Crystal structure of limonoid TS3, isolated from <i>Trichilia rubescens</i>
Kenfack Tsobnang, Patrice; Tsamo Tontsa, Armelle; Mkounga, Pierre; Ephrem Nkengfack, Augustin; Tonlé Kenfack, Ignas; Acta Crystallographica Section E 74 (2018) 1083–1086; doi:10.1107/S2056989018009775

data_2243188
_publ_section_title
;
 Crystal structure of limonoid TS3, isolated from <i>Trichilia
 rubescens</i>
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1083
_journal_page_last               1086
_journal_paper_doi               10.1107/S2056989018009775
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C26 H28 O5, 0.5H2 O1'
_chemical_formula_moiety         'C26 H28 O5, 0.5(H2 O1)'
_chemical_formula_sum            'C26 H29 O5.5'
_chemical_formula_weight         429.49
_chemical_name_systematic
;(3a<i>S</i>,3b<i>S</i>,4a<i>S</i>,5a<i>S</i>,6<i>S</i>,7a<i>R</i>,8a<i>R</i>,8b<i>S</i>,11a<i>R</i>)-6-(Furan-3-yl)-3a,5a,8b,11a-tetramethyl-3a,4a,5,5a,6,7,7a,8b,11,11a-decahydrooxireno[2',3':4b,5]oxireno[2'',3'':2',3']cyclopenta[1',2':7,8]phenanthro[10,1-<i>bc</i>]furan-3(3a<i>H</i>)-one
hemihydrate
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4711(2)
_cell_length_b                   12.0986(2)
_cell_length_c                   13.7645(2)
_cell_measurement_reflns_used    30836
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.50
_cell_measurement_theta_min      3.55
_cell_volume                     2075.87(6)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015), publCIF (Westrip, 2010) and
enCIFer (Allen <i>et al.</i>,  2004)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture Photon'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33504
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.503
_diffrn_reflns_theta_min         3.546
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       needle
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.237
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3527 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
(SHELXL2018; Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8304
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0454P)^2^+0.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                8067
_reflns_number_total             8304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5448sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C26 H29 O5.50'
_cod_database_code               2243188
_cod_database_fobs_code          2243188
_shelx_hkl_checksum              24690
_shelx_res_checksum              92840