Crystal structure of (1S,3aR,3bR,10aR,10bR,12aR)-8-amino-3a,3b,6,6,10a-pentamethyl-1-((S)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)-2,3,3a,3b,4,5,5a,6,10,10a,10b,11,12,12a-tetradecahydro-1H-cyclopenta[7,8]phenanthro[2,3-d]thiazol-12-ol – a panaxadiol dervative, C31H50N2O2S
Wang, Jia-Zhen; Weng, Wei-Zhao; Ma, Ying; He, Xiu-Ting; Meng, Qing-Guo; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 397–400; doi:10.1515/ncrs-2018-0238

data_8105658
_publ_section_title
;
 Crystal structure of
 (1S,3aR,3bR,10aR,10bR,12aR)-8-amino-3a,3b,6,6,10a-pentamethyl-1-((S)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)-2,3,3a,3b,4,5,5a,6,10,10a,10b,11,12,12a-tetradecahydro-1H-cyclopenta[7,8]phenanthro[2,3-d]thiazol-12-ol
 -- a panaxadiol dervative, C31H50N2O2S
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              397
_journal_page_last               400
_journal_paper_doi               10.1515/ncrs-2018-0238
_journal_volume                  234
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H50 N2 O2 S'
_chemical_formula_sum            'C31 H50 N2 O2 S'
_chemical_formula_weight         514.79
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9922(9)
_cell_length_b                   16.7099(8)
_cell_length_c                   29.1262(16)
_cell_measurement_reflns_used    1727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.1990
_cell_measurement_theta_min      3.0390
_cell_volume                     5836.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS97 (Sheldrick,1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART,CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13666
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        66.044
_diffrn_reflns_theta_max         66.044
_diffrn_reflns_theta_min         3.049
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7150
_exptl_absorpt_correction_T_min  0.6330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1015 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.00061(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         9090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0196P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.608
_reflns_Friedel_fraction_full    0.756
_reflns_Friedel_fraction_max     0.756
_reflns_number_gt                4692
_reflns_number_total             9090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0238_suppl.cif
_cod_data_source_block           shelxl
_cod_database_code               8105658
_shelx_estimated_absorpt_t_min   0.633
_shelx_estimated_absorpt_t_max   0.715
_shelx_hkl_checksum              20821