Ethyl 3-hydroxy-13-methyl-4'-phenyl-2'-(3,4,5-trimethoxyphenyl)-6,7,8,9,11,12,13,14,15,16-decahydrospiro[cyclopenta[<i>a</i>]phenanthrene-16,3'-pyrrolidine]-5'-carboxylate
Kamala, E. Theboral Sugi; Murugan, R.; Nirmala, S.; Sudha, L.; Narayanan, S. Sriman; Acta Crystallographica Section E 64 (2008) o2219–o2220; doi:10.1107/S1600536808034582

data_2219791
_publ_section_title
;Ethyl
 3-hydroxy-13-methyl-4'-phenyl-2'-(3,4,5-trimethoxyphenyl)-6,7,8,9,11,12,13,14,15,16-decahydrospiro[cyclopenta[<i>a</i>]phenanthrene-16,3'-pyrrolidine]-5'-carboxylate
;
_journal_coeditor_code           BT2805
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2219
_journal_page_last               o2220
_journal_paper_doi               10.1107/S1600536808034582
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C39 H45 N O7'
_chemical_formula_moiety         'C39 H45 N O7'
_chemical_formula_sum            'C39 H45 N O7'
_chemical_formula_weight         639.76
_chemical_name_common
;
Spiro[3-phenyl-5-(3,4,5-trimethoxyphenyl)-2-ethoxycarbonyl
pyrrolidine-4,31-estrone]
;
_chemical_name_systematic
;
Ethyl
3-hydroxy-13-methyl-4'-phenyl-2'-(3,4,5-trimethoxyphenyl)-
6,7,8,9,11,12,13,14,15,16-decahydrospiro[cyclopenta[a]phenanthrene-
16,3'-pyrrolidine]-5'-carboxylate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 91.1250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1776(6)
_cell_length_b                   10.3379(2)
_cell_length_c                   13.6631(3)
_cell_measurement_reflns_used    38566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      1.5
_cell_volume                     3696.81(14)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT and XPREP Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2003)'
_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  'Bruker KappaAPEXII'
_diffrn_measurement_method       '\w and \f'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38566
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.9769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.241
_refine_ls_extinction_coef       0.0112(9)
_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   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0466
_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^)+(0.082P)^2^+1.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                3186
_reflns_number_total             3462
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2805.cif
_cod_data_source_block           I
_cod_original_cell_volume        3696.82(14)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2219791
_cod_database_fobs_code          2219791