(2<i>S</i>,3<i>S</i>)-2-Azaniumyl-4-[(1<i>S</i>,4a<i>S</i>,4b<i>S</i>,6<i>S</i>,7<i>S</i>,8a<i>S</i>,10a<i>S</i>)-6,7-dihydroxy-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydrophenanthren-1-yl]-3-methoxybutanoate–methanol–water (1/1/1)
Eitel, Michael; Schollmeyer, Dieter; Gross, Harald; Koch, Pierre; IUCrData 3 (2018) x181194–; doi:10.1107/S241431461801194X

data_1549869
_publ_section_title
;
 (2<i>S</i>,3<i>S</i>)-2-Azaniumyl-4-[(1<i>S</i>,4a<i>S</i>,4b<i>S</i>,6<i>S</i>,7<i>S</i>,8a<i>S</i>,10a<i>S</i>)-6,7-dihydroxy-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydrophenanthren-1-yl]-3-methoxybutanoate--methanol--water
 (1/1/1)
;
_journal_coeditor_code           HB4254
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x181194
_journal_paper_doi               10.1107/S241431461801194X
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          'C24 H41 N O5, C H4 O, H2 O'
_chemical_formula_moiety         'C24 H41 N O5, C H4 O, H2 O'
_chemical_formula_sum            'C25 H47 N O7'
_chemical_formula_weight         473.63
_chemical_name_systematic
'(2<i>S</i>,3<i>S</i>)-2-Azaniumyl-4-[(1<i>S</i>,4a<i>S</i>,4b<i>S</i>,6<i>S</i>,7<i>S</i>,8a<i>S</i>,10a<i>S</i>)-6,7-dihydroxy-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydrophenanthren-1-yl]-3-methoxybutanoate--methanol--water (1/1/1)'
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9093(2)
_cell_length_b                   13.3712(4)
_cell_length_c                   25.3669(7)
_cell_measurement_reflns_used    15328
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      1.72
_cell_volume                     2682.72(13)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2011)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17021
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         1.722
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       coloumn
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.185
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1941 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.6(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+1.5011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                5482
_reflns_number_total             6656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4254sup1.cif
_cod_data_source_block           I
_cod_database_code               1549869
_cod_database_fobs_code          1549869
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              958
_shelx_res_checksum              84030