3-Nitroso-2,4,6,8-tetraphenyl-3,7-diazabicyclo[3.3.1]nonan-9-one
Natarajan, Sampath; Mathews, Rita; Acta Crystallographica Section E 67 (2011) o1686–; doi:10.1107/S1600536811022203

data_2230760
_publ_section_title
;
 3-Nitroso-2,4,6,8-tetraphenyl-3,7-diazabicyclo[3.3.1]nonan-9-one
;
_journal_coeditor_code           JJ2089
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1686
_journal_paper_doi               10.1107/S1600536811022203
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C31 H27 N3 O2'
_chemical_formula_moiety         'C31 H27 N3 O2'
_chemical_formula_sum            'C31 H27 N3 O2'
_chemical_formula_weight         473.56
_chemical_name_systematic
;
3-Nitroso-2,4,6,8-tetraphenyl-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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.728(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.723(4)
_cell_length_b                   8.8319(17)
_cell_length_c                   15.806(3)
_cell_measurement_reflns_used    19483
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.25
_cell_volume                     2527.8(9)
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SMART (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19483
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.0811
_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^)+(0.0715P)^2^+0.6524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                3235
_reflns_number_total             5385
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2089.cif
_cod_data_source_block           I
_cod_original_cell_volume        2527.8(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230760
_cod_database_fobs_code          2230760