Crystal structure of 13-(<i>E</i>)-(2-aminobenzylidene)parthenolide
Bommagani, Shobanbabu; Penthala, Narsihma R.; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 74 (2018) 1543–1546; doi:10.1107/S2056989018013622

data_2242671
_publ_section_title
;
 Crystal structure of 13-(<i>E</i>)-(2-aminobenzylidene)parthenolide
;
_journal_coeditor_code           SJ5564
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1543
_journal_page_last               1546
_journal_paper_doi               10.1107/S2056989018013622
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C21 H25 N O3'
_chemical_formula_moiety         'C21 H25 N O3'
_chemical_formula_sum            'C21 H25 N O3'
_chemical_formula_weight         339.42
_chemical_name_common
;
13-(<i>E</i>)-(2-Aminobenzylidene)parthenolide
;
_chemical_name_systematic
(1a<i>R</i>,4<i>E</i>,7a<i>S</i>,8<i>E</i>,10a<i>S</i>,10b<i>R</i>)-8-(2-Aminobenzylidene)-1a,5-dimethyl-2,3,6,7,7a,8,10a,10b-octahydrooxireno[2',3':9,10]cyclodeca[1,2-<i>b</i>]furan-9(1a<i>H</i>)-one
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.3850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6136(3)
_cell_length_b                   6.24030(10)
_cell_length_c                   12.6875(3)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.15
_cell_measurement_theta_min      3.93
_cell_volume                     890.67(3)
_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</i> in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)
;
_computing_structure_refinement
;
<i>SHELXL2013</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.997
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24004
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.147
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.139
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 811 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013), as calculated by PLATON (Spek,
2009).
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2592
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0449P)^2^+0.1894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                2559
_reflns_number_total             2592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5564sup1.cif
_cod_data_source_block           I
_cod_database_code               2242671
_cod_database_fobs_code          2242671
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           .2013