(<i>E</i>)-17β,19-Epoxymethano-17,23,24-tridemethyl-4-nor-5β,18α-olean-3-one oxime
Froelich, Anna; Kazakova, Oxana B.; Tolstikov, Genrikh; Gzella, Andrzej K.; Acta Crystallographica Section E 65 (2009) o1262–; doi:10.1107/S1600536809016675

data_2221998
_publ_section_title
;(<i>E</i>)-17\b,19-Epoxymethano-17,23,24-tridemethyl-4-nor-5\b,18\a-olean-3-one
 oxime
;
_journal_coeditor_code           FB2138
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1262
_journal_paper_doi               10.1107/S1600536809016675
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C27 H43 N O2'
_chemical_formula_moiety         'C27 H43 N O2'
_chemical_formula_sum            'C27 H43 N O2'
_chemical_formula_weight         413.62
_chemical_melting_point_gt       468
_chemical_melting_point_lt       470
_chemical_name_common
;
(<i>E</i>)-17\b,19-Epoxymethano-17,23,24-tridemethyl-4-nor-5\b,18\a-olean-
3-one oxime
;
_chemical_name_systematic
;(3<i>E</i>,3a<i>S</i>,5a<i>R</i>,5b<i>R</i>,7a<i>R</i>,11<i>R</i>,11a<i>R</i>,
11b<i>R</i>,13a<i>R</i>,13b<i>R</i>)-5a,5b,10,10,13b-
pentamethylicosahydro-1<i>H</i>-11,7a-
(epoxymethano)cyclopenta[<i>a</i>]chrysen-3-one
 oxime
;
_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   difmap
_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            4
_cell_length_a                   12.5887(16)
_cell_length_b                   13.2550(11)
_cell_length_c                   14.5355(12)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      14.5
_cell_volume                     2425.4(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)'
_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 diffractometer'
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4994
_diffrn_reflns_theta_full        70.14
_diffrn_reflns_theta_max         70.14
_diffrn_reflns_theta_min         4.51
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.120
_refine_diff_density_min         -0.116
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    163
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0523P)^2^+0.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                2240
_reflns_number_total             2610
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            fb2138.cif
_cod_data_source_block           I
_cod_database_code               2221998
_cod_database_fobs_code          2221998