X-ray Structure Analysis of (dl)-DeN-Corynoline, Derived from Hexahydorobenzo[c]phenanthridine Type Alkaloid Corynoline
KAMIGAUCHI, Miyoko; IN, Yasuko; ISHIDA, Toshimasa; X-ray Structure Analysis Online 25 (2009) 27–; doi:10.2116/xraystruct.25.27

data_1551812
_publ_section_title
;
 X-ray Structure Analysis of (dl)-DeN-Corynoline, Derived from
 Hexahydorobenzo[c]phenanthridine Type Alkaloid Corynoline
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              27
_journal_paper_doi               10.2116/xraystruct.25.27
_journal_volume                  25
_journal_year                    2009
_chemical_formula_sum            'C20 H20 O5'
_chemical_formula_weight         340.36
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   13.435(3)
_cell_length_b                   23.358(3)
_cell_length_c                   10.139(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      10.3
_cell_volume                     3181.8(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2921
_diffrn_reflns_theta_full        67.58
_diffrn_reflns_theta_max         67.58
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.8504
_exptl_absorpt_correction_T_min  0.5539
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North, et al.,1968'
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00191(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0433P)^2^+3.4116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                2336
_reflns_number_total             2829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            25_27_1.cif
_cod_data_source_block           (dl)-deN-Corynoline
_cod_original_cell_volume        3181.8(14)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1551812