#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003251.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003251 loop_ _publ_author_name 'Schultz, L. W.' 'Clardy, J.' 'Lessinger, L.' _publ_section_title ; 9,11-Secogorgost-5-en-9-one-3\b,11-diol, a Marine Steroid from the Sea Whip Pseudopterogorgia hummelinkii ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 415 _journal_page_last 419 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C30 H50 O3' _chemical_formula_weight 458.73 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 103.90(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.1860(10) _cell_length_b 15.064(3) _cell_length_c 17.281(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296 _cell_measurement_theta_max 22.48 _cell_measurement_theta_min 15.39 _cell_volume 2826.7(11) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \q/2\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4186 _diffrn_reflns_theta_max 58 _diffrn_standards_decay_% +-2.6 _diffrn_standards_interval_count 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_meas 1.077(5) _exptl_crystal_density_method ' Flotation in a hexane-CCl~4~ mixture' _exptl_crystal_description Block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.28 _refine_diff_density_min -0.24 _refine_ls_extinction_coef none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.1313 _refine_ls_hydrogen_treatment 'see text' _refine_ls_number_parameters 650 _refine_ls_number_reflns 4028 _refine_ls_R_factor_obs 0.0529 _refine_ls_shift/esd_max 0.34 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w=1/[\s^2^(F) + 0.0025F^2^]' _refine_ls_wR_factor_obs 0.0674 _reflns_number_observed 3602 _reflns_number_total 4028 _reflns_observed_criterion F>4\s(F) _[local]_cod_data_source_file cr1102.cif _[local]_cod_data_source_block cr1102a _[local]_cod_cif_authors_sg_Hall 'P 2y1' _cod_original_cell_volume 2826.7 _cod_database_code 2003251 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z 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) .0520(10) C6a .0053(4) .7442(5) .6341(2) .0610(10) C7a .0149(5) .7800(5) .7172(3) .069(2) C8a .0744(3) .8725(5) .7269(2) .0460(10) C9a .1913(3) .8602(5) .6996(2) .0480(10) O9a .2926(2) .8615(5) .7456(2) .0630(10) C10a .1750(3) .8399(5) .6111(2) .0520(10) C19a .1458(5) .9286(6) .5655(3) .079(2) O11a .0420(3) 1.1829(5) .6985(2) .0890(10) C11a .0838(4) 1.1141(5) .7538(2) .0580(10) C12a -.0260(3) 1.0602(5) .7626(2) .0470(10) C13a -.0037(3) .9834(5) .8230(2) .0420(10) C18a -.1264(3) .9363(5) .8145(2) .0550(10) C14a .0980(3) .9182(5) .8094(2) .0480(10) C15a .1245(4) .8594(5) .8837(2) .0570(10) C16a .1025(4) .9188(5) .9508(2) .0540(10) C17a .0547(3) 1.0094(5) .9123(2) .0430(10) C20a -.0244(3) 1.0643(5) .9562(2) .0480(10) C21a -.0209(5) 1.1634(5) .9368(3) .075(2) C22a .0108(3) 1.0554(5) 1.0472(2) .0450(10) C23a -.0476(3) .9955(5) 1.0980(2) .0470(10) 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) .0540(10) 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) .0810(10) C4b .5250(4) .9414(5) .4930(3) .065(2) C5b .5373(3) .8851(5) .4220(2) .0580(10) 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) .0500(10) C9b .6683(3) .7870(5) .3583(2) .0530(10) O9b .7696(3) .7730(5) .3487(2) .0780(10) C10b .6522(3) .8278(5) .4352(2) .0530(10) 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) .0500(10) C18b .3733(4) .7101(6) .1232(3) .069(2) C14b .5839(3) .7142(5) .2239(2) .0460(10) C15b .6361(4) .7702(5) .1663(2) .0580(10) C16b .6242(4) .7116(5) .0916(2) .0550(10) C17b .5636(3) .6246(5) .1099(2) .0440(10) C20b .5015(3) .5679(3) .0362(2) .0510(10) C21b .5017(6) .4685(5) .0592(3) .082(2) C22b .5640(3) .5756(5) -.0329(2) .0480(10) C23b .5216(3) .6323(5) -.1075(2) .0480(10) 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) .0610(10) 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) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2a C1a C10a 112.8(3) yes C1a C2a C3a 111.1(4) yes C2a C3a O3a 109.1(5) yes C2a C3a C4a 111.2(6) yes O3a C3a C4a 112.4(3) yes C3a C4a C5a 110.7(3) yes C4a C5a C6a 122.3(5) yes C4a C5a C10a 115.2(4) yes C6a C5a C10a 122.4(4) yes C5a C6a C7a 124.4(6) yes C6a C7a C8a 110.9(5) yes C7a C8a C9a 103.9(5) yes C7a C8a C14a 118.6(4) yes C9a C8a C14a 112.0(3) yes C8a C9a O9a 122.4(3) yes C8a C9a C10a 115.8(3) yes O9a C9a C10a 121.7(4) yes C1a C10a C5a 108.5(5) yes C1a C10a C9a 108.9(3) yes C5a C10a C9a 109.0(4) yes C1a C10a C19a 110.1(4) yes C5a C10a C19a 112.8(4) yes C9a C10a C19a 107.3(5) yes O11a C11a C12a 108.5(4) yes C11a C12a C13a 118.0(3) yes C12a C13a C18a 106.9(3) yes C12a C13a C14a 112.1(3) yes C18a C13a C14a 111.4(6) yes C12a C13a C17a 116.1(5) yes C18a C13a C17a 111.3(3) yes C14a C13a C17a 99.1(3) yes C8a C14a C13a 116.7(3) yes C8a C14a C15a 118.1(6) yes C13a C14a C15a 103.8(3) yes C14a C15a C16a 105.3(6) yes C15a C16a C17a 106.8(4) yes C13a C17a C16a 102.8(5) yes C13a C17a C20a 117.7(3) yes C16a C17a C20a 116.1(4) yes C17a C20a C21a 111.6(4) yes C17a C20a C22a 115.0(4) yes C21a C20a C22a 107.1(5) yes C2b C1b C10b 113.1(4) yes C1b C2b C3b 110.7(4) yes C2b C3b O3b 111.8(4) yes C2b C3b C4b 111.0(6) yes O3b C3b C4b 109.2(4) yes C3b C4b C5b 109.8(4) yes C4b C5b C6b 121.9(5) yes C4b C5b C10b 115.6(3) yes C6b C5b C10b 122.3(5) yes C5b C6b C7b 124.4(5) yes C6b C7b C8b 112.7(4) yes C7b C8b C9b 107.6(6) yes C7b C8b C14b 117.6(4) yes C9b C8b C14b 111.4(3) yes C8b C9b O9b 121.6(4) yes C8b C9b C10b 117.8(3) yes O9b C9b C10b 120.5(4) yes C1b C10b C5b 109.0(6) yes C1b C10b C9b 108.4(4) yes C5b C10b C9b 112.0(3) yes C1b C10b C19b 111.4(4) yes C5b C10b C19b 110.9(4) yes C9b C10b C19b 105.1(6) yes O11b C11b C12b 113.8(6) yes C11b C12b C13b 118.3(4) yes C12b C13b C18b 106.6(4) yes C12b C13b C14b 113.3(3) yes C18b C13b C14b 112.4(6) yes C12b C13b C17b 116.1(6) yes C18b C13b C17b 109.9(3) yes C14b C13b C17b 98.6(3) yes C8b C14b C13b 119.8(3) yes C8b C14b C15b 117.2(6) yes C13b C14b C15b 103.8(3) yes C14b C15b C16b 105.1(5) yes C15b C16b C17b 105.5(4) yes C13b C17b C16b 102.7(5) yes C13b C17b C20b 119.3(3) yes C16b C17b C20b 115.6(4) yes C17b C20b C21b 110.5(4) yes C17b C20b C22b 113.6(4) yes C21b C20b C22b 107.5(5) yes C20a C22a C23a 127.4(4) yes C20a C22a C34a 117.1(4) yes C23a C22a C34a 59.7(4) yes C22a C23a C34a 59.5(4) yes C22a C23a C33a 120.1(3) yes C34a C23a C33a 119.2(4) yes C22a C23a C24a 115.8(3) yes C34a C23a C24a 115.2(5) yes C33a C23a C24a 115.5(6) yes C22a C34a C23a 60.8(4) yes C23a C24a C28a 111.7(4) yes C23a C24a C25a 113.5(3) yes C28a C24a C25a 111.0(6) yes C24a C25a C26a 112.5(5) yes C24a C25a C27a 113.5(6) yes C26a C25a C27a 109.1(5) yes C20b C22b C23b 126.6(4) yes C20b C22b C34b 117.8(4) yes C23b C22b C34b 59.4(4) yes C22b C23b C34b 59.5(4) yes C22b C23b C33b 119.0(4) yes C34b C23b C33b 118.3(4) yes C22b C23b C24b 116.8(3) yes C34b C23b C24b 115.9(5) yes C33b C23b C24b 115.7(6) yes C22b C34b C23b 61.1(4) yes C23b C24b C28b 112.1(5) yes C23b C24b C25b 113.6(4) yes C28b C24b C25b 110.4(6) yes C24b C25b C26b 112.6(5) yes C24b C25b C27b 114.1(7) yes C26b C25b C27b 111.6(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1a C2a 1.522(7) yes C1a C10a 1.551(6) yes C2a C3a 1.502(10) yes C3a O3a 1.450(6) yes C3a C4a 1.517(8) yes C4a C5a 1.517(7) yes C5a C6a 1.327(7) yes C5a C10a 1.512(8) yes C6a C7a 1.513(7) yes C7a C8a 1.536(10) yes C8a C9a 1.504(6) yes C8a C14a 1.548(6) yes C9a O9a 1.218(4) yes C9a C10a 1.526(5) yes C10a C19a 1.546(10) yes O11a C11a 1.412(9) yes C11a C12a 1.510(8) yes C12a C13a 1.537(8) yes C13a C18a 1.520(7) yes C13a C14a 1.563(8) yes C13a C17a 1.574(5) yes C14a C15a 1.529(7) yes C15a C16a 1.531(8) yes C16a C17a 1.555(9) yes C17a C20a 1.538(7) yes C20a C21a 1.533(11) yes C20a C22a 1.533(5) yes C22a C23a 1.512(8) yes C22a C34a 1.492(7) yes C23a C34a 1.495(11) yes C23a C33a 1.507(8) yes C23a C24a 1.534(5) yes C24a C28a 1.513(10) yes C24a C25a 1.545(7) yes C25a C26a 1.520(7) yes C25a C27a 1.515(11) yes C1b C2b 1.533(9) yes C1b C10b 1.546(8) yes C2b C3b 1.502(8) yes C3b O3b 1.434(8) yes C3b C4b 1.505(8) yes C4b C5b 1.524(8) yes C5b C6b 1.322(5) yes C5b C10b 1.520(8) yes C6b C7b 1.508(8) yes C7b C8b 1.516(10) yes C8b C9b 1.532(5) yes C8b C14b 1.540(7) yes C9b O9b 1.203(5) yes C9b C10b 1.512(7) yes C10b C19b 1.548(10) yes O11b C11b 1.427(7) yes C11b C12b 1.496(9) yes C12b C13b 1.543(9) yes C13b C18b 1.549(7) yes C13b C14b 1.545(7) yes C13b C17b 1.559(6) yes C14b C15b 1.524(8) yes C15b C16b 1.544(8) yes C16b C17b 1.543(10) yes C17b C20b 1.552(7) yes C20b C21b 1.549(11) yes C20b C22b 1.527(6) yes C22b C23b 1.524(7) yes C22b C34b 1.500(7) yes C23b C34b 1.499(11) yes C23b C33b 1.521(8) yes C23b C24b 1.517(7) yes C24b C28b 1.526(10) yes C24b C25b 1.549(6) yes C25b C26b 1.486(12) yes C25b C27b 1.498(12) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag C10a C5a C6a C7a 3.2 yes C5a C6a C7a C8a 21.5 yes C6a C7a C8a C9a -52.0 yes C7a C8a C9a C10a 67.1 yes C8a C9a C10a C5a -43.8 yes C6a C5a C10a C9a 6.5 yes C4a C5a C6a C7a 179.8 yes C6a C7a C8a C14a -177.0 yes C14a C8a C9a O9a 20.0 yes C7a C8a C9a O9a -109.1 yes O9a C9a C10a C5a 132.4 yes O9a C9a C10a C19a -105.0 yes C8a C9a C10a C1a -162.1 yes O9a C9a C10a C1a 14.2 yes C6a C5a C10a C1a 125.0 yes C17a C13a C14a C15a 45.8 yes C13a C14a C15a C16a -31.4 yes C14a C15a C16a C17a 3.9 yes C15a C16a C17a C13a 24.8 yes C14a C13a C17a C16a -42.6 yes C10b C5b C6b C7b -1.0 yes C5b C6b C7b C8b 24.4 yes C6b C7b C8b C9b -47.6 yes C7b C8b C9b C10b 54.9 yes C8b C9b C10b C5b -33.1 yes C6b C5b C10b C9b 4.7 yes C4b C5b C6b C7b 173.2 yes C6b C7b C8b C14b -174.3 yes C14b C8b C9b O9b 3.7 yes C7b C8b C9b O9b -126.6 yes O9b C9b C10b C5b 148.4 yes O9b C9b C10b C19b -91.1 yes C8b C9b C10b C1b -153.4 yes O9b C9b C10b C1b 28.1 yes C6b C5b C10b C1b 124.6 yes C17b C13b C14b C15b 46.9 yes C13b C14b C15b C16b -30.1 yes C14b C15b C16b C17b 0.8 yes C15b C16b C17b C13b 28.4 yes C14b C13b C17b C16b -45.8 yes