#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/7/7051236.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_7051236 _journal_name_full 'New Journal of Chemistry' _journal_year 2000 _space_group_IT_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _[local]_cod_cif_authors_sg_H-M 'C c' loop_ _publ_author_name 'Kiviniemi, Sari ' 'Nissinen Maija ' 'Lms, Markku ' 'Rissanen, Kari ' 'Pursiainen Jouni' _chemical_melting_point '213-216' _chemical_formula_moiety 'C20 H24 O6, (C3 H4 N S)+ (Cl O4)-' _chemical_formula_sum 'C23 H28 Cl N O10 S' _chemical_formula_weight 545.97 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.840(1) _cell_length_b 14.251(1) _cell_length_c 12.3267(6) _cell_angle_alpha 90.00 _cell_angle_beta 129.535(3) _cell_angle_gamma 90.00 _cell_volume 2417.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(2) _exptl_crystal_density_diffrn 1.500 _diffrn_ambient_temperature 173.0(2) 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.50227(7) -0.02302(9) -0.45342(11) 0.0366(3) Uani 1 1 d . . . C2 C -0.5113(3) -0.7770(3) -0.2023(5) 0.0310(10) Uani 1 1 d . . . H2A H -0.4933 -0.8413 -0.1630 0.037 Uiso 1 1 calc R . . H2B H -0.5335 -0.7792 -0.2992 0.037 Uiso 1 1 calc R . . C3 C -0.5904(3) -0.7396(4) -0.2039(5) 0.0341(10) Uani 1 1 d . . . H3A H -0.6452 -0.7846 -0.2520 0.041 Uiso 1 1 calc R . . H3B H -0.5656 -0.7311 -0.1063 0.041 Uiso 1 1 calc R . . C5 C -0.7112(3) -0.6207(3) -0.3085(5) 0.0319(10) Uani 1 1 d . . . H5A H -0.6994 -0.6032 -0.2210 0.038 Uiso 1 1 calc R . . H5B H -0.7599 -0.6718 -0.3549 0.038 Uiso 1 1 calc R . . C6 C -0.7479(3) -0.5384(3) -0.4036(5) 0.0316(10) Uani 1 1 d . . . H6A H -0.7517 -0.5536 -0.4853 0.038 Uiso 1 1 calc R . . H6B H -0.8139 -0.5216 -0.4388 0.038 Uiso 1 1 calc R . . C8 C -0.6946(3) -0.3839(3) -0.4054(4) 0.0254(9) Uani 1 1 d . . . C9 C -0.7720(3) -0.3728(3) -0.5469(4) 0.0305(10) Uani 1 1 d . . . H9 H -0.8225 -0.4182 -0.5965 0.037 Uiso 1 1 calc R . . C10 C -0.7745(3) -0.2930(4) -0.6159(5) 0.0333(10) Uani 1 1 d . . . H10 H -0.8265 -0.2852 -0.7137 0.040 Uiso 1 1 calc R . . C11 C -0.7034(3) -0.2262(3) -0.5446(5) 0.0333(10) Uani 1 1 d . . . H11 H -0.7069 -0.1720 -0.5925 0.040 Uiso 1 1 calc R . . C12 C -0.6254(3) -0.2378(4) -0.4012(5) 0.0320(10) Uani 1 1 d . . . H12 H -0.5753 -0.1920 -0.3522 0.038 Uiso 1 1 calc R . . C13 C -0.6211(3) -0.3153(3) -0.3313(4) 0.0280(9) Uani 1 1 d . . . C15 C -0.4637(3) -0.2745(3) -0.1173(5) 0.0315(10) Uani 1 1 d . . . H15A H -0.4799 -0.2134 -0.0985 0.038 Uiso 1 1 calc R . . H15B H -0.4445 -0.2629 -0.1759 0.038 Uiso 1 1 calc R . . C16 C -0.3816(3) -0.3192(3) 0.0182(5) 0.0315(10) Uani 1 1 d . . . H16A H -0.3262 -0.2750 0.0737 0.038 Uiso 1 1 calc R . . H16B H -0.4022 -0.3350 0.0739 0.038 Uiso 1 1 calc R . . C18 C -0.2635(3) -0.4389(3) 0.1128(4) 0.0304(10) Uani 1 1 d . . . H18A H -0.2743 -0.4665 0.1756 0.036 Uiso 1 1 calc R . . H18B H -0.2150 -0.3880 0.1643 0.036 Uiso 1 1 calc R . . C19 C -0.2272(3) -0.5126(3) 0.0699(5) 0.0307(10) Uani 1 1 d . . . H19A H -0.2225 -0.4868 -0.0002 0.037 Uiso 1 1 calc R . . H19B H -0.1619 -0.5342 0.1526 0.037 Uiso 1 1 calc R . . C21 C -0.2821(3) -0.6596(3) -0.0525(4) 0.0288(10) Uani 1 1 d . . . C22 C -0.2048(3) -0.6656(3) -0.0533(4) 0.0296(10) Uani 1 1 d . . . H22 H -0.1559 -0.6185 -0.0088 0.036 Uiso 1 1 calc R . . C23 C -0.1993(3) -0.7416(4) -0.1200(5) 0.0358(11) Uani 1 1 d . . . H23 H -0.1463 -0.7462 -0.1203 0.043 Uiso 1 1 calc R . . C24 C -0.2699(3) -0.8092(4) -0.1847(5) 0.0364(11) Uani 1 1 d . . . H24 H -0.2652 -0.8607 -0.2289 0.044 Uiso 1 1 calc R . . C25 C -0.3481(3) -0.8032(3) -0.1863(4) 0.0314(10) Uani 1 1 d . . . H25 H -0.3973 -0.8500 -0.2327 0.038 Uiso 1 1 calc R . . C26 C -0.3543(3) -0.7289(3) -0.1200(4) 0.0241(9) Uani 1 1 d . . . C28 C -0.4655(3) -0.5544(4) 0.0360(5) 0.0369(11) Uani 1 1 d . . . H28 H -0.4481 -0.5873 -0.0120 0.044 Uiso 1 1 calc R A 1 C30 C -0.5489(3) -0.4500(4) 0.0597(4) 0.0330(10) Uani 1 1 d . . . H30 H -0.5956 -0.4020 0.0288 0.040 Uiso 1 1 calc R B 1 O1 O -0.4288(2) -0.7149(2) -0.1160(3) 0.0323(7) Uani 1 1 d . . . O4 O -0.6229(2) -0.6516(2) -0.2762(3) 0.0306(7) Uani 1 1 d . . . O7 O -0.6822(2) -0.4603(2) -0.3261(3) 0.0288(7) Uani 1 1 d . . . O14 O -0.54697(19) -0.3352(2) -0.1909(3) 0.0275(7) Uani 1 1 d . . . O17 O -0.3526(2) -0.4023(2) -0.0110(3) 0.0296(7) Uani 1 1 d . . . O20 O -0.2950(2) -0.5894(2) 0.0100(3) 0.0299(7) Uani 1 1 d . . . O101 O -0.5028(3) -0.0059(3) -0.3396(4) 0.0592(11) Uani 1 1 d . . . O102 O -0.4420(3) -0.1028(3) -0.4215(4) 0.0630(12) Uani 1 1 d . . . O103 O -0.5992(3) -0.0431(3) -0.5781(4) 0.0611(11) Uani 1 1 d . . . O104 O -0.4635(4) 0.0565(3) -0.4730(5) 0.0742(14) Uani 1 1 d . . . N29 N -0.5349(3) -0.4894(3) -0.0261(4) 0.0346(9) Uani 1 1 d . C . H29 H -0.5687 -0.4735 -0.1150 0.041 Uiso 1 1 calc R . . S27 S -0.41537(13) -0.57226(15) 0.19316(17) 0.0406(6) Uani 0.561(6) 1 d P C 1 C31 C -0.48295(14) -0.48887(16) 0.2128(2) 0.0359(7) Uani 0.561(6) 1 d P C 1 H31 H -0.4793 -0.4738 0.2912 0.043 Uiso 0.561(6) 1 calc PR C 1 S27B S -0.48295(14) -0.48887(16) 0.2128(2) 0.0359(7) Uani 0.439(6) 1 d P C 2 C31B C -0.41537(13) -0.57226(15) 0.19316(17) 0.0406(6) Uani 0.439(6) 1 d P C 2 H31B H -0.3646 -0.6142 0.2592 0.049 Uiso 0.439(6) 1 calc PR C 2 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 Cl1 0.0339(6) 0.0405(7) 0.0374(6) -0.0019(5) 0.0236(5) -0.0013(5) C2 0.033(2) 0.025(3) 0.033(2) -0.0023(18) 0.021(2) -0.0051(19) C3 0.035(2) 0.036(3) 0.038(2) 0.002(2) 0.027(2) -0.004(2) C5 0.031(2) 0.032(3) 0.037(2) -0.006(2) 0.024(2) -0.007(2) C6 0.024(2) 0.029(3) 0.036(2) -0.0043(19) 0.017(2) -0.0063(19) C8 0.024(2) 0.029(3) 0.0264(19) 0.0008(17) 0.0170(17) 0.0030(18) C9 0.032(2) 0.034(3) 0.030(2) -0.0048(18) 0.0214(19) 0.0008(19) C10 0.036(2) 0.042(3) 0.027(2) 0.007(2) 0.0223(19) 0.012(2) C11 0.036(2) 0.034(3) 0.039(2) 0.007(2) 0.027(2) 0.012(2) C12 0.032(2) 0.036(3) 0.036(2) 0.001(2) 0.026(2) 0.002(2) C13 0.027(2) 0.033(3) 0.026(2) 0.0028(18) 0.0183(18) 0.0063(19) C15 0.029(2) 0.031(3) 0.037(2) -0.005(2) 0.023(2) -0.002(2) C16 0.031(2) 0.031(3) 0.030(2) -0.0086(19) 0.0183(19) -0.007(2) C18 0.026(2) 0.038(3) 0.023(2) -0.0026(19) 0.0137(19) -0.0025(19) C19 0.022(2) 0.036(3) 0.032(2) -0.007(2) 0.0164(19) -0.005(2) C21 0.033(2) 0.036(3) 0.0234(19) 0.0024(18) 0.0204(19) 0.005(2) C22 0.030(2) 0.032(3) 0.028(2) 0.0059(18) 0.0191(19) 0.0052(19) C23 0.039(3) 0.045(3) 0.032(2) 0.010(2) 0.027(2) 0.015(2) C24 0.043(3) 0.040(3) 0.030(2) 0.006(2) 0.025(2) 0.013(2) C25 0.037(2) 0.030(3) 0.026(2) 0.0055(18) 0.020(2) 0.008(2) C26 0.025(2) 0.029(2) 0.0200(18) 0.0036(17) 0.0153(17) 0.0054(18) C28 0.040(3) 0.034(3) 0.045(3) -0.004(2) 0.030(2) -0.006(2) C30 0.035(2) 0.033(3) 0.034(2) 0.000(2) 0.023(2) 0.002(2) O1 0.0307(16) 0.037(2) 0.0316(15) -0.0068(13) 0.0209(14) -0.0052(14) O4 0.0286(15) 0.0325(19) 0.0371(16) 0.0036(14) 0.0239(14) 0.0007(13) O7 0.0293(16) 0.0304(18) 0.0235(14) -0.0015(12) 0.0153(13) -0.0037(13) O14 0.0223(14) 0.0336(19) 0.0225(14) -0.0037(12) 0.0124(12) -0.0048(13) O17 0.0263(15) 0.0350(19) 0.0222(13) -0.0034(13) 0.0130(12) 0.0017(14) O20 0.0290(15) 0.0333(19) 0.0311(15) -0.0067(14) 0.0208(13) -0.0048(14) O101 0.063(2) 0.083(3) 0.050(2) -0.016(2) 0.045(2) -0.005(2) O102 0.056(2) 0.065(3) 0.058(2) 0.009(2) 0.032(2) 0.029(2) O103 0.036(2) 0.082(3) 0.040(2) -0.008(2) 0.0125(17) -0.002(2) O104 0.105(4) 0.057(3) 0.092(3) -0.016(2) 0.078(3) -0.037(3) N29 0.035(2) 0.041(2) 0.0245(18) 0.0055(17) 0.0175(17) 0.0042(19) S27 0.0402(11) 0.0506(13) 0.0342(10) 0.0066(8) 0.0252(9) 0.0042(9) C31 0.0331(12) 0.0395(14) 0.0335(11) 0.0033(9) 0.0204(9) 0.0011(9) S27B 0.0331(12) 0.0395(14) 0.0335(11) 0.0033(9) 0.0204(9) 0.0011(9) C31B 0.0402(11) 0.0506(13) 0.0342(10) 0.0066(8) 0.0252(9) 0.0042(9) 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 Cl1 O104 1.426(4) . ? Cl1 O101 1.429(3) . ? Cl1 O103 1.432(4) . ? Cl1 O102 1.437(4) . ? C2 O1 1.445(5) . ? C2 C3 1.497(6) . ? C3 O4 1.430(6) . ? C5 O4 1.426(5) . ? C5 C6 1.484(7) . ? C6 O7 1.449(5) . ? C8 C9 1.381(6) . ? C8 O7 1.384(5) . ? C8 C13 1.409(6) . ? C9 C10 1.404(7) . ? C10 C11 1.367(7) . ? C11 C12 1.399(6) . ? C12 C13 1.373(6) . ? C13 O14 1.382(5) . ? C15 O14 1.437(5) . ? C15 C16 1.492(7) . ? C16 O17 1.427(5) . ? C18 O17 1.428(5) . ? C18 C19 1.496(6) . ? C19 O20 1.439(5) . ? C21 O20 1.368(5) . ? C21 C22 1.387(6) . ? C21 C26 1.401(6) . ? C22 C23 1.400(7) . ? C23 C24 1.368(7) . ? C24 C25 1.387(6) . ? C25 C26 1.384(6) . ? C26 O1 1.375(5) . ? C28 N29 1.330(6) . ? C28 S27 1.553(5) . ? C30 N29 1.354(6) . ? C30 C31 1.558(5) . ? S27 C31 1.816(3) . ?