#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006235.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_2006235 loop_ _publ_author_name 'Chen, Hao' 'Tan, Ren-Xiang' 'Liu, Zhi-Li' 'Zhao, Cong-Yuan' 'Sun, Jie' _publ_section_title ; A Clerodane Diterpene with Antibacterial Activity from Ajuga lupulina ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 814 _journal_page_last 816 _journal_paper_doi 10.1107/S0108270196013637 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac 'C30 H46 O11' _chemical_formula_sum 'C30 H46 O11' _chemical_formula_weight 582.7 _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' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.750(2) _cell_length_b 26.735(6) _cell_length_c 10.5330(10) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293 _cell_measurement_theta_max 21.39 _cell_measurement_theta_min 18.71 _cell_volume 3027.2(9) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1985, 1992)' _computing_publication_material SHELXL93 _computing_structure_refinement SHELXTL-Plus _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 20.0 _diffrn_measurement_device 'Rigaku AFC-7R' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.004 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2995 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% none _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.35 _refine_diff_density_min -0.41 _refine_ls_extinction_coef 4E-4(4) _refine_ls_extinction_method 'Zachariasen (1967) type 2, Gaussian isotropic' _refine_ls_goodness_of_fit_obs 2.38 _refine_ls_hydrogen_treatment 'H atoms not refined' _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 2310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_obs .0465 _refine_ls_shift/esd_max 0.020 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0003F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1370 _refine_ls_wR_factor_obs .0614 _reflns_number_observed 2310 _reflns_number_total 2945 _reflns_observed_criterion F>4\s(F) _cod_data_source_file na1249.cif _cod_data_source_block afc7 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 92 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F) + 0.0003F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F) + 0.0003F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 3027.2(15) _cod_database_code 2006235 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) .0700(10) .0690(10) .0570(10) .0160(10) .0070(10) .0160(10) O(2) .0790(10) .0470(10) .0480(10) .0210(10) .0080(10) .0080(10) O(3) .0630(10) .0410(10) .0510(10) .0120(10) .0000(10) -.0120(10) O(4) .0500(10) .0470(10) .0750(10) -.0070(10) .0180(10) -.0070(10) O(5) .0650(10) .0700(10) .0580(10) -.0010(10) -.0030(10) .0060(10) O(6) .0950(10) .0930(10) .0600(10) .0400(10) .0220(10) .0160(10) O(7) .0490(10) .0450(10) .0480(10) .0130(10) -.0020(10) .0060(10) O(8) .0740(10) .0350(10) .0470(10) .0120(10) -.0010(10) .0030(10) O(9) .0710(10) .0480(10) .0490(10) -.0030(10) .0030(10) .0060(10) O(10) .0590(10) .0370(10) .0520(10) -.0040(10) -.0040(10) -.0060(10) O(11) .1290(10) .0540(10) .0740(10) -.0310(10) -.0070(10) .0100(10) C(1) .0650(10) .0540(10) .0580(10) .0160(10) .0020(10) .0080(10) C(2) .0780(10) .0420(10) .0930(10) .0120(10) .0080(10) .0020(10) C(3) .0600(10) .0350(10) .0890(10) -.0020(10) .0010(10) .0030(10) C(4) .0590(10) .0460(10) .0680(10) .0100(10) .0150(10) .0170(10) C(5) .0670(10) .0340(10) .0600(10) .0050(10) -.0020(10) -.0070(10) C(6) .0470(10) .0320(10) .0470(10) .0030(10) .0020(10) .0020(10) C(7) .0500(10) .0340(10) .0440(10) .0040(10) -.0040(10) .0010(10) C(8) .0430(10) .0330(10) .0350(10) .0060(10) -.0010(10) .0020(10) C(9) .0470(10) .0320(10) .0500(10) .0050(10) .0060(10) -.0020(10) C(10) .0430(10) .0380(10) .0480(10) .0000(10) .0030(10) .0010(10) C(11) .0550(10) .0350(10) .0430(10) -.0040(10) -.0030(10) -.0030(10) C(12) .0480(10) .0340(10) .0370(10) .0050(10) -.0010(10) -.0020(10) C(13) .0470(10) .0320(10) .0390(10) .0070(10) -.0030(10) -.0010(10) C(14) .0490(10) .0360(10) .0420(10) .0100(10) .0010(10) .0060(10) C(15) .0470(10) .0440(10) .0560(10) .0020(10) -.0030(10) .0050(10) C(16) .0490(10) .0370(10) .0530(10) .0010(10) -.0050(10) .0040(10) C(17) .0940(10) .0850(10) .0760(10) -.0220(10) -.0320(10) .0140(10) C(18) .0670(10) .0410(10) .0480(10) .0000(10) -.0090(10) -.0030(10) C(19) .0570(10) .0470(10) .0930(10) -.0080(10) -.0030(10) .0040(10) C(20) .0600(10) .0530(10) .0460(10) .0050(10) .0000(10) -.0080(10) C(21) .0530(10) .0500(10) .0480(10) .0110(10) .0030(10) -.0010(10) C(22) .0800(10) .0640(10) .0680(10) .0340(10) .0020(10) -.0060(10) C(23) .0570(10) .0280(10) .0460(10) .0060(10) -.0020(10) .0010(10) C(24) .0450(10) .0410(10) .0420(10) -.0010(10) -.0050(10) .0070(10) C(25) .0900(10) .0430(10) .0730(10) .0060(10) -.0070(10) .0110(10) C(26) .0570(10) .0440(10) .0640(10) -.0070(10) .0090(10) -.0050(10) C(27) .0640(10) .0500(10) .0960(10) -.0100(10) .0140(10) -.0200(10) C(28) .0920(10) .0660(10) .1290(10) -.0280(10) .0030(10) -.0070(10) C(29) .1620(10) .0960(10) .1990(10) -.0450(10) .0780(10) -.0670(10) C(30) .1340(10) .0530(10) .1560(10) .0030(10) -.0060(10) .0110(10) C(30') .1260(10) .0990(10) .0860(10) .0240(10) .0170(10) -.0380(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom O(1) .71440(10) .54510(10) .45500(10) .0650(10) Uani ? ? O(2) .56020(10) .59550(10) .36150(10) .0580(10) Uani ? ? O(3) .51930(10) .83450(10) .35360(10) .0520(10) Uani ? ? O(4) .90460(10) .76400(10) .20180(10) .0570(10) Uani ? ? O(5) .86610(10) .57110(10) .30990(10) .0640(10) Uani ? ? O(6) .23240(10) .78930(10) .4475(2) .0830(10) Uani ? ? O(7) .29980(10) .78780(10) .24790(10) .0470(10) Uani ? ? O(8) .48670(10) .82660(10) .08910(10) .0520(10) Uani ? ? O(9) .51370(10) .82940(10) -.11990(10) .0560(10) Uani ? ? O(10) .77280(10) .84000(10) .32290(10) .0490(10) Uani ? ? O(11) .76300(10) .89220(10) .15670(10) .0860(10) Uani ? ? C(1) .81070(10) .53030(10) .37150(10) .0590(10) Uani ? ? C(2) .74910(10) .49780(10) .27450(10) .0710(10) Uani ? ? C(3) .61750(10) .51920(10) .26360(10) .0620(10) Uani ? ? C(4) .59910(10) .54670(10) .38830(10) .0570(10) Uani ? ? C(5) .59670(10) .55930(10) .16110(10) .0540(10) Uani ? ? C(6) .59970(10) .60910(10) .23600(10) .0420(10) Uani ? ? C(7) .52250(10) .65450(10) .18590(10) .0430(10) Uani ? ? C(8) .58540(10) .70310(10) .23910(10) .0370(10) Uani ? ? C(9) .71870(10) .71170(10) .19220(10) .0430(10) Uani ? ? C(10) .78720(10) .75370(10) .25920(10) .0430(10) Uani ? ? C(11) .71130(10) .80150(10) .25040(10) .0440(10) Uani ? ? C(12) .58310(10) .79180(10) .30400(10) .0400(10) Uani ? ? C(13) .50890(10) .75380(10) .22370(10) .0390(10) Uani ? ? C(14) .37730(10) .74450(10) .27390(10) .0420(10) Uani ? ? C(15) .31620(10) .69960(10) .21290(10) .0490(10) Uani ? ? C(16) .38760(10) .65160(10) .23740(10) .0460(10) Uani ? ? C(17) .91960(10) .60750(10) .39270(10) .0850(10) Uani ? ? C(18) .52710(10) .65340(10) .04010(10) .0520(10) Uani ? ? C(19) .31130(10) .60690(10) .19360(10) .0660(10) Uani ? ? C(20) .56520(10) .79730(10) .44260(10) .0530(10) Uani ? ? C(21) .23380(10) .80640(10) .34330(10) .0500(10) Uani ? ? C(22) .16160(10) .85150(10) .30440(10) .0710(10) Uani ? ? C(23) .50090(10) .77270(10) .08600(10) .0430(10) Uani ? ? C(24) .49690(10) .85050(10) -.02150(10) .0430(10) Uani ? ? C(25) .48300(10) .90530(10) -.0057(2) .0690(10) Uani ? ? C(26) .79120(10) .88420(10) .26470(10) .0550(10) Uani ? ? C(27) .84710(10) .92170(10) .35580(10) .0700(10) Uani ? ? C(28) .92300(10) .95980(10) .28280(10) .0950(10) Uani ? ? C(29) .75870(10) .93870(10) .44890(10) .1520(10) Uani ? ? C(30) .65610(10) .96400(10) .39450(10) .1150(10) Uani ? ? C(30') .74370(10) .98830(10) .49520(10) .1030(10) Uani ? ? H(4A) .9378 .7368 .1773 .080 Uani ? ? H(1A) .8725 .5116 .4173 .080 Uani ? ? H(2A) .7920 .5007 .1949 .080 Uani ? ? H(2B) .7482 .4634 .3002 .080 Uani ? ? H(3A) .5577 .4928 .2544 .080 Uani ? ? H(4B) .5365 .5301 .4377 .080 Uani ? ? H(5A) .6625 .5583 .0995 .080 Uani ? ? H(5B) .5185 .5551 .1184 .080 Uani ? ? H(6A) .6850 .6194 .2423 .080 Uani ? ? H(8A) .5928 .6978 .3289 .080 Uani ? ? H(9A) .7649 .6812 .2026 .080 Uani ? ? H(9B) .7161 .7193 .1032 .080 Uani ? ? H(10A) .7991 .7450 .3468 .080 Uani ? ? H(11A) .7048 .8117 .1633 .080 Uani ? ? H(14A) .3812 .7391 .3639 .080 Uani ? ? H(15A) .2330 .6963 .2448 .080 Uani ? ? H(15B) .3112 .7050 .1229 .080 Uani ? ? H(16A) .3941 .6487 .3280 .080 Uani ? ? H(17A) .9553 .6343 .3443 .080 Uani ? ? H(17B) .9831 .5918 .4428 .080 Uani ? ? H(17C) .8561 .6205 .4475 .080 Uani ? ? H(18A) .6119 .6554 .0121 .080 Uani ? ? H(18B) .4812 .6813 .0071 .080 Uani ? ? H(18C) .4906 .6228 .0101 .080 Uani ? ? H(19A) .2298 .6085 .2306 .080 Uani ? ? H(19B) .3514 .5764 .2196 .080 Uani ? ? H(19C) .3045 .6075 .1028 .080 Uani ? ? H(20A) .6368 .8059 .4925 .080 Uani ? ? H(20B) .5062 .7759 .4840 .080 Uani ? ? H(22A) .1157 .8639 .3759 .080 Uani ? ? H(22B) .1048 .8425 .2378 .080 Uani ? ? H(22C) .2171 .8770 .2743 .080 Uani ? ? H(23A) .4305 .7578 .0447 .080 Uani ? ? H(23B) .5747 .7635 .0401 .080 Uani ? ? H(25A) .4900 .9215 -.0867 .080 Uani ? ? H(25B) .5473 .9172 .0498 .080 Uani ? ? H(25C) .4031 .9126 .0306 .080 Uani ? ? H(27A) .9067 .9031 .4045 .080 Uani ? ? H(28A) .9593 .9834 .3405 .080 Uani ? ? H(28B) .8695 .9770 .2244 .080 Uani ? ? H(28C) .9877 .9430 .2366 .080 Uani ? ? H(29B) .7917 .9663 .4965 .080 Uani ? ? H(29C) .6889 .9505 .4006 .080 Uani ? ? H(29A) .7323 .9128 .5059 .080 Uani ? ? H(30A) .6043 .9738 .4644 .080 Uani ? ? H(30B) .6098 .9426 .3385 .080 Uani ? ? H(30C) .6829 .9932 .3491 .080 Uani ? ? H(30D) .6692 .9893 .5454 .080 Uani ? ? H(30E) .7409 1.0144 .4326 .080 Uani ? ? H(30F) .8147 .9931 .5490 .080 Uani ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' O 0.011 0.006 'International Tables' 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 C(1) O(1) C(4) 109.80(10) no C(4) O(2) C(6) 109.50(10) no C(12) O(3) C(20) 61.80(10) yes C(1) O(5) C(17) 114.70(10) yes C(14) O(7) C(21) 117.60(10) no C(23) O(8) C(24) 116.60(10) no C(11) O(10) C(26) 116.90(10) no O(1) C(1) O(5) 112.3(2) no O(1) C(1) C(2) 105.30(10) no O(5) C(1) C(2) 108.80(10) yes C(1) C(2) C(3) 104.20(10) no C(2) C(3) C(4) 103.70(10) yes C(2) C(3) C(5) 116.60(10) yes C(4) C(3) C(5) 104.60(10) no O(1) C(4) O(2) 112.90(10) yes O(1) C(4) C(3) 107.30(10) no O(2) C(4) C(3) 108.40(10) yes C(3) C(5) C(6) 103.80(10) no O(2) C(6) C(5) 104.30(10) no O(2) C(6) C(7) 110.50(10) yes C(5) C(6) C(7) 119.00(10) no C(6) C(7) C(8) 107.10(10) yes C(6) C(7) C(16) 109.90(10) no C(8) C(7) C(16) 108.70(10) no C(6) C(7) C(18) 107.70(10) no C(8) C(7) C(18) 111.10(10) no C(16) C(7) C(18) 112.20(10) no C(7) C(8) C(9) 114.40(10) no C(7) C(8) C(13) 116.40(10) no C(9) C(8) C(13) 108.80(10) no C(8) C(9) C(10) 114.50(10) no O(4) C(10) C(9) 112.00(10) yes O(4) C(10) C(11) 106.70(10) no C(9) C(10) C(11) 109.50(10) no O(10) C(11) C(10) 108.80(10) no O(10) C(11) C(12) 110.10(10) no C(10) C(11) C(12) 108.80(10) no O(3) C(12) C(11) 115.60(10) yes O(3) C(12) C(13) 118.60(10) no C(11) C(12) C(13) 112.30(10) no O(3) C(12) C(20) 59.90(10) yes C(11) C(12) C(20) 118.00(10) no C(13) C(12) C(20) 122.60(10) yes C(8) C(13) C(12) 103.80(10) yes C(8) C(13) C(14) 107.70(10) no C(12) C(13) C(14) 113.30(10) no C(8) C(13) C(23) 113.80(10) no C(12) C(13) C(23) 109.20(10) yes C(14) C(13) C(23) 109.10(10) no O(7) C(14) C(13) 109.60(10) no O(7) C(14) C(15) 107.70(10) no C(13) C(14) C(15) 112.60(10) no C(14) C(15) C(16) 112.30(10) no C(7) C(16) C(15) 111.80(10) no C(7) C(16) C(19) 115.90(10) no C(15) C(16) C(19) 110.00(10) no O(3) C(20) C(12) 58.30(10) no O(6) C(21) O(7) 124.2(2) yes O(6) C(21) C(22) 123.90(10) no O(7) C(21) C(22) 111.90(10) no O(8) C(23) C(13) 108.10(10) no O(8) C(24) O(9) 123.0(2) no O(8) C(24) C(25) 111.50(10) no O(9) C(24) C(25) 125.50(10) no O(10) C(26) O(11) 123.5(2) no O(10) C(26) C(27) 110.60(10) no O(11) C(26) C(27) 125.8(2) no C(26) C(27) C(28) 109.70(10) no C(26) C(27) C(29) 112.30(10) no C(28) C(27) C(29) 119.4(2) no C(27) C(29) C(30) 112.90(10) no C(27) C(29) C(30') 127.00(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(1) ? ? 1.4150(10) yes O(1) C(4) ? ? 1.4260(10) no O(2) C(4) ? ? 1.397(2) no O(2) C(6) ? ? 1.4350(10) no O(3) C(12) ? ? 1.429(2) yes O(3) C(20) ? ? 1.453(2) yes O(4) C(10) ? ? 1.4260(10) yes O(5) C(1) ? ? 1.402(2) no O(5) C(17) ? ? 1.427(2) yes O(6) C(21) ? ? 1.1880(10) yes O(7) C(14) ? ? 1.453(2) no O(7) C(21) ? ? 1.3280(10) no O(8) C(23) ? ? 1.451(2) no O(8) C(24) ? ? 1.333(2) no O(9) C(24) ? ? 1.194(2) no O(10) C(11) ? ? 1.442(2) no O(10) C(26) ? ? 1.345(2) no O(11) C(26) ? ? 1.1960(10) no C(1) C(2) ? ? 1.494(2) no C(2) C(3) ? ? 1.531(2) no C(3) C(4) ? ? 1.519(2) no C(3) C(5) ? ? 1.537(2) no C(5) C(6) ? ? 1.546(2) no C(6) C(7) ? ? 1.564(2) no C(7) C(8) ? ? 1.568(2) no C(7) C(16) ? ? 1.5510(10) no C(7) C(18) ? ? 1.5360(10) no C(8) C(9) ? ? 1.5320(10) no C(8) C(13) ? ? 1.593(2) yes C(9) C(10) ? ? 1.517(2) no C(10) C(11) ? ? 1.519(2) no C(11) C(12) ? ? 1.5120(10) no C(12) C(13) ? ? 1.545(2) no C(12) C(20) ? ? 1.4800(10) yes C(13) C(14) ? ? 1.5310(10) yes C(13) C(23) ? ? 1.5380(10) yes C(14) C(15) ? ? 1.511(2) no C(15) C(16) ? ? 1.516(2) no C(16) C(19) ? ? 1.522(2) no C(21) C(22) ? ? 1.492(2) no C(24) C(25) ? ? 1.481(3) no C(26) C(27) ? ? 1.512(2) no C(27) C(28) ? ? 1.514(2) no C(27) C(29) ? ? 1.4390(10) no C(29) C(30) ? ? 1.415(2) no C(29) C(30') ? ? 1.423(3) no C(30) C(30') ? ? 1.560(5) no