Ergotaminine
Merkel, Stefan; Köppen, Robert; Koch, Matthias; Emmerling, Franziska; Nehls, Irene; Acta Crystallographica Section E 68 (2012) o610–o611; doi:10.1107/S1600536812003674

data_2233776
_publ_section_title
;
 Ergotaminine
;
_journal_coeditor_code           DS2173
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o610
_journal_page_last               o611
_journal_paper_doi               10.1107/S1600536812003674
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C33 H35 N5 O5'
_chemical_formula_moiety         'C33 H35 N5 O5'
_chemical_formula_sum            'C33 H35 N5 O5'
_chemical_formula_weight         581.66
_chemical_name_common            Ergotaminine
_chemical_name_systematic
;
(6a<i>R</i>,9<i>S</i>)-<i>N</i>-[(2<i>R</i>,5<i>S</i>,10a<i>S</i>,
10b<i>S</i>)-5-Benzyl-10b-hydroxy-2-methyl-3,6-dioxooctahydro-8<i>H</i>-
oxazolo[3,2-<i>a</i>]pyrrolo[2,1-<i>c</i>]pyrazin-2-yl]-7-methyl-
4,6,6a,7,8,9-hexahydroindolo[4,3-<i>fg</i>]quinoline-9-carboxamide
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.059(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.974(3)
_cell_length_b                   9.662(2)
_cell_length_c                   14.450(4)
_cell_measurement_reflns_used    86
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      4
_cell_volume                     1479.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w/2\q
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20196
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.192
_refine_ls_abs_structure_details syn
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         2781
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                2240
_reflns_number_total             2781
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ds2173.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233776
_cod_database_fobs_code          2233776