3-Cyano-11-oxo-3,4-seco-12a-aza-<i>C</i>-homoolean-4(23)-en-28-oic acid methyl ester
Froelich, A.; Bednarczyk-Cwynar, B.; Gzella, A. K.; Acta Crystallographica Section E 68 (2012) o532–; doi:10.1107/S1600536812002863

data_2233439
_publ_section_title
;
 3-Cyano-11-oxo-3,4-seco-12a-aza-<i>C</i>-homoolean-4(23)-en-28-oic acid
 methyl ester
;
_journal_coeditor_code           FJ2500
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o532
_journal_paper_doi               10.1107/S1600536812002863
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C31 H48 N2 O3'
_chemical_formula_moiety         'C31 H48 N2 O3'
_chemical_formula_sum            'C31 H48 N2 O3'
_chemical_formula_weight         496.71
_chemical_melting_point_gt       532
_chemical_melting_point_lt       535
_chemical_name_systematic
;
3-Cyano-11-oxo-3,4-seco-12a-aza-<i>C</i>-homoolean-4(23)-en-28-oic acid
methyl ester
;
_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                 91.607(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8549(10)
_cell_length_b                   11.711(2)
_cell_length_c                   17.356(3)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      15.48
_cell_volume                     1392.8(4)
_computing_cell_refinement       'KM-4 Software (Kuma Diffraction, 1996)'
_computing_data_collection
;
KM-4 Software (Kuma Diffraction, 1996)
;
_computing_data_reduction        'KM-4 Software (Kuma Diffraction, 1996)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
WinGX (Farrugia, 1999), PLATON (Spek, 2009) and enCIFer (Allen
<i>et al.</i>,
2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kuma Diffraction KM-4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5219
_diffrn_reflns_theta_full        70.18
_diffrn_reflns_theta_max         70.18
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.184
_refine_ls_abs_structure_details 'Flack (1983), 2248 Friedel pairs'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0184(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0684P)^2^+0.1756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                4815
_reflns_number_total             5045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2500.cif
_cod_data_source_block           I
_cod_original_cell_volume        1392.7(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233439
_cod_database_fobs_code          2233439