#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003251.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_2003251 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 415 _journal_page_last 419 _publ_section_title ; 9,11-Secogorgost-5-en-9-one-3\b,11-diol, a Marine Steroid from the Sea Whip Pseudopterogorgia hummelinkii ; _chemical_formula_sum 'C30 H50 O3' _chemical_formula_weight 458.73 _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,y+1/2,-z' _cell_length_a 11.186(1) _cell_length_b 15.064(3) _cell_length_c 17.281(5) _cell_angle_alpha 90 _cell_angle_beta 103.90(2) _cell_angle_gamma 90 _cell_volume 2826.7 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_meas 1.077(5) _exptl_crystal_density_method ; Flotation in a hexane-CCl~4~ mixture ; _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.39 _cell_measurement_theta_max 22.48 _exptl_absorpt_coefficient_mu 0.486 _cell_measurement_temperature 296 _exptl_crystal_description 'Block' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour 'Colorless' _chemical_compound_source ; slow evaporation from CH~2~Cl~2~/iso-octane solution ; _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 4186 _reflns_number_total 4028 _reflns_number_observed 3602 _reflns_observed_criterion F>4\s(F) _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_theta_max 58 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% +-2.6 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0529 _refine_ls_wR_factor_obs 0.0674 _refine_ls_goodness_of_fit_obs 1.1313 _refine_ls_number_reflns 4028 _refine_ls_number_parameters 650 _refine_ls_hydrogen_treatment 'see text' _refine_ls_weighting_scheme 'w=1/[\s^2^(F) + 0.0025F^2^]' _refine_ls_shift/esd_max 0.34 _refine_diff_density_max 0.28 _refine_diff_density_min -0.24 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef none _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1a .2965(4) .8002 .5981(3) .077(2) C2a .2832(4) .7642(6) .5141(3) .087(2) C3a .1827(4) .6959(6) .4942(2) .077(2) O3a .1756(3) .6619(5) .4147(2) .100(2) C4a .0609(4) .7335(6) .5031(2) .065(2) C5a .0738(3) .7718(5) .5859(2) .052(1) C6a .0053(4) .7442(5) .6341(2) .061(1) C7a .0149(5) .7800(5) .7172(3) .069(2) C8a .0744(3) .8725(5) .7269(2) .046(1) C9a .1913(3) .8602(5) .6996(2) .048(1) O9a .2926(2) .8615(5) .7456(2) .063(1) C10a .1750(3) .8399(5) .6111(2) .052(1) C19a .1458(5) .9286(6) .5655(3) .079(2) O11a .0420(3) 1.1829(5) .6985(2) .089(1) C11a .0838(4) 1.1141(5) .7538(2) .058(1) C12a -.0260(3) 1.0602(5) .7626(2) .047(1) C13a -.0037(3) .9834(5) .8230(2) .042(1) C18a -.1264(3) .9363(5) .8145(2) .055(1) C14a .0980(3) .9182(5) .8094(2) .048(1) C15a .1245(4) .8594(5) .8837(2) .057(1) C16a .1025(4) .9188(5) .9508(2) .054(1) C17a .0547(3) 1.0094(5) .9123(2) .043(1) C20a -.0244(3) 1.0643(5) .9562(2) .048(1) C21a -.0209(5) 1.1634(5) .9368(3) .075(2) C22a .0108(3) 1.0554(5) 1.0472(2) .045(1) C23a -.0476(3) .9955(5) 1.0980(2) .047(1) C34a -.0772(5) 1.0924(5) 1.0914(3) .067(2) C33a -.1448(4) .9295(6) 1.0593(3) .072(2) C24a .0366(3) .9663(5) 1.1777(2) .054(1) C28a .1246(5) .8939(6) 1.1666(3) .095(2) C25a -.0342(5) .9393(6) 1.2406(3) .077(2) C26a .0512(6) .9200(7) 1.3215(3) .115(3) C27a -.1297(6) 1.0068(7) 1.2506(3) .103(3) H1b .7793 .9254 .4298 .085(2) H2b .8365 .8477 .4872 .085(2) H3b .8229 .9788 .5590 .085(2) H4b .7464 .9020 .5851 .085(2) H5b .6477 1.0360 .4782 .085(2) H6b .6810 1.0906 .5938 .085(2) H7b .5156 .9032 .5356 .085(2) H8b .4541 .9791 .4775 .085(2) H9b .3868 .9281 .3480 .085(2) H10b .3926 .8285 .2462 .085(2) H11b .5101 .8855 .2472 .085(2) H12b .5026 .7188 .3131 .085(2) H13b .6365 .7763 .5385 .119(3) H14b .5703 .7140 .4687 .119(3) H15b .7137 .7094 .5008 .119(3) H16b .5108 .5560 .3583 .085(2) H17b .5902 .5081 .2404 .085(2) H18b .4830 .4666 .2725 .085(2) H19b .3816 .5454 .1740 .085(2) H20b .3880 .6097 .2462 .085(2) H21b .4001 .7583 .0950 .119(3) H22b .3205 .6715 .0858 .119(3) H23b .3290 .7333 .1599 .119(3) H24b .6448 .6772 .2574 .085(2) H25b .5896 .8240 .1531 .085(2) H26b .7208 .7846 .1892 .085(2) H27b .7040 .6998 .0823 .085(2) H28b .5735 .7402 .0457 .085(2) H29b .6209 .5795 .1344 .085(2) H30b .4192 .5907 .0190 .085(2) H31b .4531 .4619 .0977 .119(3) H32b .4682 .4317 .0138 .119(3) H33b .5850 .4509 .0826 .119(3) H34b .6413 .5726 .0060 .085(2) H35b .4193 .5106 -.1182 .085(2) H36b .5474 .4969 -.1385 .085(2) H37b .4405 .7506 -.0967 .119(3) H38b .3688 .6950 -.1699 .119(3) H39b .3541 .6728 -.0841 .119(3) H40b .6787 .6183 -.1414 .085(2) H41b .7606 .7584 -.1212 .119(3) H42b .6331 .7974 -.1153 .119(3) H43b .7088 .7374 -.0466 .119(3) H44b .5188 .7350 -.2391 .085(2) H45b .7412 .7535 -.2525 .119(3) H46b .7029 .6537 -.2675 .119(3) H47b .6424 .7264 -.3296 .119(3) H48b .4262 .6038 -.2628 .119(3) H49b .4749 .6209 -.3393 .119(3) H50b .5504 .5609 -.2706 .119(3) C1b .7663(4) .8858(6) .4705(2) .067(2) C2b .7522(4) .9411(6) .5422(3) .079(2) C3b .6384(4) .9977(5) .5208(2) .065(2) O3b .6246(3) 1.0516(5) .5865(2) .081(1) C4b .5250(4) .9414(5) .4930(3) .065(2) C5b .5373(3) .8851(5) .4220(2) .058(1) C6b .4583(4) .8915(6) .3518(3) .069(2) C7b .4727(5) .8451(6) .2772(3) .086(2) C8b .5520(3) .7625(5) .2949(2) .050(1) C9b .6683(3) .7870(5) .3583(2) .053(1) O9b .7696(3) .7730(5) .3487(2) .078(1) C10b .6522(3) .8278(5) .4352(2) .053(1) C19b .6434(5) .7480(6) .4900(3) .084(2) O11b .5778(4) .5563(5) .3432(2) .098(2) C11b .5249(5) .5207(6) .2660(3) .079(2) C12b .4350(4) .5816(5) .2134(3) .066(2) C13b .4859(3) .6557(5) .1686(2) .050(1) C18b .3733(4) .7101(6) .1232(3) .069(2) C14b .5839(3) .7142(5) .2239(2) .046(1) C15b .6361(4) .7702(5) .1663(2) .058(1) C16b .6242(4) .7116(5) .0916(2) .055(1) C17b .5636(3) .6246(5) .1099(2) .044(1) C20b .5015(3) .5679(3) .0362(2) .051(1) C21b .5017(6) .4685(5) .0592(3) .082(2) C22b .5640(3) .5756(5) -.0329(2) .048(1) C23b .5216(3) .6323(5) -.1075(2) .048(1) C34b .5012(5) .5338(5) -.1109(3) .067(2) C33b .4104(4) .6926(6) -.1145(3) .075(2) C24b .6208(4) .6663(5) -.1463(2) .061(1) C28b .6873(6) .7472(6) -.1031(3) .099(2) C25b .5739(6) .6856(6) -.2365(3) .088(2) C26b .6742(9) .7139(9) -.2740(4) .176(5) C27b .4985(8) .6123(7) -.2826(3) .125(3) H1a .3221 .7527 .6354 .085(2) H2a .3583 .8458 .6076 .085(2) H3a .3596 .7375 .5105 .085(2) H4a .2637 .8123 .4768 .085(2) H5a .2016 .6474 .5311 .085(2) H6a .0990 .6591 .3930 .085(2) H7a .0004 .6870 .4944 .085(2) H8a .0348 .7795 .4643 .085(2) H9a -.0543 .6985 .6150 .085(2) H10a -.0661 .7839 .7266 .085(2) H11a .0643 .7403 .7553 .085(2) H12a .0166 .9138 .6961 .085(2) H13a .1411 .9198 .5098 .119(3) H14a .0694 .9528 .5720 .119(3) H15a .2116 .9691 .5872 .119(3) H16a .1051 1.2083 .6895 .085(2) H17a .1403 1.0768 .7349 .085(2) H18a .1245 1.1390 .8045 .085(2) H19a -.0828 1.1004 .7779 .085(2) H20a -.0629 1.0353 .7113 .085(2) H21a -.1180 .8911 .8546 .119(3) H22a -.1814 .9815 .8240 .119(3) H23a -.1588 .9104 .7629 .119(3) H24a .1713 .9488 .8047 .085(2) H25a .0697 .8094 .8760 .085(2) H26a .2081 .8389 .8957 .085(2) H27a .0421 .8925 .9749 .085(2) H28a .1780 .9272 .9905 .085(2) H29a .1189 1.0526 .9161 .085(2) H30a -.1054 1.0398 .9369 .085(2) H31a -.0480 1.1709 .8802 .119(3) H32a -.0734 1.1969 .9626 .119(3) H33a .0623 1.1843 .9547 .119(3) H34a .0951 1.0617 1.0445 .085(2) H35a -.0478 1.1307 1.1364 .085(2) H36a -.1574 1.1117 1.0627 .085(2) H37a -.1020 .8759 1.0524 .119(3) H38a -.2048 .9168 1.0892 .119(3) H39a -.1853 .9528 1.0080 .119(3) H40a .0839 1.0180 1.1984 .085(2) H41a .1829 .8760 1.2144 .119(3) H42a .0745 .8440 1.1445 .119(3) H43a .1678 .9154 1.1286 .119(3) H44a -.0764 .8857 1.2198 .085(2) H45a .1084 .8727 1.3208 .119(3) H46a .0954 .9746 1.3350 .119(3) H47a .0050 .9072 1.3603 .119(3) H48a -.1905 1.0279 1.2052 .119(3) H49a -.1696 .9874 1.2910 .119(3) H50a -.0731 1.0538 1.2713 .119(3) _cod_database_code 2003251