8,9-Dimethoxy-6-methyl-6,11,12,14-tetrahydro-6a<i>H</i>-1,3-dioxolo[4,5-<i>h</i>]isoquino[2,1-<i>b</i>]isoquinoline
Li, Wu; Yang, Lu; Zheng, Qi-Tai; Acta Crystallographica Section E 62 (2006) o3137–o3138; doi:10.1107/S1600536806024287

data_2210008
_publ_section_title
8,9-Dimethoxy-6-methyl-6,11,12,14-tetrahydro-6a<i>H</i>-1,3-dioxolo[4,5-<i>h</i>]isoquino[2,1-<i>b</i>]isoquinoline
_journal_coeditor_code           TK2055
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3137
_journal_page_last               o3138
_journal_paper_doi               10.1107/S1600536806024287
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C21 H23 N O4'
_chemical_formula_moiety         'C21 H23 N O4'
_chemical_formula_sum            'C21 H23 N O4'
_chemical_formula_weight         353.40
_chemical_name_common            cavidine
_chemical_name_systematic
;
8,9-Dimethoxy-6-methyl-6,11,12,14-tetrahydro-6aH-1,3-
dioxolo[4,5-h]isoquino[2,1-b]isoquinoline
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7400(10)
_cell_length_b                   8.2320(10)
_cell_length_c                   28.499(2)
_cell_measurement_reflns_used    9552
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.6
_cell_volume                     1815.8(3)
_computing_cell_refinement       'SCALE (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        SCALE
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLUTON (Spek, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'MAC DIP 2030K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            9552
_diffrn_reflns_theta_full        27.2
_diffrn_reflns_theta_max         27.2
_diffrn_reflns_theta_min         2.6
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.26
_refine_ls_extinction_coef       0.079(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.090
_refine_ls_R_factor_gt           0.070
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+1.0977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.163
_refine_ls_wR_factor_ref         0.177
_reflns_number_gt                1920
_reflns_number_total             2261
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2055.cif
_cod_data_source_block           I
_cod_database_code               2210008
_cod_database_fobs_code          2210008