Diethyl 2,6-diisopropyl-4,8-dioxoperhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
Li, Yi-Tao; Li, Juan; Acta Crystallographica Section E 62 (2006) o5144–o5145; doi:10.1107/S1600536806042644

data_2211211
_publ_section_title
;Diethyl
 2,6-diisopropyl-4,8-dioxoperhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
;
_journal_coeditor_code           SJ2144
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5144
_journal_page_last               o5145
_journal_paper_doi               10.1107/S1600536806042644
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C20 H32 N6 O6'
_chemical_formula_moiety         'C20 H32 N6 O6'
_chemical_formula_sum            'C20 H32 N6 O6'
_chemical_formula_weight         452.52
_chemical_name_systematic
;
Diethyl
2,6-diisopropyl-4,8-dioxoperhydro-2,3a,4a,6,7a,8a-
hexaazacyclopenta[def]fluorene-8b,8c-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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.621(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4577(15)
_cell_length_b                   9.2015(13)
_cell_length_c                   21.164(3)
_cell_measurement_reflns_used    4685
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.42
_cell_volume                     2216.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_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 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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10681
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+0.6272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1973
_reflns_number_gt                2920
_reflns_number_total             3883
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2144.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2211211
_cod_database_fobs_code          2211211