1-[(4-Chlorophenyl)(phenylimino)methyl]-7-methoxy-2-naphthol–1,4-diazabicyclo[2.2.2]octane (2/1)
Nagasawa, Atsushi; Mitsui, Ryosuke; Kato, Yuichi; Okamoto, Akiko; Yonezawa, Noriyuki; Acta Crystallographica Section E 66 (2010) o2498–; doi:10.1107/S1600536810034690

data_2227670
_publ_section_title
;
 1-[(4-Chlorophenyl)(phenylimino)methyl]-7-methoxy-2-naphthol--1,4-diazabicyclo[2.2.2]octane
 (2/1)
;
_journal_coeditor_code           IS2593
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2498
_journal_paper_doi               10.1107/S1600536810034690
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2(C24 H18 Cl N O2), C6 H12 N2'
_chemical_formula_moiety         '2(C24 H18 Cl N O2), C6 H12 N2'
_chemical_formula_sum            'C54 H48 Cl2 N4 O4'
_chemical_formula_weight         887.86
_chemical_melting_point_gt       445.6
_chemical_melting_point_lt       446.0
_chemical_name_systematic
;
1-[(4-Chlorophenyl)(phenylimino)methyl]-7-methoxy-2-naphthol--
1,4-diazabicyclo[2.2.2]octane (2/1)
;
_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                 114.6210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0027(5)
_cell_length_b                   9.92298(18)
_cell_length_c                   20.0052(4)
_cell_measurement_reflns_used    33487
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.6
_cell_volume                     4512.07(16)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0110
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39753
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.5481
_exptl_absorpt_correction_T_min  0.3809
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>NUMABS</i>; Higashi, 1999)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.317
_refine_ls_extinction_coef       0.00076(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0539P)^2^+2.6288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                3831
_reflns_number_total             4125
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is2593.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2227670
_cod_database_fobs_code          2227670