Diethyl 4,8-dioxo-2,6-di-<i>p</i>-chlorophenyl-1,3,5,7-tetrahydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
Yin, Guo-Dong; Zhou, Bao-Han; Wu, An-Xin; Acta Crystallographica Section E 61 (2005) o2787–o2788; doi:10.1107/S1600536805024116

data_2206819
_publ_section_title
;Diethyl
 4,8-dioxo-2,6-di-<i>p</i>-chlorophenyl-1,3,5,7-tetrahydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
;
_journal_coeditor_code           WW6416
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2787
_journal_page_last               o2788
_journal_paper_doi               10.1107/S1600536805024116
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C26 H26 Cl2 N6 O6'
_chemical_formula_moiety         'C26 H26 Cl2 N6 O6'
_chemical_formula_sum            'C26 H26 Cl2 N6 O6'
_chemical_formula_weight         589.43
_chemical_name_systematic
;
Diethyl 4,8-dioxo-2,6-di-p-chlorophenyl-1,3,5,7-tetrahydro-2,3a,4a,6,7a,8a-
hexaazacyclopenta[def]fluorene-8b,8c-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                103.836(17)
_cell_angle_beta                 103.21(2)
_cell_angle_gamma                105.087(19)
_cell_formula_units_Z            2
_cell_length_a                   8.300(2)
_cell_length_b                   12.698(3)
_cell_length_c                   14.428(4)
_cell_measurement_reflns_used    4340
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.26
_cell_volume                     1355.3(7)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9438
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.278
_refine_ls_extinction_coef       0.0066(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0603P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                3709
_reflns_number_total             4737
_reflns_threshold_expression     I>2\s
_cod_data_source_file            ww6416.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        1355.2(6)
_cod_database_code               2206819
_cod_database_fobs_code          2206819