#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003302.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003302 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 721 _journal_page_last 723 _publ_section_title ; 3'-Methoxy-spiro[bicyclo[3.1.0]hexane-6,16'-estra-1',3',5'(10')-trien]-17'-one ; _chemical_formula_moiety 'C24 H30 O2' _chemical_formula_sum 'C24 H30 O2' _chemical_formula_structural 'C24 H30 O2' _chemical_formula_weight 350.50 _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 6.6532(6) _cell_length_b 7.1539(4) _cell_length_c 20.3786(13) _cell_angle_alpha 90 _cell_angle_beta 93.473(7) _cell_angle_gamma 90 _cell_volume 968.17(12) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.202 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.47 _cell_measurement_theta_max 21.20 _exptl_absorpt_coefficient_mu 0.54 _cell_measurement_temperature 293(2) _exptl_crystal_description 'plate-like' _exptl_crystal_size_max 1.25 _exptl_crystal_size_mid 0.85 _exptl_crystal_size_min 0.05 _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Enraf Nonius CAD-4F' _diffrn_measurement_method 'profile data from \q/2\q scans' _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.973 _diffrn_reflns_number 4773 _reflns_number_total 2160 _reflns_number_observed 2128 _reflns_observed_criterion '>2.5sigma(I)' _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 74.99 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.030 _refine_ls_wR_factor_obs 0.034 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 0.18 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 2128 _refine_ls_number_parameters 326 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme ; Calculated weights (McCandlish, Stout & Andrews,1975) with p = 0.02 ; _refine_ls_shift/esd_max 0.02 _refine_diff_density_max 0.16 _refine_diff_density_min -0.11 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source O ;International Tables (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H ;International Tables (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; C ;International Tables (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _refine_ls_abs_structure_details ; The absolute structure was selected to comply with the known chirality ; _refine_ls_abs_structure_Flack ? ##; PLATON93 (Spek, 1990). User interface software: S (Spek, 1994) ##; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O3 1 1.3279(2) 0.38260 0.03044(6) 0.0542(4) O17 1 0.0740(2) 0.0902(3) 0.32949(8) 0.0659(5) C1 1 0.8731(3) 0.1739(4) 0.09316(9) 0.0531(6) C2 1 1.0412(3) 0.1914(4) 0.05617(8) 0.0540(6) C3 1 1.1596(3) 0.3482(3) 0.06438(7) 0.0435(5) C4 1 1.1116(3) 0.4835(3) 0.10969(8) 0.0428(4) C5 1 0.9438(3) 0.4651(3) 0.14706(7) 0.0391(4) C6 1 0.9069(3) 0.6141(3) 0.19784(9) 0.0477(5) C7 1 0.6986(3) 0.6023(3) 0.22493(9) 0.0453(5) C8 1 0.6452(2) 0.4002(3) 0.24049(7) 0.0367(4) C9 1 0.6295(3) 0.2874(3) 0.17588(8) 0.0397(4) C10 1 0.8200(2) 0.3071(3) 0.13878(7) 0.0403(5) C11 1 0.5679(3) 0.0833(3) 0.18689(10) 0.0517(6) C12 1 0.3762(3) 0.0643(4) 0.22528(9) 0.0498(5) C13 1 0.4000(2) 0.1750(3) 0.28894(8) 0.0397(4) C14 1 0.4471(2) 0.3796(3) 0.27334(7) 0.0388(4) C15 1 0.4104(3) 0.4873(4) 0.33683(9) 0.0479(5) C16 1 0.2348(3) 0.3800(4) 0.36391(7) 0.0449(5) C17 1 0.2137(2) 0.1992(3) 0.32745(8) 0.0452(5) C18 1 0.5568(3) 0.0840(4) 0.33795(10) 0.0525(6) C19 1 1.3937(4) 0.2395(5) -0.01082(12) 0.0689(8) C20 1 0.1855(3) 0.3681(4) 0.43600(8) 0.0548(6) C21 1 0.2735(4) 0.5146(5) 0.48256(10) 0.0734(9) C22 1 0.2168(4) 0.7029(5) 0.45177(11) 0.0727(8) C23 1 0.0350(4) 0.6674(5) 0.40359(12) 0.0698(8) C24 1 0.0411(3) 0.4619(4) 0.38802(8) 0.0516(5) H1 1 0.795(3) 0.061(4) 0.0882(11) 0.0639(12) H2 1 1.067(3) 0.093(4) 0.0272(10) 0.0639(12) H4 1 1.202(3) 0.598(4) 0.1149(11) 0.0639(12) H8 1 0.761(3) 0.347(4) 0.2709(11) 0.0639(12) H9 1 0.522(4) 0.344(4) 0.1462(11) 0.0639(12) H14 1 0.342(4) 0.415(4) 0.2404(12) 0.0639(12) H20 1 0.157(3) 0.238(4) 0.4522(11) 0.0639(12) H24 1 -0.084(4) 0.397(4) 0.3737(12) 0.0639(12) H61 1 1.012(3) 0.598(4) 0.2356(11) 0.0639(12) H62 1 0.937(3) 0.737(4) 0.1765(11) 0.0639(12) H71 1 0.707(3) 0.684(4) 0.2668(11) 0.0639(12) H72 1 0.595(4) 0.648(4) 0.1894(12) 0.0639(12) H111 1 0.538(4) 0.022(4) 0.1439(11) 0.0639(12) H112 1 0.679(4) 0.012(4) 0.2109(11) 0.0639(12) H121 1 0.259(3) 0.113(4) 0.1988(11) 0.0639(12) H122 1 0.351(4) -0.071(4) 0.2334(12) 0.0639(12) H151 1 0.535(4) 0.476(4) 0.3686(11) 0.0639(12) H152 1 0.370(3) 0.615(4) 0.3281(11) 0.0639(12) H181 1 0.566(3) 0.157(4) 0.3799(12) 0.0639(12) H182 1 0.690(3) 0.079(4) 0.3191(10) 0.0639(12) H183 1 0.514(4) -0.047(4) 0.3487(11) 0.0639(12) H191 1 1.414(4) 0.130(4) 0.0121(12) 0.0639(12) H192 1 1.507(4) 0.284(4) -0.0314(11) 0.0639(12) H193 1 1.292(4) 0.207(4) -0.0457(11) 0.0639(12) H211 1 0.221(3) 0.488(4) 0.5283(11) 0.0639(12) H212 1 0.425(3) 0.491(4) 0.4898(11) 0.0639(12) H221 1 0.335(4) 0.753(4) 0.4283(11) 0.0639(12) H222 1 0.186(4) 0.808(4) 0.4842(11) 0.0639(12) H231 1 0.048(4) 0.744(4) 0.3648(12) 0.0639(12) H232 1 -0.088(3) 0.693(4) 0.4265(11) 0.0639(12) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O3 0.0536(7) 0.0040(7) 0.0194(5) 0.0595(8) 0.0003(7) 0.0515(6) O17 0.0480(7) -0.0156(7) 0.0221(7) 0.0597(9) -0.0080(8) 0.0923(10) C1 0.0524(10) -0.0092(9) 0.0113(7) 0.0567(11) -0.0163(9) 0.0513(9) C2 0.0587(10) -0.0002(10) 0.0102(7) 0.0599(11) -0.0133(8) 0.0443(8) C3 0.0427(8) 0.0073(7) 0.0062(6) 0.0532(10) 0.0049(7) 0.0350(7) C4 0.0440(8) 0.0020(7) 0.0061(6) 0.0420(8) 0.0035(7) 0.0428(7) C5 0.0410(7) 0.0036(7) 0.0047(6) 0.0392(7) 0.0028(6) 0.0373(6) C6 0.0508(9) -0.0053(7) 0.0179(7) 0.0392(9) -0.0054(7) 0.0548(9) C7 0.0489(9) 0.0008(7) 0.0170(7) 0.0342(8) -0.0006(7) 0.0546(9) C8 0.0383(7) -0.0007(6) 0.0047(6) 0.0339(7) 0.0002(6) 0.0382(7) C9 0.0390(8) -0.0001(7) 0.0021(6) 0.0413(8) -0.0030(6) 0.0389(7) C10 0.0410(8) 0.0004(7) 0.0010(6) 0.0436(9) -0.0020(6) 0.0361(7) C11 0.0542(10) -0.0090(9) 0.0152(8) 0.0433(9) -0.0130(8) 0.0591(10) C12 0.0471(9) -0.0096(8) 0.0082(7) 0.0445(10) -0.0071(8) 0.0583(9) C13 0.0350(7) -0.0023(7) 0.0046(6) 0.0381(8) 0.0030(6) 0.0464(7) C14 0.0393(8) 0.0000(7) 0.0067(6) 0.0376(8) 0.0010(7) 0.0401(7) C15 0.0501(10) -0.0070(8) 0.0178(7) 0.0460(9) -0.0068(8) 0.0493(8) C16 0.0417(8) -0.0037(8) 0.0100(6) 0.0506(9) 0.0005(8) 0.0434(7) C17 0.0385(8) -0.0032(7) 0.0052(6) 0.0459(9) 0.0049(8) 0.0516(8) C18 0.0446(9) 0.0024(9) 0.0036(8) 0.0512(11) 0.0176(9) 0.0616(10) C19 0.0771(14) 0.0088(12) 0.0355(12) 0.0666(14) -0.0032(11) 0.0669(12) C20 0.0533(10) -0.0132(10) 0.0092(7) 0.0703(13) 0.0050(9) 0.0415(8) C21 0.0736(14) -0.0232(14) 0.0032(9) 0.101(2) -0.0063(11) 0.0456(9) C22 0.0811(15) -0.0212(14) 0.0272(11) 0.0799(16) -0.0240(12) 0.0600(11) C23 0.0751(15) 0.0071(12) 0.0202(11) 0.0701(14) -0.0163(12) 0.0662(12) C24 0.0450(9) -0.0023(9) 0.0107(7) 0.0652(11) -0.0077(9) 0.0457(8) _cod_database_code 2003302