1,2,3,5a,6,11,12,14a-Octahydro-9-methoxy-12-(2-methylprop-1-enyl)-5<i>H</i>,14<i>H</i>-pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-<i>b</i>]indole-5,14-dione
Wang, Feng-Wu; Jiao, Rui-Hua; Tan, Ren-Xiang; Zhu, Hai-Liang; Tiekink, Edward R. T.; Acta Crystallographica Section E 62 (2006) o1375–o1377; doi:10.1107/S1600536806007513

data_2208719
_publ_section_title
1,2,3,5a,6,11,12,14a-Octahydro-9-methoxy-12-(2-methylprop-1-enyl)-5<i>H</i>,14<i>H</i>-pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-<i>b</i>]indole-5,14-dione
_journal_coeditor_code           SJ2013
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1375
_journal_page_last               o1377
_journal_paper_doi               10.1107/S1600536806007513
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C22 H25 N3 O3'
_chemical_formula_moiety         'C22 H25 N3 O3'
_chemical_formula_sum            'C22 H25 N3 O3'
_chemical_formula_weight         379.45
_chemical_name_common            'fumitremorgine C'
_chemical_name_systematic
;
1,2,3,5a,6,11,12,14a-Octahydro-9-methoxy-12-(2-methylprop-1-enyl)-5H,14H-
pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-b]indole-5,14-dione
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_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                   8.7795(12)
_cell_length_b                   8.7795
_cell_length_c                   26.020(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.0
_cell_measurement_theta_min      10.0
_cell_volume                     2005.6(5)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens 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  0.071
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2264
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       0.0095(18)
_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   1.21
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.21
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.124
_refine_ls_wR_factor_ref         0.136
_reflns_number_gt                1408
_reflns_number_total             2004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2013.cif
_cod_data_source_block           I
_cod_database_code               2208719
_cod_database_fobs_code          2208719