Unexpected Spiro-benzoquinolines in the Reaction of N-(Arylidene)naphthalen-2-amine, Arylaldehyde, and 1,3-Dimethylbarbituric Acid in Water
Wang, Xiang-Shan; Zhang, Mei-Mei; Jiang, Hong; Yao, Chang-Sheng; Tu, Shu-Jiang; Chemistry Letters 36 (2007) 450–; doi:10.1246/cl.2007.450

data_8000161
_publ_section_title
;
 Unexpected Spiro-benzoquinolines in the Reaction of
 N-(Arylidene)naphthalen-2-amine, Arylaldehyde, and 1,3-Dimethylbarbituric
 Acid in Water
;
_journal_issue                   3
_journal_name_full               'Chemistry Letters'
_journal_page_first              450
_journal_paper_doi               10.1246/cl.2007.450
_journal_volume                  36
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H25 N3 O3'
_chemical_formula_sum            'C30 H25 N3 O3'
_chemical_formula_weight         475.53
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8386(16)
_cell_length_b                   8.5314(8)
_cell_length_c                   17.3856(18)
_cell_measurement_reflns_used    8236
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.3
_cell_volume                     2349.2(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21771
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            light-Yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack(1983), 2047 Friedel pairs'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         2224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0465P)^2^+0.5281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                2152
_reflns_number_total             2224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-450sup1.cif
_cod_data_source_block           shelxl
_cod_database_code               8000161