13-(<i>N</i>,<i>N</i>-Dimethylamino)micheliolide 0.08-hydrate
Bommagani, Shobanbabu; Penthala, Narsimha Reddy; Janganati, Venumadhav; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 69 (2013) o1789–o1790; doi:10.1107/S1600536813030304

data_2238924
_publ_section_title
;
 13-(<i>N</i>,<i>N</i>-Dimethylamino)micheliolide 0.08-hydrate
;
_journal_coeditor_code           SJ5365
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1789
_journal_page_last               o1790
_journal_paper_doi               10.1107/S1600536813030304
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H27 N O3, 0.08H2 O'
_chemical_formula_moiety         'C17 H27 N O3, 0.08(H2 O)'
_chemical_formula_sum            'C17 H27.16 N O3.08'
_chemical_formula_weight         295.01
_chemical_name_common
;
13-(<i>N</i>,<i>N</i>-Dimethylamino)micheliolide 0.08-hydrate
;
_chemical_name_systematic
'(3<i>R</i>,3a<i>S</i>,9<i>R</i>,9a<i>S</i>,9b<i>S</i>)-3-[(Dimethylamino)methyl]-9-hydroxy-6,9-dimethyl-3,3a,4,5,7,8,9,9a-octahydroazuleno[4,5-<i>b</i>]furan-2(9b<i>H</i>)-one 0.08-hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1329(2)
_cell_length_b                   10.5227(2)
_cell_length_c                   16.7194(3)
_cell_measurement_reflns_used    9518
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      5.29
_cell_volume                     1606.78(5)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2006)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2006)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2006)'
_computing_molecular_graphics
'<i>XP in SHELXTL</i> (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  '<i>SHELXL2013</i> (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  '<i>SHELXL2013</i> (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20070
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.323
_diffrn_reflns_theta_min         5.291
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.127
_refine_ls_abs_structure_details
;
Flack parameter determined using 1227 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                2908
_reflns_number_total             2925
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5365.cif
_cod_data_source_block           I
_cod_database_code               2238924
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.925
_shelx_hkl_checksum              24808
_shelx_res_checksum              83266
_shelxl_version_number           .2013