Photoinduced Isomerization of 23-Oxosapogenins: Conformational Analysis and Spectroscopic Characterization of 22-Isosapogenins
Izabella Jastrzębska; Marcin Górecki; Jadwiga Frelek; Rosa Santillan; Leszek Siergiejczyk; Jacek W. Morzycki; Journal of Organic Chemistry 77 (2012) 11257–11269; doi:10.1021/jo3022549

data_4027797
_publ_section_title
;
 Photoinduced Isomerization of 23-Oxosapogenins: Conformational Analysis
 and Spectroscopic Characterization of 22-Isosapogenins
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11257
_journal_page_last               11269
_journal_paper_doi               10.1021/jo3022549
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C29 H44 O5'
_chemical_formula_weight         472.64
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6580(3)
_cell_length_b                   7.3450(3)
_cell_length_c                   16.5860(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1298.40(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.858
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7390
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.081
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_F_000             516
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0695P)^2^+0.1974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                3456
_reflns_number_total             3741
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo3022549_si_002.cif
_cod_data_source_block           monoc
_cod_database_code               4027797