2,4,6,8-Tetrakis(4-chlorophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one <i>O</i>-benzyloxime acetone monosolvate
Park, Dong Ho; Ramkumar, V.; Parthiban, P.; Acta Crystallographica Section E 68 (2012) o1481–; doi:10.1107/S1600536812016509

data_2234616
_publ_section_title
;
 2,4,6,8-Tetrakis(4-chlorophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one
 <i>O</i>-benzyloxime acetone monosolvate
;
_journal_coeditor_code           HB6689
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1481
_journal_paper_doi               10.1107/S1600536812016509
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C38 H31 Cl4 N3 O, C3 H6 O'
_chemical_formula_moiety         'C38 H31 Cl4 N3 O, C3 H6 O'
_chemical_formula_sum            'C41 H37 Cl4 N3 O2'
_chemical_formula_weight         745.54
_chemical_name_systematic
;
2,4,6,8-Tetrakis(4-chlorophenyl)-3,7-diazabicyclo[3.3.1]nonan-9-one
<i>O</i>-benzyloxime acetone monosolvate
;
_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                 93.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9237(5)
_cell_length_b                   10.5064(3)
_cell_length_c                   24.6015(7)
_cell_measurement_reflns_used    6628
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.64
_cell_volume                     3851.7(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35931
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.9340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+3.3824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1880
_reflns_number_gt                4263
_reflns_number_total             7173
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6689.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234616
_cod_database_fobs_code          2234616