13-(Imidazol-1-yl)-11,13-dihydromelampomagnolide B monohydrate
Janganati, Venumadhav; Penthala, Narsimha Reddy; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 69 (2013) o1734–o1735; doi:10.1107/S1600536813029188

data_2238922
_publ_section_title
;
 13-(Imidazol-1-yl)-11,13-dihydromelampomagnolide B monohydrate
;
_journal_coeditor_code           SJ5362
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1734
_journal_page_last               o1735
_journal_paper_doi               10.1107/S1600536813029188
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C18 H24 N2 O4, H2 O'
_chemical_formula_moiety         'C18 H24 N2 O4, H2 O'
_chemical_formula_sum            'C18 H26 N2 O5'
_chemical_formula_weight         350.41
_chemical_name_common
;
13-(Imidazol-1-yl)-11,13-dihydromelampomagnolide B monohydrate
;
_chemical_name_systematic
'(1a<i>R</i>,7a<i>S</i>,8<i>R</i>,10a<i>S</i>,10b<i>S</i>,<i>E</i>)-5-Hydroxymethyl-8-[(1<i>H</i>-imidazol-1-yl)methyl]-1a-methyl-2,3,6,7,7a,8,10a,10b-octahydrooxireno[2',3':9,10]cyclodeca[1,2-b]furan-9(1a<i>H</i>)-one monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.0150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8073(2)
_cell_length_b                   8.27840(10)
_cell_length_c                   10.7741(2)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.05
_cell_measurement_theta_min      4.12
_cell_volume                     871.39(3)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXL2013 (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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  0.0299
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10767
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.054
_diffrn_reflns_theta_min         4.526
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       tablet
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.150
_refine_ls_abs_structure_details
;
Flack parameter determined using 747 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_coef       0.0090(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2008a)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0332P)^2^+0.1700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                2425
_reflns_number_total             2437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5362.cif
_cod_data_source_block           I
_cod_database_code               2238922
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              59473
_shelx_hkl_file                  {b79648a5-fb07-468c-bce1-f40779c6fa22}
_shelx_res_checksum              51240
_shelxl_version_number           .2013