The zwitterion (23'<i>E</i>)-(23<i>R</i>,25<i>S</i>)-23-[1-(oxidoiminio)ethyl]-5β-spirostan-3β-yl acetate
Hernández Linares, María-Guadalupe; Sandoval Ramírez, Jesús; Meza Reyes, Socorro; Montiel Smith, Sara; Bernès, Sylvain; Acta Crystallographica Section E 65 (2009) o2954–o2955; doi:10.1107/S1600536809044651

data_2223951
_publ_section_title
;The zwitterion
 (23'<i>E</i>)-(23<i>R</i>,25<i>S</i>)-23-[1-(oxidoiminio)ethyl]-5\b-spirostan-3\b-yl
 acetate
;
_journal_coeditor_code           NK2010
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2954
_journal_page_last               o2955
_journal_paper_doi               10.1107/S1600536809044651
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C31 H49 N O5'
_chemical_formula_moiety         'C31 H49 N O5'
_chemical_formula_sum            'C31 H49 N O5'
_chemical_formula_weight         515.71
_chemical_melting_point          516
_chemical_name_systematic
;
(23'<i>E</i>)-(23<i>R</i>,25<i>S</i>)-23-[1-(oxidoiminio)ethyl]-5\b-
spirostan-3\b-yl acetate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.385(2)
_cell_length_b                   11.5627(16)
_cell_length_c                   30.420(5)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      4.71
_cell_volume                     2949.3(9)
_computing_cell_refinement       'XSCANS (Siemens, 1994)'
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'XSCANS (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            4182
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.247
_refine_ls_extinction_coef       0.0095(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+1.0057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                2512
_reflns_number_total             2956
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nk2010.cif
_cod_data_source_block           I
_cod_original_cell_volume        2949.2(10)
_cod_database_code               2223951
_cod_database_fobs_code          2223951