The product of a regiospecific and stereoselective ene-reaction of a polycyclic terpenoid system
Abad, Antonio; Agulló, Consuelo; Cuñat, Ana C.; Navarro, Ismael; Ramírez de Arellano, Carmen; Acta Crystallographica Section E 57 (2001) o553–o554; doi:10.1107/S1600536801008510

data_2200327
_publ_section_title
;
 The product of a regiospecific and stereoselective ene-reaction of a
 polycyclic terpenoid system
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o553
_journal_page_last               o554
_journal_paper_doi               10.1107/S1600536801008510
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C25 H32 O7'
_chemical_formula_sum            'C25 H32 O7'
_chemical_formula_weight         444.51
_chemical_melting_point          430
_chemical_name_systematic
;
 dimethyl(Z)-[(8aS,2R, 4aR, 4bR)-8a-methoxycarbonyl-1,4a,7-
-trimethyl-8-oxo-2,3,4,4a,4b,5,8,8a,9,10-decahydro-
-phenanthren-2-yl]-2-butenedioate
;
_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'
_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                   11.810(2)
_cell_length_b                   13.985(3)
_cell_length_c                   14.434(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     2384.0(8)
_computing_cell_refinement       CAD4/PC
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1996)'
_computing_data_reduction        'MolEN (Fair, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  Nonius-CAD4
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0298
_diffrn_reflns_av_sigmaI/netI    .0472
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6144
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          .64
_exptl_crystal_size_mid          .62
_exptl_crystal_size_min          .44
_refine_diff_density_max         .149
_refine_diff_density_min         -.137
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   .5(16)
_refine_ls_extinction_coef       .0069(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          .0778
_refine_ls_R_factor_gt           .0491
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1230
_reflns_number_gt                3049
_reflns_number_total             4163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6041.cif
_cod_data_source_block           I
_cod_database_code               2200327
_cod_database_fobs_code          2200327