<small>L</small>-Menthyl ester of highly estrogenic (–)-(<i>Z</i>)-bisdehydrodoisynolic acid 3-methyl ether
Robinson, Paul D.; Hou, Yuqing; Meyers, Cal Y.; Adler, Stuart; Banz, William J.; Winters, Todd A.; Acta Crystallographica Section C 55 (1999) IUC9900020–; doi:10.1107/S0108270199099540

data_2008416
_publ_section_title
;
 <small>L</small>-Menthyl ester of highly estrogenic
 (--)-(<i>Z</i>)-bisdehydrodoisynolic acid 3-methyl ether
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900020
_journal_paper_doi               10.1107/S0108270199099540
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C29 H40 O3'
_chemical_formula_weight         436.61
_chemical_name_systematic
;
L-menthyl (-)-3-methoxy-13-methyl-14-ethyl-11,12,13(S)14(R)-
tetrahydrophenanthrene 13-carboxylate
IUPAC: L-menthyl (-)-(1R,2S)-1-ethyl-7-methoxy-2-methyl-
1,2,3,4-tetrahydrophenanthrene-2-carboxylate
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9185(11)
_cell_length_b                   28.281(4)
_cell_length_c                   8.6380(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296
_cell_measurement_theta_max      9.9
_cell_measurement_theta_min      9.0
_cell_volume                     2667.3(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1996)
;
_computing_data_reduction
'TEXSAN PROCESS  (Molecular Structure Corporation, 1997)'
_computing_molecular_graphics    'TEXSAN ORTEP (Johnson, 1965)'
_computing_publication_material  'TEXSAN, SHELXL97 and PLATON (Spek, 1990)'
_computing_structure_refinement  'TEXSAN LS and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'TEXSAN SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       '\w scans (rate 4\% min^-1^ in \w)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3004
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.095
_refine_diff_density_min         -0.109
_refine_ls_abs_structure_details
;
ascertained from the known absolute configuration of
the L-menthyl moiety
;
_refine_ls_abs_structure_Flack   3(3)
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.186
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0412P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.121
_reflns_number_gt                1046
_reflns_number_total             3004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0088.cif
_cod_data_source_block           QB0088
_cod_database_code               2008416