<i>rel</i>-(11b<i>R</i>,11c<i>S</i>)-Diethyl 5,10-dihydro-7-nitro-4,11-dioxo-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
Qin, Shuqi; Yin, Guodong; Acta Crystallographica Section E 61 (2005) o3164–o3165; doi:10.1107/S1600536805027741

data_2206995
_publ_section_title
;<i>rel</i>-(11b<i>R</i>,11c<i>S</i>)-Diethyl
 5,10-dihydro-7-nitro-4,11-dioxo-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           JH6016
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3164
_journal_page_last               o3165
_journal_paper_doi               10.1107/S1600536805027741
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C20 H21 N5 O9'
_chemical_formula_moiety         'C20 H21 N5 O9'
_chemical_formula_sum            'C20 H21 N5 O9'
_chemical_formula_weight         475.42
_chemical_name_systematic
;
Diethyl
(11bR,11cS)-rel-5,10-dihydro-7-nitro-4,11-dioxo-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 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                 99.427(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0454(18)
_cell_length_b                   25.564(5)
_cell_length_c                   8.4997(15)
_cell_measurement_reflns_used    3635
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.20
_cell_volume                     2153.3(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_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 area-detector'
_diffrn_measurement_method       '\f and \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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11538
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0729P)^2^+1.0059P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1719
_reflns_number_gt                3284
_reflns_number_total             4225
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jh6016.cif
_cod_data_source_block           I
_cod_original_cell_volume        2153.2(7)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206995
_cod_database_fobs_code          2206995