Diethyl 2,6-bis(4-ethynylphenyl)-4,8-dioxoperhydro-2,3a,4a,6,7a,8a-hexaaza-cyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
Hu, Sheng-Li; Wang, Shuai; Cao, Liping; Acta Crystallographica Section E 63 (2007) o4542–o4542; doi:10.1107/S160053680705458X

data_2216620
_publ_section_title
;Diethyl
 2,6-bis(4-ethynylphenyl)-4,8-dioxoperhydro-2,3a,4a,6,7a,8a-hexaaza-cyclopenta[<i>def</i>]fluorene-8b,8c-dicarboxylate
;
_journal_coeditor_code           LH2535
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4542
_journal_page_last               o4542
_journal_paper_doi               10.1107/S160053680705458X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C30 H28 N6 O6'
_chemical_formula_moiety         'C30 H28 N6 O6'
_chemical_formula_sum            'C30 H28 N6 O6'
_chemical_formula_weight         568.58
_chemical_name_systematic
;
Diethyl 2,6-bis(4-ethynylphenyl)-4,8-dioxoperhydro-
2,3a,4a,6,7a,8a-hexaaza-cyclopenta[def]fluorene-8b,8c-dicarboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.5230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0226(10)
_cell_length_b                   14.0617(9)
_cell_length_c                   13.7870(9)
_cell_measurement_reflns_used    3199
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.74
_cell_measurement_theta_min      2.18
_cell_volume                     2803.1(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12898
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                1952
_reflns_number_total             3057
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2535.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_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2216620
_cod_database_fobs_code          2216620