5a-Hydroxy-9-methoxy-11-(3-methyl-2-butenyl)-12-(2-methyl-1-propenyl)-2,3,11,12-tetrahydro-1<i>H</i>,5<i>H</i>-pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-<i>b</i>]indole-5,6,14(5a<i>H</i>,14a<i>H</i>)-trione
Fa-Zuo Wang; Min Zhang; Wei Sun; Qian-Qun Gu; Wei-Ming Zhu; Acta Crystallographica Section E 63 (2007) o1859–o1860; doi:10.1107/S1600536807012056

data_2212790
_publ_section_title
5a-Hydroxy-9-methoxy-11-(3-methyl-2-butenyl)-12-(2-methyl-1-propenyl)-2,3,11,12-tetrahydro-1<i>H</i>,5<i>H</i>-pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-<i>b</i>]indole-5,6,14(5a<i>H</i>,14a<i>H</i>)-trione
_journal_coeditor_code           BT2286
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1859
_journal_page_last               o1860
_journal_paper_doi               10.1107/S1600536807012056
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C27 H31 N3 O5'
_chemical_formula_moiety         'C27 H31 N3 O5'
_chemical_formula_sum            'C27 H31 N3 O5'
_chemical_formula_weight         477.55
_chemical_name_common            '13-Oxofumitremorgin B'
_chemical_name_systematic
;
5a-Hydroxy-9-methoxy-11-(3-methyl-2-butenyl)-12-(2-methyl-1-propenyl)-
2,3,11,12-tetrahydro-1H,5H-
pyrrolo[1'',2'':4',5']pyrazino[1',2':1,6]pyrido[3,4-b]indole-
5,6,14(5aH,14aH)-trione
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.806(2)
_cell_length_b                   15.064(3)
_cell_length_c                   21.247(3)
_cell_measurement_reflns_used    3028
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.144
_cell_measurement_theta_min      2.346
_cell_volume                     2498.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'XP (Siemens, 1994) and CAMERON (Watkin <i>et al.</i>,  1993)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX 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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12939
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0523P)^2^+1.178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                1836
_reflns_number_total             2517
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2286.cif
_cod_data_source_block           I
_cod_database_code               2212790
_cod_database_fobs_code          2212790