Ethyl 12b-allyl-1-hydroxy-3,6,7,12b-tetrahydro-4<i>H</i>-1,3-dioxolo[4,5-<i>g</i>]pyrido[2,1-<i>a</i>]isoquinoline-2-carboxylate
Ya-Wen Wang; Yu Peng; Acta Crystallographica Section E 62 (2006) o3966–o3967; doi:10.1107/S1600536806031977

data_2210228
_publ_section_title
;Ethyl
 12b-allyl-1-hydroxy-3,6,7,12b-tetrahydro-4<i>H</i>-1,3-dioxolo[4,5-<i>g</i>]pyrido[2,1-<i>a</i>]isoquinoline-2-carboxylate
;
_journal_coeditor_code           FL2046
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3966
_journal_page_last               o3967
_journal_paper_doi               10.1107/S1600536806031977
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C20 H23 N O5'
_chemical_formula_moiety         'C20 H23 N O5'
_chemical_formula_sum            'C20 H23 N O5'
_chemical_formula_weight         357.39
_chemical_name_systematic
;Ethyl
 12b-allyl-1-hydroxy-3,6,7,12b-tetrahydro-4H-1,3-dioxolo[4,5-g]pyrido[2,1-
a]isoquinoline-2-carboxylate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.854(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5365(7)
_cell_length_b                   20.0523(18)
_cell_length_c                   10.6574(9)
_cell_measurement_reflns_used    1800
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.19
_cell_volume                     1797.4(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9495
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.402
_refine_ls_extinction_coef       0.0022(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   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0336P)^2^+2.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                1915
_reflns_number_total             3350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2046.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2210228
_cod_database_fobs_code          2210228