Accurate stereochemistry for two related 22,26-epiminocholestene derivatives
Vega-Baez, José Luis; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Montiel-Smith, Sara; Gómez-Calvario, Victor; Bernès, Sylvain; Acta Crystallographica Section C 64 (2008) o214–o216; doi:10.1107/S0108270108005763

data_2016544
_publ_section_title
;
 Accurate stereochemistry for two related 22,26-epiminocholestene
 derivatives
;
_journal_coeditor_code           GD3197
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o214
_journal_page_last               o216
_journal_paper_doi               10.1107/S0108270108005763
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C31 H47 N O4'
_chemical_formula_moiety         'C31 H47 N O4'
_chemical_formula_sum            'C31 H47 N O4'
_chemical_formula_weight         497.70
_chemical_melting_point          462
_chemical_name_common
;
3,16-diacetyl pseudosolasodine B
;
_chemical_name_systematic
;
(25R)-22,26-epiminocholesta-5,22(<i>N</i>)-diene-3\b,16\b-diyl diacetate
;
_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           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1137(16)
_cell_length_b                   11.6779(14)
_cell_length_c                   41.330(5)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      11.37
_cell_measurement_theta_min      4.75
_cell_volume                     2950.8(9)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL-Plus (Release 5.10; Sheldrick, 2008)'
_computing_publication_material
'SHELXTL-Plus (Release 5.10; Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXTL-Plus (Release 5.10; Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-Plus (Release 5.10; Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            3812
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.196
_refine_ls_extinction_coef       0.0077(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL-Plus
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     332
_refine_ls_number_reflns         3026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0744P)^2^+0.5847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                1931
_reflns_number_total             3026
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3197.cif
_cod_data_source_block           I
_cod_database_code               2016544
_cod_database_fobs_code          2016544