#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/8101472.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_8101472 _journal_name_full 'Zeitschrift fur Kristallographie - NCS' _journal_year 1999 _publ_section_title ; Trimethyl 3-Methyl-4-oxo-E-8-cyclodecene-1,1,6-tricarboxylate ; loop_ _publ_author_name 'Ullmann, Astrid' 'Zahn, Gernot' 'Schnaubelt, J\"urgen' 'Reissig, Hans-Ulrich' _chemical_formula_moiety 'C17 H24 O7' _chemical_formula_sum 'C17 H24 O7' _chemical_formula_iupac 'C17 H24 O7' _chemical_formula_weight 340.36 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8574(6) _cell_length_b 14.7910(11) _cell_length_c 16.8742(15) _cell_angle_alpha 107.160(5) _cell_angle_beta 99.995(5) _cell_angle_gamma 97.512(5) _cell_volume 1810.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _exptl_crystal_density_diffrn 1.249 _refine_ls_R_factor_obs 0.0494 _refine_ls_wR_factor_obs 0.0948 _refine_diff_density_rms 0.032 loop_ _atom_site_label _atom_site_type_symbol _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_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.6505(2) 0.81502(12) 0.18721(11) 0.0683(5) Uani 1 d . . O2 O -0.0726(2) 0.76471(12) 0.02533(10) 0.0619(5) Uani 1 d . . O3 O 0.0139(2) 0.62319(12) -0.01058(10) 0.0683(5) Uani 1 d . . O4 O 0.1096(2) 0.6400(2) 0.23083(13) 0.0999(7) Uani 1 d . . O5 O -0.1357(2) 0.64166(13) 0.14495(10) 0.0669(5) Uani 1 d . . O6 O 0.7238(3) 1.1272(2) 0.0967(2) 0.1089(8) Uani 1 d . . O7 O 0.9443(2) 1.05736(13) 0.13269(12) 0.0758(5) Uani 1 d . . C1 C 0.5670(3) 0.8185(2) 0.12096(15) 0.0519(6) Uani 1 d . . C2 C 0.4082(3) 0.7410(2) 0.06828(14) 0.0515(6) Uani 1 d . . H2 H 0.3275(3) 0.7705(2) 0.03713(14) 0.059(7) Uiso 1 calc R . C3 C 0.4736(4) 0.6652(2) 0.0031(2) 0.0713(8) Uani 1 d . . H3A H 0.3760(4) 0.6149(2) -0.0314(2) 0.085(9) Uiso 1 calc R . H3B H 0.5589(4) 0.6383(2) 0.0324(2) 0.093(10) Uiso 1 calc R . H3C H 0.5269(4) 0.6949(2) -0.0324(2) 0.089(10) Uiso 1 calc R . C4 C 0.3079(3) 0.6966(2) 0.1223(2) 0.0576(6) Uani 1 d . . H4A H 0.3822(3) 0.7143(2) 0.1789(2) 0.060(7) Uiso 1 calc R . H4B H 0.2880(3) 0.6269(2) 0.0978(2) 0.063(7) Uiso 1 calc R . C5 C 0.1290(3) 0.7264(2) 0.13065(14) 0.0505(6) Uani 1 d . . C6 C 0.0116(3) 0.7092(2) 0.04371(14) 0.0492(6) Uani 1 d . . C7 C -0.0981(5) 0.5988(3) -0.0947(2) 0.0949(10) Uani 1 d . . H7A H -0.0896(24) 0.5356(7) -0.1286(5) 0.142(14) Uiso 1 calc R . H7B H -0.0610(20) 0.6450(10) -0.1210(6) 0.149(17) Uiso 1 calc R . H7C H -0.2180(7) 0.5998(16) -0.0900(2) 0.181(20) Uiso 1 calc R . C8 C 0.0368(3) 0.6645(2) 0.1747(2) 0.0590(7) Uani 1 d . . C9 C -0.2397(4) 0.5916(2) 0.1874(2) 0.0768(8) Uani 1 d . . H9A H -0.3572(9) 0.5672(15) 0.1531(7) 0.149(15) Uiso 1 calc R . H9B H -0.2435(25) 0.6354(5) 0.2416(7) 0.135(14) Uiso 1 calc R . H9C H -0.1877(18) 0.5389(10) 0.1956(13) 0.189(19) Uiso 1 calc R . C10 C 0.1463(3) 0.8321(2) 0.18768(15) 0.0628(7) Uani 1 d . . H10A H 0.0289(3) 0.8452(2) 0.18913(15) 0.073(8) Uiso 1 calc R . H10B H 0.2044(3) 0.8384(2) 0.24521(15) 0.062(7) Uiso 1 calc R . C11 C 0.2448(3) 0.9067(2) 0.1609(2) 0.0611(7) Uani 1 d . . H11 H 0.1956(3) 0.9135(2) 0.1092(2) 0.076(9) Uiso 1 calc R . C12 C 0.3963(3) 0.9640(2) 0.2044(2) 0.0690(8) Uani 1 d . . H12 H 0.4400(3) 0.9616(2) 0.2584(2) 0.078(9) Uiso 1 calc R . C13 C 0.5033(3) 1.0324(2) 0.1743(2) 0.0780(8) Uani 1 d . . H13A H 0.5356(3) 1.0952(2) 0.2180(2) 0.096(9) Uiso 1 calc R . H13B H 0.4332(3) 1.0392(2) 0.1239(2) 0.098(10) Uiso 1 calc R . C14 C 0.6709(3) 0.9974(2) 0.1535(2) 0.0585(7) Uani 1 d . . H14 H 0.7419(3) 0.9931(2) 0.2057(2) 0.059(7) Uiso 1 calc R . C15 C 0.7776(3) 1.0677(2) 0.1244(2) 0.0655(7) Uani 1 d . . C16 C 1.0607(5) 1.1202(3) 0.1050(3) 0.1013(11) Uani 1 d . . H16A H 1.1761(10) 1.1047(13) 0.1124(16) 0.207(21) Uiso 1 calc R . H16B H 1.0672(26) 1.1861(3) 0.1383(11) 0.149(17) Uiso 1 calc R . H16C H 1.0158(19) 1.1114(13) 0.0460(5) 0.178(20) Uiso 1 calc R . C17 C 0.6265(3) 0.8972(2) 0.08634(15) 0.0572(6) Uani 1 d . . H17A H 0.5340(3) 0.8964(2) 0.03969(15) 0.056(6) Uiso 1 calc R . H17B H 0.7297(3) 0.8844(2) 0.06391(15) 0.066(7) Uiso 1 calc R . O8 O -0.5412(2) 0.33562(12) 0.48685(10) 0.0651(5) Uani 1 d . . O9 O 0.1316(2) 0.26355(12) 0.61351(10) 0.0675(5) Uani 1 d . . O10 O -0.0479(2) 0.12057(11) 0.55155(10) 0.0640(5) Uani 1 d . . O11 O -0.1418(3) 0.1604(2) 0.33583(12) 0.1068(8) Uani 1 d . . O12 O 0.1202(2) 0.17501(13) 0.41518(10) 0.0716(5) Uani 1 d . . O13A O -0.3797(5) 0.6518(5) 0.7629(3) 0.125(3) Uani 0.583(9) d PG 1 O14A O -0.6527(6) 0.5804(5) 0.6898(5) 0.064(2) Uani 0.583(9) d PG 1 C32A C -0.4782(7) 0.5898(6) 0.7045(3) 0.063(3) Uani 0.583(9) d PG 1 O13B O -0.4620(10) 0.5639(7) 0.7794(3) 0.098(3) Uani 0.417(9) d PG 2 O14B O -0.6160(17) 0.6110(9) 0.6802(7) 0.082(3) Uani 0.417(9) d PG 2 C32B C -0.5046(18) 0.5600(10) 0.7068(3) 0.073(5) Uani 0.417(9) d PG 2 C18 C -0.4607(3) 0.3325(2) 0.5536(2) 0.0534(6) Uani 1 d . . C19 C -0.3618(3) 0.2514(2) 0.55723(15) 0.0539(6) Uani 1 d . . H19 H -0.2612(3) 0.2768(2) 0.60617(15) 0.045(6) Uiso 1 calc R . C20 C -0.4876(4) 0.1728(2) 0.5729(2) 0.0813(9) Uani 1 d . . H20A H -0.4291(4) 0.1204(2) 0.5756(2) 0.096(10) Uiso 1 calc R . H20B H -0.5906(4) 0.1498(2) 0.5273(2) 0.110(11) Uiso 1 calc R . H20C H -0.5213(4) 0.1994(2) 0.6257(2) 0.101(11) Uiso 1 calc R . C21 C -0.2918(3) 0.2120(2) 0.47717(15) 0.0590(7) Uani 1 d . . H21A H -0.3507(3) 0.2344(2) 0.43314(15) 0.067(7) Uiso 1 calc R . H21B H -0.3247(3) 0.1422(2) 0.45753(15) 0.065(7) Uiso 1 calc R . C22 C -0.0912(3) 0.23956(15) 0.48672(13) 0.0449(5) Uani 1 d . . C23 C 0.0115(3) 0.2117(2) 0.55850(15) 0.0480(6) Uani 1 d . . C24 C 0.0469(4) 0.0849(2) 0.6141(2) 0.0809(9) Uani 1 d . . H24A H -0.0253(12) 0.0285(10) 0.6163(10) 0.142(14) Uiso 1 calc R . H24B H 0.0751(26) 0.1339(6) 0.6690(3) 0.148(15) Uiso 1 calc R . H24C H 0.1536(15) 0.0689(15) 0.5984(8) 0.137(14) Uiso 1 calc R . C25 C -0.0445(3) 0.1862(2) 0.4037(2) 0.0551(6) Uani 1 d . . C26 C 0.1899(5) 0.1386(3) 0.3401(2) 0.0910(10) Uani 1 d . . H26A H 0.3052(14) 0.1260(17) 0.3568(2) 0.229(24) Uiso 1 calc R . H26B H 0.1972(29) 0.1857(7) 0.3115(9) 0.131(15) Uiso 1 calc R . H26C H 0.1135(18) 0.0800(9) 0.3025(7) 0.151(15) Uiso 1 calc R . C27 C -0.0258(3) 0.34792(15) 0.50020(14) 0.0500(6) Uani 1 d . . H27A H 0.1012(3) 0.35951(15) 0.50715(14) 0.057(7) Uiso 1 calc R . H27B H -0.0758(3) 0.36138(15) 0.44914(14) 0.048(6) Uiso 1 calc R . C28 C -0.0699(3) 0.4172(2) 0.57450(14) 0.0485(6) Uani 1 d . . H28 H -0.0207(3) 0.4170(2) 0.62867(14) 0.053(6) Uiso 1 calc R . C29 C -0.1743(3) 0.4787(2) 0.5680(2) 0.0508(6) Uani 1 d . . H29 H -0.2143(3) 0.4822(2) 0.5140(2) 0.051(6) Uiso 1 calc R . C30 C -0.2341(3) 0.5433(2) 0.6396(2) 0.0627(7) Uani 1 d . . H30A H -0.2148(3) 0.6087(2) 0.6377(2) 0.067(7) Uiso 1 calc R . H30B H -0.1652(3) 0.5437(2) 0.6934(2) 0.054(6) Uiso 1 calc R . C31 C -0.4293(3) 0.5097(2) 0.63444(15) 0.0598(7) Uani 1 d . . H31A H -0.4949(3) 0.5096(2) 0.57942(15) 0.060(7) Uiso 0.583(9) calc PR 1 H31B H -0.4988(3) 0.5125(2) 0.58135(15) 0.060(7) Uiso 0.417(9) calc PR 2 C33 C -0.7088(5) 0.6583(3) 0.7487(2) 0.1125(12) Uani 1 d . . H33A H -0.8350(5) 0.6485(3) 0.7358(2) 0.195(14) Uiso 0.583(9) calc PR 1 H33B H -0.6608(5) 0.7188(3) 0.7433(2) 0.195(14) Uiso 0.583(9) calc PR 1 H33C H -0.6674(5) 0.6590(3) 0.8059(2) 0.195(14) Uiso 0.583(9) calc PR 1 H33D H -0.7879(5) 0.6942(3) 0.7273(2) 0.195(14) Uiso 0.417(9) calc PR 2 H33E H -0.6230(5) 0.7011(3) 0.7975(2) 0.195(14) Uiso 0.417(9) calc PR 2 H33F H -0.7740(5) 0.6096(3) 0.7647(2) 0.195(14) Uiso 0.417(9) calc PR 2 C34 C -0.4660(3) 0.4064(2) 0.63659(15) 0.0609(7) Uani 1 d . . H34A H -0.3792(3) 0.4003(2) 0.68218(15) 0.066(7) Uiso 1 calc R . H34B H -0.5811(3) 0.3934(2) 0.64888(15) 0.090(9) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0596(11) 0.0803(12) 0.0603(11) 0.0221(10) -0.0030(9) 0.0209(9) O2 0.0601(11) 0.0699(11) 0.0591(11) 0.0246(9) 0.0064(8) 0.0254(9) O3 0.0718(12) 0.0675(12) 0.0558(11) 0.0065(9) 0.0042(9) 0.0252(9) O4 0.0698(13) 0.173(2) 0.0858(14) 0.085(2) 0.0109(11) 0.0317(13) O5 0.0544(11) 0.0894(13) 0.0646(11) 0.0396(10) 0.0099(9) 0.0114(9) O6 0.0817(15) 0.111(2) 0.153(2) 0.078(2) 0.0050(14) 0.0322(13) O7 0.0537(11) 0.0894(13) 0.0984(14) 0.0502(11) 0.0140(10) 0.0206(10) C1 0.0447(14) 0.061(2) 0.0490(14) 0.0110(12) 0.0087(12) 0.0253(12) C2 0.0452(13) 0.0598(15) 0.0484(14) 0.0134(12) 0.0071(11) 0.0206(12) C3 0.066(2) 0.074(2) 0.062(2) 0.002(2) 0.018(2) 0.017(2) C4 0.0476(14) 0.069(2) 0.059(2) 0.0216(14) 0.0080(13) 0.0217(12) C5 0.0459(13) 0.062(2) 0.0445(13) 0.0165(12) 0.0087(11) 0.0186(12) C6 0.0428(14) 0.058(2) 0.0491(14) 0.0162(13) 0.0147(11) 0.0130(12) C7 0.108(3) 0.096(3) 0.051(2) -0.005(2) -0.008(2) 0.021(2) C8 0.054(2) 0.077(2) 0.0496(15) 0.0210(14) 0.0111(13) 0.0249(14) C9 0.074(2) 0.091(2) 0.070(2) 0.036(2) 0.021(2) 0.002(2) C10 0.050(2) 0.079(2) 0.050(2) 0.0053(14) 0.0078(13) 0.0201(14) C11 0.052(2) 0.057(2) 0.064(2) 0.0030(14) 0.0097(14) 0.0212(13) C12 0.057(2) 0.068(2) 0.066(2) -0.0067(15) 0.0144(15) 0.0217(15) C13 0.057(2) 0.057(2) 0.099(2) -0.002(2) 0.012(2) 0.0136(14) C14 0.0466(14) 0.059(2) 0.059(2) 0.0091(13) 0.0008(12) 0.0117(12) C15 0.056(2) 0.066(2) 0.068(2) 0.0194(15) -0.0030(14) 0.0158(14) C16 0.077(2) 0.114(3) 0.139(3) 0.077(3) 0.033(2) 0.012(2) C17 0.0486(15) 0.064(2) 0.0550(15) 0.0135(13) 0.0055(13) 0.0184(12) O8 0.0542(10) 0.0768(12) 0.0585(11) 0.0242(9) -0.0050(9) 0.0109(9) O9 0.0621(11) 0.0632(11) 0.0627(11) 0.0143(9) -0.0107(9) 0.0096(9) O10 0.0751(12) 0.0518(11) 0.0646(11) 0.0236(9) 0.0093(9) 0.0081(9) O11 0.0903(15) 0.151(2) 0.0499(12) -0.0094(12) -0.0072(11) 0.0505(14) O12 0.0532(11) 0.0988(14) 0.0510(10) 0.0049(9) 0.0154(9) 0.0138(10) O13A 0.071(3) 0.148(6) 0.093(3) -0.042(4) -0.008(3) 0.033(3) O14A 0.045(2) 0.072(4) 0.073(4) 0.018(2) 0.018(2) 0.013(2) C32A 0.056(6) 0.088(6) 0.046(5) 0.015(4) 0.006(4) 0.037(5) O13B 0.105(5) 0.144(7) 0.045(3) 0.017(3) 0.009(3) 0.071(5) O14B 0.115(9) 0.085(7) 0.080(4) 0.048(4) 0.048(5) 0.061(5) C32B 0.055(8) 0.069(6) 0.076(11) 0.008(5) -0.011(6) 0.018(4) C18 0.0318(12) 0.070(2) 0.058(2) 0.0273(14) 0.0051(12) 0.0018(12) C19 0.0349(13) 0.068(2) 0.059(2) 0.0268(13) 0.0043(12) 0.0057(12) C20 0.068(2) 0.086(2) 0.107(3) 0.053(2) 0.027(2) 0.014(2) C21 0.0475(15) 0.059(2) 0.061(2) 0.0142(13) -0.0002(12) 0.0045(12) C22 0.0414(13) 0.0438(13) 0.0438(13) 0.0101(11) 0.0043(10) 0.0054(10) C23 0.0475(14) 0.0470(15) 0.0491(14) 0.0112(12) 0.0146(12) 0.0133(12) C24 0.112(3) 0.077(2) 0.076(2) 0.044(2) 0.030(2) 0.037(2) C25 0.056(2) 0.0528(15) 0.048(2) 0.0078(12) 0.0035(13) 0.0109(12) C26 0.084(2) 0.116(3) 0.061(2) 0.002(2) 0.034(2) 0.018(2) C27 0.0478(15) 0.0513(14) 0.0504(14) 0.0175(12) 0.0087(11) 0.0082(11) C28 0.0467(14) 0.0473(14) 0.0475(15) 0.0146(11) 0.0047(11) 0.0045(11) C29 0.0503(14) 0.0489(14) 0.055(2) 0.0225(12) 0.0101(12) 0.0058(12) C30 0.067(2) 0.054(2) 0.067(2) 0.0185(14) 0.0128(14) 0.0186(13) C31 0.056(2) 0.079(2) 0.0474(15) 0.0196(13) 0.0075(12) 0.0322(14) C33 0.126(3) 0.128(3) 0.099(2) 0.025(2) 0.043(2) 0.084(2) C34 0.0450(15) 0.088(2) 0.056(2) 0.0309(15) 0.0125(12) 0.0176(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.213(2) . no O2 C6 1.196(2) . no O3 C6 1.334(3) . no O3 C7 1.449(3) . no O4 C8 1.192(3) . no O5 C8 1.321(3) . no O5 C9 1.444(3) . no O6 C15 1.202(3) . no O7 C15 1.327(3) . no O7 C16 1.449(3) . no C1 C2 1.517(3) . no C1 C17 1.507(3) . no C2 C3 1.533(3) . no C2 C4 1.533(3) . no C2 H2 0.98 . no C3 H3A 0.96 . no C3 H3B 0.96 . no C3 H3C 0.96 . no C4 C5 1.545(3) . no C4 H4A 0.97 . no C4 H4B 0.97 . no C5 C6 1.522(3) . no C5 C8 1.527(3) . no C5 C10 1.549(3) . no C7 H7A 0.96 . no C7 H7B 0.96 . no C7 H7C 0.96 . no C9 H9A 0.96 . no C9 H9B 0.96 . no C9 H9C 0.96 . no C10 C11 1.488(3) . no C10 H10A 0.97 . no C10 H10B 0.97 . no C11 C12 1.319(3) . no C11 H11 0.93 . no C12 C13 1.488(4) . no C12 H12 0.93 . no C13 C14 1.535(3) . no C13 H13A 0.97 . no C13 H13B 0.97 . no C14 C15 1.498(3) . no C14 C17 1.529(3) . no C14 H14 0.98 . no C16 H16A 0.96 . no C16 H16B 0.96 . no C16 H16C 0.96 . no C17 H17A 0.97 . no C17 H17B 0.97 . no O8 C18 1.210(2) . no O9 C23 1.194(2) . no O10 C23 1.331(3) . no O10 C24 1.451(3) . no O11 C25 1.184(3) . no O12 C25 1.315(3) . no O12 C26 1.452(3) . no O13A C32A 1.19 . no O14A C32A 1.33 . no O14A C33 1.456(10) . no C32A C31 1.549(5) . no O13B C32B 1.19 . no O14B C32B 1.33 . no O14B C33 1.519(14) . no C32B C31 1.491(7) . no C18 C19 1.521(3) . no C18 C34 1.512(3) . no C19 C20 1.540(3) . no C19 C21 1.531(3) . no C19 H19 0.98 . no C20 H20A 0.96 . no C20 H20B 0.96 . no C20 H20C 0.96 . no C21 C22 1.543(3) . no C21 H21A 0.97 . no C21 H21B 0.97 . no C22 C25 1.524(3) . no C22 C23 1.527(3) . no C22 C27 1.554(3) . no C24 H24A 0.96 . no C24 H24B 0.96 . no C24 H24C 0.96 . no C26 H26A 0.96 . no C26 H26B 0.96 . no C26 H26C 0.96 . no C27 C28 1.493(3) . no C27 H27A 0.97 . no C27 H27B 0.97 . no C28 C29 1.318(3) . no C28 H28 0.93 . no C29 C30 1.493(3) . no C29 H29 0.93 . no C30 C31 1.528(3) . no C30 H30A 0.97 . no C30 H30B 0.97 . no C31 C34 1.530(3) . no C31 H31A 0.98 . no C31 H31B 0.98 . no C33 H33A 0.96 . no C33 H33B 0.96 . no C33 H33C 0.96 . no C33 H33D 0.96 . no C33 H33E 0.96 . no C33 H33F 0.96 . no C34 H34A 0.97 . no C34 H34B 0.97 . no loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_contact_distance_HA _geom_angle_DHA _geom_contact_site_symmetry_A _geom_contact_publ_flag C7 H7A O4 2.627(4) 172.6(11) 2_565 no C9 H9B O9 2.396(9) 156.7(18) 2_566 no C16 H16C O2 2.507(10) 125.3(8) 2_675 no C17 H17A O6 2.692(3) 173.6(2) 2_675 no C17 H17B O2 2.522(3) 146.0(2) 1_655 no C19 H19 O4 2.642(3) 154.5(2) 2_566 no C34 H34A O4 2.601(3) 164.0(2) 2_566 no C34 H34B O9 2.620(3) 144.7(2) 1_455 no _eof