2,4,6,8-Tetrakis(4-bromophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one
Loh, Wan-Sin; Fun, Hoong-Kun; Sarveswari, S.; Vijayakumar, V.; Reddy, B. Palakshi; Acta Crystallographica Section E 66 (2010) o265–o266; doi:10.1107/S1600536809055226

data_2224891
_publ_section_title
;
 2,4,6,8-Tetrakis(4-bromophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one
;
_journal_coeditor_code           CI2986
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o265
_journal_page_last               o266
_journal_paper_doi               10.1107/S1600536809055226
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C31 H24 Br4 N2 O'
_chemical_formula_moiety         'C31 H24 Br4 N2 O'
_chemical_formula_sum            'C31 H24 Br4 N2 O'
_chemical_formula_weight         760.16
_chemical_name_systematic
;
2,4,6,8-Tetrakis(4-bromophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one
;
_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                 101.067(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7409(5)
_cell_length_b                   27.7762(10)
_cell_length_c                   7.1538(2)
_cell_measurement_reflns_used    8924
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.61
_cell_volume                     2874.62(16)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector diffractometer
;
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37831
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.628
_exptl_absorpt_correction_T_max  0.6141
_exptl_absorpt_correction_T_min  0.0818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.794
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       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^)+(0.0556P)^2^+2.5808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1410
_reflns_number_gt                4019
_reflns_number_total             8336
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2986.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               2224891
_cod_database_fobs_code          2224891