Diethyl 1,4-dioxo-6-(3-pyridyl)perhydro-2,3,4a,6,7a-pentaazacyclopenta[<i>cd</i>]indene-2a,7b-dicarboxylate 1,2-dichoroethane solvate
Li-ping Cao; Zhi-guo Wang; Yan Hu; Acta Crystallographica Section E 63 (2007) o4540–o4540; doi:10.1107/S1600536807054566

data_2216377
_publ_section_title
;Diethyl
 1,4-dioxo-6-(3-pyridyl)perhydro-2,3,4a,6,7a-pentaazacyclopenta[<i>cd</i>]indene-2a,7b-dicarboxylate
 1,2-dichoroethane solvate
;
_journal_coeditor_code           CV2321
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4540
_journal_page_last               o4540
_journal_paper_doi               10.1107/S1600536807054566
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C18 H22 N6 O6, C2 H4 Cl2'
_chemical_formula_moiety         'C18 H22 N6 O6, C2 H4 Cl2'
_chemical_formula_sum            'C20 H26 Cl2 N6 O6'
_chemical_formula_weight         517.37
_chemical_name_systematic
;
Diethyl
1,4-dioxo-6-(3-pyridyl)perhydro-2,3,4a,6,7a-pentaazacyclopenta[cd]indene-
2a,7b-dicarboxylate 1,2-dichoroethane solvate
;
_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                 114.6570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9023(9)
_cell_length_b                   16.4032(11)
_cell_length_c                   12.1719(8)
_cell_measurement_reflns_used    2658
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      21.10
_cell_measurement_theta_min      2.30
_cell_volume                     2341.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (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      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 4K CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13883
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.9375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1319P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2247
_reflns_number_gt                2684
_reflns_number_total             4114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2321.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2216377
_cod_database_fobs_code          2216377