-dioxo-5,10-dihydro-1<i>H</i>,3<i>H</i>,4<i>H</i>,11<i>H</i>-2-oxa-3a,4a,10a,11a-tetraazabenz[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
Jing Li; Kunru Wang; Nengfang She; Acta Crystallographica Section E 63 (2007) o4579–o4579; doi:10.1107/S1600536807054670

data_2216475
_publ_section_title
;(11b<i>R</i>,11c<i>S</i>)-<i>rel</i>-Diethyl
 6-bromo-9-methoxy-4,11-dioxo-5,10-dihydro-1<i>H</i>,3<i>H</i>,4<i>H</i>,11<i>H</i>-2-oxa-3a,4a,10a,11a-tetraazabenz[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
;
_journal_coeditor_code           HB2614
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4579
_journal_page_last               o4579
_journal_paper_doi               10.1107/S1600536807054670
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H23 Br N4 O8'
_chemical_formula_moiety         'C21 H23 Br N4 O8'
_chemical_formula_sum            'C21 H23 Br N4 O8'
_chemical_formula_weight         539.34
_chemical_name_systematic
;
(11bR,11cS)-rel-Diethyl 6-bromo-9-methoxy-4,11-dioxo-5,10-dihydro-
1H,3H,4H,11H-2-Oxa-3a,4a,10a,11a-tetraazabenz[f]indeno[2,1,7-ija]azulene-
11b,11c-dicarboxylate
;
_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                 95.3870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2246(6)
_cell_length_b                   11.6031(8)
_cell_length_c                   21.4749(15)
_cell_measurement_reflns_used    2981
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      19.81
_cell_measurement_theta_min      2.33
_cell_volume                     2288.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18458
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4236
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0404P)^2^+3.1185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                2704
_reflns_number_total             4236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hb2614.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      'P 21/n'
_cod_database_code               2216475
_cod_database_fobs_code          2216475