12-Methoxy-15-(1-pyrrolidino)podocarpa-8,11,13-triene-15-one
Butcher, Ray J.; Bakare, Oladapo; John, Nicole J.; Acta Crystallographica Section E 62 (2006) o945–o947; doi:10.1107/S1600536806001668

data_2208342
_publ_section_title
;
 12-Methoxy-15-(1-pyrrolidino)podocarpa-8,11,13-triene-15-one
;
_journal_coeditor_code           HG6293
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o945
_journal_page_last               o947
_journal_paper_doi               10.1107/S1600536806001668
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C22 H31 N O2'
_chemical_formula_moiety         'C22 H31 N O2'
_chemical_formula_sum            'C22 H31 N O2'
_chemical_formula_weight         341.48
_chemical_name_common
;
12-Methoxy-15-(4-pyrrolidin-1-yl)podocarpa-8,11,13-trien-15-one
;
_chemical_name_systematic
;
3-Methoxy-4b,8-dimethyl-8-(4-pyrrolidin-1-ylcarbonyl)-
4b,5,6,7,8,8a,9,10-octahydrophenanthrene
;
_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           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                   9.2758(18)
_cell_length_b                   14.886(3)
_cell_length_c                   13.785(3)
_cell_measurement_reflns_used    5585
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.59
_cell_volume                     1903.4(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14559
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                2279
_reflns_number_total             2585
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6293.cif
_cod_data_source_block           I
_cod_original_cell_volume        1903.5(7)
_cod_database_code               2208342
_cod_database_fobs_code          2208342