(11<i>R</i>)-13-Dimethylammonio-11,13-dihydro-4,5-epoxycostunolide semifumarate
Neelakantan, Sundar; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 65 (2009) o1569–; doi:10.1107/S1600536809021941

data_2222335
_publ_section_title
;
 (11<i>R</i>)-13-Dimethylammonio-11,13-dihydro-4,5-epoxycostunolide
 semifumarate
;
_journal_coeditor_code           HG2516
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1569
_journal_paper_doi               10.1107/S1600536809021941
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C17 H28 N O3 +, C4 H3 O4 -'
_chemical_formula_moiety         'C17 H28 N O3 +, C4 H3 O4 -'
_chemical_formula_sum            'C21 H31 N O7'
_chemical_formula_weight         409.47
_chemical_name_common
;(11<i>R</i>)-13-Dimethylammonio-11,13-dihydro-4,5-epoxycostunolide
 semifumarate
;
_chemical_name_systematic
;(11<i>R</i>)-13-Dimethylammonio-11,13-dihydro-4,5-epoxycostunolide
 semifumarate
;
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.31640(10)
_cell_length_b                   15.1650(2)
_cell_length_c                   22.0028(3)
_cell_measurement_reflns_used    5373
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.02
_cell_measurement_theta_min      3.54
_cell_volume                     2107.61(5)
_computing_cell_refinement       'SAINT (Bruker--Nonius, 2006)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2006)'
_computing_data_reduction        'SAINT (Bruker--Nonius, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELX97 (Sheldrick, 2008) and local procedures'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16991
_diffrn_reflns_theta_full        68.02
_diffrn_reflns_theta_max         68.02
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in APEX2; Bruker--Nonius, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.139
_refine_ls_abs_structure_details 'Flack (1983), 1525 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.00093(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0359P)^2^+0.3552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                3640
_reflns_number_total             3762
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2516.cif
_cod_data_source_block           I
_cod_database_code               2222335
_cod_database_fobs_code          2222335