(11<i>R</i>)-13-[2-(4-Hydroxyphenyl)ethylamino]-4,5-epoxy-11,13-dihydrocostunolide monohydrate
Nasim, Shama.; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 64 (2008) o644–; doi:10.1107/S1600536808003863

data_2217782
_publ_section_title
;(11<i>R</i>)-13-[2-(4-Hydroxyphenyl)ethylamino]-4,5-epoxy-11,13-dihydrocostunolide
 monohydrate
;
_journal_coeditor_code           HG2375
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o644
_journal_paper_doi               10.1107/S1600536808003863
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C23 H31 N O4, H2 O1'
_chemical_formula_moiety         'C23 H31 N O4, H2 O1'
_chemical_formula_sum            'C23 H33 N O5'
_chemical_formula_weight         403.50
_chemical_name_common
;
(11R)-13-[2-(4-Hydroxyphenyl)ethylamino]-4,5-epoxy-11,13-dihydrocostunolide
monohydrate
;
_chemical_name_systematic
;
12-{[2-(4-hydroxyphenyl)ethyl]aminomethyl}-4,8-dimethyl-
3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one monohydrate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.631(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8307(7)
_cell_length_b                   6.9478(5)
_cell_length_c                   14.4835(9)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      3.06
_cell_volume                     1086.32(12)
_computing_cell_refinement       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'APEX2 (Bruker--Nonius, 2004)'
_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 18
_diffrn_measured_fraction_theta_full .983
_diffrn_measured_fraction_theta_max .983
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'Bruker Helios multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13335
_diffrn_reflns_theta_full        68.05
_diffrn_reflns_theta_max         68.05
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in APEX2; Bruker--Nonius, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         .397
_refine_diff_density_min         -.205
_refine_ls_abs_structure_details 'Flack (1983), 1365 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                3420
_reflns_number_total             3532
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2375.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2217782
_cod_database_fobs_code          2217782