Diethyl 2-<i>tert</i>-butyl-6,9-dibromo-4,11-dioxo-5,10-dihydro-<i>cis</i>-1<i>H</i>,3<i>H</i>,4<i>H</i>,11<i>H</i>-2-azo-3a,4a,10a,11a-tetraazabenz[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
Jing Qin; Hui-Zhen Guo; Li-Ping Cao; Acta Crystallographica Section E 64 (2008) o37–o38; doi:10.1107/S1600536807062472

data_2217136
_publ_section_title
;Diethyl
 2-<i>tert</i>-butyl-6,9-dibromo-4,11-dioxo-5,10-dihydro-<i>cis</i>-1<i>H</i>,3<i>H</i>,4<i>H</i>,11<i>H</i>-2-azo-3a,4a,10a,11a-tetraazabenz[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
;
_journal_coeditor_code           IS2227
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o37
_journal_page_last               o38
_journal_paper_doi               10.1107/S1600536807062472
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C24 H29 Br2 N5 O6'
_chemical_formula_moiety         'C24 H29 Br2 N5 O6'
_chemical_formula_sum            'C24 H29 Br2 N5 O6'
_chemical_formula_weight         643.34
_chemical_name_systematic
;
Diethyl 2-tert-butyl-6,9-dibromo-4,11-dioxo-5,10-dihydro-cis-1H,3H,4H,11H-
2-azo-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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.6920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4151(8)
_cell_length_b                   11.3801(8)
_cell_length_c                   23.1649(17)
_cell_measurement_reflns_used    2626
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.78
_cell_measurement_theta_min      2.18
_cell_volume                     2742.6(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18064
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4828
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                2185
_reflns_number_total             4828
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2227.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217136
_cod_database_fobs_code          2217136