Diethyl 2-<i>tert</i>-butyl-4,11-dioxo-2,3-dihydro-<i>cis</i>-1<i>H</i>,5<i>H</i>,10<i>H</i>-2,3a,4a,10a,11a-pentaazabenzo[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
Zhu, Yanping; Sun, Yichong; Qiu, Mingqiang; Acta Crystallographica Section E 66 (2010) o289–; doi:10.1107/S1600536810000097

data_2224927
_publ_section_title
;Diethyl
 2-<i>tert</i>-butyl-4,11-dioxo-2,3-dihydro-<i>cis</i>-1<i>H</i>,5<i>H</i>,10<i>H</i>-2,3a,4a,10a,11a-pentaazabenzo[<i>f</i>]indeno[2,1,7-<i>ija</i>]azulene-11b,11c-dicarboxylate
;
_journal_coeditor_code           CV2681
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o289
_journal_paper_doi               10.1107/S1600536810000097
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C24 H31 N5 O6'
_chemical_formula_moiety         'C24 H31 N5 O6'
_chemical_formula_sum            'C24 H31 N5 O6'
_chemical_formula_weight         485.54
_chemical_name_systematic
;
Diethyl 2-<i>tert</i>-butyl-4,11-dioxo-2,3-dihydro-<i>cis</i>-
1<i>H</i>,5<i>H</i>,10<i>H</i>-2,3a,4a,10a,11a-
pentaazabenzo[<i>f</i>]indeno[2,1,7<i>ija</i>]azulene-11b,11c-dicarboxylate
;
_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                100.493(2)
_cell_angle_beta                 105.438(2)
_cell_angle_gamma                102.445(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7133(14)
_cell_length_b                   11.1013(15)
_cell_length_c                   11.3352(15)
_cell_measurement_reflns_used    2728
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      2.33
_cell_volume                     1227.2(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART 4K CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4253
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1160P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                2734
_reflns_number_total             4253
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2681.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_database_code               2224927
_cod_database_fobs_code          2224927