6-Phenyl-6,7-dihydrodibenzo[<i>c</i>,<i>f</i>][1,5]azabismocin-12(5<i>H</i>)-yl perchlorate
Zhang, Xiao-Wen; Fan, Ting; Acta Crystallographica Section E 67 (2011) m875–; doi:10.1107/S1600536811021039

data_2230915
_publ_section_title
;
 6-Phenyl-6,7-dihydrodibenzo[<i>c</i>,<i>f</i>][1,5]azabismocin-12(5<i>H</i>)-yl
 perchlorate
;
_journal_coeditor_code           XU5208
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m875
_journal_paper_doi               10.1107/S1600536811021039
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Bi (C20 H17 N) (Cl O4)]'
_chemical_formula_moiety         'C20 H17 Bi Cl N O4'
_chemical_formula_sum            'C20 H17 Bi Cl N O4'
_chemical_formula_weight         579.78
_chemical_name_systematic
;
6-Phenyl-6,7-dihydrodibenzo[<i>c</i>,<i>f</i>][1,5]azabismocin-12(5<i>H</i>)-yl
perchlorate
;
_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                 107.590(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0635(10)
_cell_length_b                   14.0755(12)
_cell_length_c                   11.5121(10)
_cell_measurement_reflns_used    2936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.7
_cell_volume                     1863.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1658
_diffrn_reflns_av_sigmaI/netI    0.1191
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9267
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    9.632
_exptl_absorpt_correction_T_max  0.145
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.203
_refine_diff_density_max         4.891
_refine_diff_density_min         -4.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0816P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                2585
_reflns_number_total             3279
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5208.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230915
_cod_database_fobs_code          2230915