Diethyl 6,13-dioxo-5,7,12,13b,13c,14-hexahydro-6<i>H</i>,13<i>H</i>-5a,6a,12a,13a-tetraazabenz[5,6]azuleno[2,1,8-<i>ija</i>]benz[<i>f</i>]azulene-13b,13c-dicarboxylate 1,2-dichloroethane solvate
Liu, Hong-Xia; Wang, Zhi-Guo; Acta Crystallographica Section E 65 (2009) o2746–o2747; doi:10.1107/S1600536809041373

data_2223753
_publ_section_title
;Diethyl
 6,13-dioxo-5,7,12,13b,13c,14-hexahydro-6<i>H</i>,13<i>H</i>-5a,6a,12a,13a-tetraazabenz[5,6]azuleno[2,1,8-<i>ija</i>]benz[<i>f</i>]azulene-13b,13c-dicarboxylate
 1,2-dichloroethane solvate
;
_journal_coeditor_code           GK2232
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2746
_journal_page_last               o2747
_journal_paper_doi               10.1107/S1600536809041373
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C26 H26 N4 O6, C2 H4 Cl2'
_chemical_formula_moiety         'C26 H26 N4 O6, C2 H4 Cl2'
_chemical_formula_sum            'C28 H30 Cl2 N4 O6'
_chemical_formula_weight         589.46
_chemical_name_systematic
;
Diethyl
6,13-dioxo-5,7,12,13b,13c,14-hexahydro-6<i>H</i>,13<i>H</i>-5a,6a,12a,13a-
tetraazabenz[5,6]azuleno[2,1,8-<i>ija</i>]benz[<i>f</i>]azulene-13b,13c-
dicarboxylate 1,2-dichloroethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.257(2)
_cell_angle_beta                 82.688(2)
_cell_angle_gamma                76.892(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9468(10)
_cell_length_b                   11.1544(13)
_cell_length_c                   15.6260(18)
_cell_measurement_reflns_used    5260
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.34
_cell_volume                     1418.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10171
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.641
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4947
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1032P)^2^+0.8923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                4056
_reflns_number_total             4947
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2232.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_cell_volume        1418.5(3)
_cod_database_code               2223753
_cod_database_fobs_code          2223753