# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zunting Zhang' _publ_contact_author_email zhangzt@snnu.edu.cn loop_ _publ_author_name 'Zunting Zhang' 'Qiu-Ya Wang' 'Wu-Wu Li' 'Qing-Hua Meng' 'Xue-Ling Zhang' # Attachment '- 3 cif.txt' data_041117t _database_code_depnum_ccdc_archive 'CCDC 865946' #TrackingRef '- 3 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 Ba O25 S2' _chemical_formula_weight 1054.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.879(14) _cell_length_b 13.43(2) _cell_length_c 20.78(4) _cell_angle_alpha 75.33(3) _cell_angle_beta 83.25(2) _cell_angle_gamma 87.71(3) _cell_volume 2112(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6112 _exptl_absorpt_correction_T_max 0.9349 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10422 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.1289 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7067 _reflns_number_gt 4375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7067 _refine_ls_number_parameters 614 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1815 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ba1 Ba 0.73333(8) 0.40400(4) 0.99872(3) 0.0468(2) Uani 1 1 d . . . S1 S -0.1936(3) 0.78034(18) 0.81481(10) 0.0505(6) Uani 1 1 d . . . S2 S 0.3049(3) 0.34979(18) 0.83328(10) 0.0465(6) Uani 1 1 d . . . O1 O 0.3488(7) 0.8635(4) 0.5429(3) 0.0433(14) Uani 1 1 d . . . O2 O -0.1137(6) 0.8877(4) 0.4702(3) 0.0379(13) Uani 1 1 d . . . O3 O 0.0438(7) 0.9498(4) 0.3510(2) 0.0353(12) Uani 1 1 d . . . H3 H -0.0367 0.9315 0.3800 0.053 Uiso 1 1 calc R . . O4 O 0.6447(7) 0.9930(4) 0.3351(3) 0.0465(15) Uani 1 1 d . . . O5 O -0.4934(8) 0.7040(5) 0.7697(3) 0.0539(16) Uani 1 1 d . . . O6 O -0.3360(11) 0.8444(6) 0.8340(4) 0.093(3) Uani 1 1 d . . . O7 O -0.2095(8) 0.6747(5) 0.8557(3) 0.0621(18) Uani 1 1 d . . . O8 O -0.0274(10) 0.8208(6) 0.8121(3) 0.075(2) Uani 1 1 d . . . O9 O 0.8707(7) 0.3302(4) 0.5743(3) 0.0422(14) Uani 1 1 d . . . O10 O 0.4009(7) 0.3730(4) 0.5063(3) 0.0433(14) Uani 1 1 d . . . O11 O 0.5509(7) 0.4467(4) 0.3873(3) 0.0435(14) Uani 1 1 d . . . H11 H 0.4716 0.4271 0.4166 0.065 Uiso 1 1 calc R . . O12 O 1.1562(7) 0.4654(4) 0.3645(3) 0.0490(15) Uani 1 1 d . . . O13 O 0.0246(8) 0.2363(5) 0.8072(3) 0.0534(16) Uani 1 1 d . . . O14 O 0.1617(8) 0.4200(5) 0.8369(3) 0.067(2) Uani 1 1 d . . . O15 O 0.2871(11) 0.2633(6) 0.8899(3) 0.076(2) Uani 1 1 d . . . O16 O 0.4672(8) 0.3999(5) 0.8235(3) 0.0586(18) Uani 1 1 d . . . C1 C 0.2029(10) 0.8369(6) 0.5833(4) 0.0384(19) Uani 1 1 d . . . H1 H 0.2136 0.8107 0.6286 0.046 Uiso 1 1 calc R . . C2 C 0.0441(10) 0.8439(5) 0.5657(4) 0.0286(17) Uani 1 1 d . . . C3 C 0.0275(9) 0.8803(5) 0.4934(3) 0.0230(16) Uani 1 1 d . . . C4 C 0.1832(9) 0.9059(5) 0.4502(4) 0.0257(16) Uani 1 1 d . . . C5 C 0.1888(9) 0.9423(5) 0.3797(4) 0.0252(16) Uani 1 1 d . . . C6 C 0.3412(10) 0.9700(5) 0.3403(4) 0.0327(18) Uani 1 1 d . . . H6 H 0.3427 0.9931 0.2942 0.039 Uiso 1 1 calc R . . C7 C 0.4932(10) 0.9636(5) 0.3696(4) 0.0336(19) Uani 1 1 d . . . C8 C 0.4933(10) 0.9276(6) 0.4378(4) 0.0383(19) Uani 1 1 d . . . H8 H 0.5948 0.9225 0.4572 0.046 Uiso 1 1 calc R . . C9 C 0.3420(10) 0.8993(5) 0.4763(4) 0.0297(17) Uani 1 1 d . . . C10 C -0.1030(9) 0.8122(5) 0.6167(4) 0.0271(17) Uani 1 1 d . . . C11 C -0.0907(10) 0.8118(5) 0.6824(4) 0.0310(17) Uani 1 1 d . . . H11A H 0.0082 0.8367 0.6929 0.037 Uiso 1 1 calc R . . C12 C -0.2182(10) 0.7761(5) 0.7327(4) 0.0328(18) Uani 1 1 d . . . C13 C -0.3719(10) 0.7397(6) 0.7180(4) 0.040(2) Uani 1 1 d . . . C14 C -0.3849(10) 0.7449(6) 0.6518(4) 0.0374(19) Uani 1 1 d . . . H14 H -0.4865 0.7252 0.6400 0.045 Uiso 1 1 calc R . . C15 C -0.2549(10) 0.7776(6) 0.6030(4) 0.0372(19) Uani 1 1 d . . . H15 H -0.2680 0.7768 0.5593 0.045 Uiso 1 1 calc R . . C16 C 0.6622(12) 1.0203(8) 0.2648(5) 0.065(3) Uani 1 1 d . . . H16A H 0.7785 1.0390 0.2483 0.098 Uiso 1 1 calc R . . H16B H 0.5881 1.0777 0.2493 0.098 Uiso 1 1 calc R . . H16C H 0.6321 0.9629 0.2489 0.098 Uiso 1 1 calc R . . C17 C -0.6472(12) 0.6621(9) 0.7554(5) 0.074(3) Uani 1 1 d . . . H17A H -0.7211 0.6384 0.7962 0.111 Uiso 1 1 calc R . . H17B H -0.6175 0.6056 0.7356 0.111 Uiso 1 1 calc R . . H17C H -0.7049 0.7146 0.7249 0.111 Uiso 1 1 calc R . . C18 C 0.7228(10) 0.3088(6) 0.6152(4) 0.0364(19) Uani 1 1 d . . . H18 H 0.7331 0.2812 0.6604 0.044 Uiso 1 1 calc R . . C19 C 0.5649(10) 0.3226(5) 0.5981(4) 0.0297(17) Uani 1 1 d . . . C20 C 0.5412(10) 0.3605(5) 0.5266(4) 0.0313(18) Uani 1 1 d . . . C21 C 0.6974(9) 0.3852(5) 0.4840(4) 0.0294(17) Uani 1 1 d . . . C22 C 0.6978(10) 0.4296(5) 0.4140(4) 0.0315(18) Uani 1 1 d . . . C23 C 0.8478(10) 0.4565(6) 0.3736(4) 0.0344(18) Uani 1 1 d . . . H23 H 0.8462 0.4856 0.3280 0.041 Uiso 1 1 calc R . . C24 C 1.0045(11) 0.4398(6) 0.4014(4) 0.040(2) Uani 1 1 d . . . C25 C 1.0094(9) 0.3964(6) 0.4688(4) 0.0346(19) Uani 1 1 d . . . H25 H 1.1128 0.3842 0.4870 0.042 Uiso 1 1 calc R . . C26 C 0.8603(10) 0.3722(5) 0.5073(4) 0.0312(18) Uani 1 1 d . . . C27 C 0.4154(10) 0.3012(5) 0.6498(4) 0.0311(18) Uani 1 1 d . . . C28 C 0.4228(10) 0.3276(6) 0.7099(4) 0.0322(18) Uani 1 1 d . . . H28 H 0.5196 0.3606 0.7156 0.039 Uiso 1 1 calc R . . C29 C 0.2928(10) 0.3068(6) 0.7611(4) 0.0338(18) Uani 1 1 d . . . C30 C 0.1478(10) 0.2563(6) 0.7545(4) 0.0339(18) Uani 1 1 d . . . C31 C 0.1388(11) 0.2300(6) 0.6942(4) 0.040(2) Uani 1 1 d . . . H31 H 0.0427 0.1967 0.6883 0.047 Uiso 1 1 calc R . . C32 C 0.2706(10) 0.2528(6) 0.6434(4) 0.0348(19) Uani 1 1 d . . . H32 H 0.2611 0.2350 0.6035 0.042 Uiso 1 1 calc R . . C33 C 1.1635(12) 0.4974(7) 0.2946(5) 0.058(3) Uani 1 1 d . . . H33A H 1.2796 0.5125 0.2758 0.086 Uiso 1 1 calc R . . H33B H 1.0940 0.5581 0.2822 0.086 Uiso 1 1 calc R . . H33C H 1.1219 0.4436 0.2779 0.086 Uiso 1 1 calc R . . C34 C -0.1153(16) 0.1690(10) 0.8060(6) 0.088(4) Uani 1 1 d . . . H34A H -0.1916 0.1609 0.8465 0.132 Uiso 1 1 calc R . . H34B H -0.0700 0.1029 0.8024 0.132 Uiso 1 1 calc R . . H34C H -0.1763 0.1989 0.7682 0.132 Uiso 1 1 calc R . . O17 O 1.0323(10) 0.5391(5) 0.9211(3) 0.0570(17) Uani 1 1 d D . . H17D H 0.985(14) 0.591(6) 0.897(5) 0.086 Uiso 1 1 d D . . H17E H 1.116(11) 0.582(8) 0.908(6) 0.086 Uiso 1 1 d D . . O18 O 0.8016(11) 0.3923(9) 0.8686(5) 0.098(3) Uani 1 1 d D . . H18A H 0.895(12) 0.411(12) 0.844(7) 0.147 Uiso 1 1 d D . . H18B H 0.727(15) 0.369(12) 0.850(8) 0.147 Uiso 1 1 d D . . O19 O 0.5878(18) 0.2286(10) 0.9672(8) 0.170(5) Uani 1 1 d . . . O20 O 0.5146(8) 0.5367(4) 0.9043(3) 0.0445(14) Uani 1 1 d D . . H20A H 0.499(14) 0.509(7) 0.873(4) 0.067 Uiso 1 1 d D . . O21 O 0.6683(11) 0.6212(6) 0.9930(4) 0.078(2) Uani 1 1 d D . . H21A H 0.677(18) 0.657(9) 1.021(5) 0.117 Uiso 1 1 d D . . H21B H 0.732(15) 0.660(8) 0.961(4) 0.117 Uiso 1 1 d D . . O22 O 0.6946(15) 0.2414(7) 1.1096(5) 0.113(4) Uani 1 1 d D . . H22A H 0.798(9) 0.262(15) 1.107(10) 0.169 Uiso 1 1 d D . . H22B H 0.63(2) 0.193(11) 1.108(10) 0.169 Uiso 1 1 d D . . O23 O 1.0054(11) 0.2689(6) 0.9914(4) 0.076(2) Uani 1 1 d D . . H23A H 1.060(16) 0.278(10) 0.952(3) 0.115 Uiso 1 1 d D . . H23B H 1.007(18) 0.217(6) 1.024(4) 0.115 Uiso 1 1 d D . . O25 O 0.264(3) 0.0477(11) 0.9040(10) 0.111(6) Uani 0.50 1 d P . . O25' O 0.752(4) 0.042(4) 0.979(2) 0.34(3) Uani 0.50 1 d P . . H20B H 0.597(8) 0.545(7) 0.874(4) 0.05(3) Uiso 1 1 d D . . O24' O -0.425(3) 0.9527(17) 0.9267(11) 0.138(8) Uani 0.50 1 d P . . O24 O -0.004(3) 0.9212(10) 0.9151(8) 0.113(8) Uani 0.50 1 d P . . 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 Ba1 0.0520(4) 0.0543(3) 0.0301(3) -0.0088(2) 0.0022(2) 0.0167(3) S1 0.0572(17) 0.0599(14) 0.0273(11) -0.0026(10) 0.0041(11) 0.0042(12) S2 0.0442(14) 0.0654(15) 0.0332(12) -0.0215(11) 0.0034(10) -0.0043(11) O1 0.022(3) 0.068(4) 0.036(3) -0.006(3) -0.002(3) 0.004(3) O2 0.017(3) 0.061(3) 0.032(3) -0.003(3) -0.005(2) 0.000(3) O3 0.026(3) 0.051(3) 0.029(3) -0.007(2) -0.007(2) -0.001(2) O4 0.025(3) 0.061(4) 0.048(4) -0.008(3) 0.009(3) -0.006(3) O5 0.034(4) 0.074(4) 0.039(3) 0.007(3) 0.013(3) -0.007(3) O6 0.110(7) 0.114(6) 0.054(5) -0.033(4) 0.003(4) 0.045(5) O7 0.051(4) 0.079(4) 0.041(4) 0.013(3) -0.001(3) -0.011(3) O8 0.086(6) 0.097(5) 0.039(4) -0.010(4) -0.002(4) -0.029(5) O9 0.024(3) 0.065(4) 0.042(3) -0.017(3) -0.015(3) 0.007(3) O10 0.011(3) 0.074(4) 0.044(3) -0.013(3) -0.006(3) 0.003(3) O11 0.021(3) 0.065(4) 0.039(3) -0.004(3) -0.005(3) -0.002(3) O12 0.024(3) 0.061(4) 0.057(4) -0.014(3) 0.012(3) -0.005(3) O13 0.038(4) 0.075(4) 0.047(4) -0.019(3) 0.010(3) -0.011(3) O14 0.048(4) 0.089(5) 0.075(5) -0.055(4) 0.013(4) 0.010(4) O15 0.105(6) 0.084(5) 0.040(4) -0.011(3) -0.013(4) -0.025(4) O16 0.046(4) 0.093(5) 0.047(4) -0.037(3) 0.002(3) -0.009(3) C1 0.028(5) 0.057(5) 0.025(4) -0.002(4) 0.001(4) 0.004(4) C2 0.027(5) 0.026(4) 0.033(4) -0.005(3) -0.009(3) 0.009(3) C3 0.016(4) 0.025(4) 0.029(4) -0.008(3) -0.002(3) -0.004(3) C4 0.024(4) 0.023(4) 0.034(4) -0.011(3) -0.013(3) 0.009(3) C5 0.020(4) 0.025(4) 0.030(4) -0.004(3) -0.004(3) 0.001(3) C6 0.035(5) 0.030(4) 0.027(4) -0.003(3) 0.008(4) 0.005(3) C7 0.021(5) 0.032(4) 0.045(5) -0.011(4) 0.010(4) 0.002(3) C8 0.024(5) 0.049(5) 0.042(5) -0.011(4) -0.009(4) 0.004(4) C9 0.022(4) 0.033(4) 0.035(4) -0.011(3) -0.003(3) -0.002(3) C10 0.021(4) 0.023(4) 0.033(4) 0.001(3) -0.001(3) 0.003(3) C11 0.028(5) 0.031(4) 0.032(4) -0.005(3) -0.003(3) 0.007(3) C12 0.032(5) 0.028(4) 0.036(4) -0.004(3) -0.003(4) 0.007(3) C13 0.030(5) 0.033(4) 0.044(5) 0.006(4) 0.006(4) 0.011(4) C14 0.025(5) 0.044(5) 0.040(5) -0.009(4) 0.004(4) -0.003(4) C15 0.034(5) 0.037(4) 0.039(5) -0.008(4) -0.002(4) 0.008(4) C16 0.038(6) 0.083(7) 0.055(6) 0.005(5) 0.024(5) 0.000(5) C17 0.034(6) 0.105(8) 0.058(7) 0.022(6) 0.002(5) -0.007(6) C18 0.029(5) 0.042(5) 0.037(4) -0.011(4) 0.000(4) 0.006(4) C19 0.032(5) 0.031(4) 0.029(4) -0.013(3) -0.006(3) 0.004(3) C20 0.022(5) 0.032(4) 0.043(5) -0.017(3) -0.002(4) 0.003(3) C21 0.023(4) 0.031(4) 0.037(4) -0.014(3) 0.000(3) 0.006(3) C22 0.029(5) 0.028(4) 0.041(5) -0.013(3) -0.011(4) 0.008(3) C23 0.026(5) 0.039(4) 0.035(4) -0.006(3) 0.002(4) -0.001(4) C24 0.030(5) 0.031(4) 0.058(6) -0.015(4) 0.002(4) 0.003(4) C25 0.009(4) 0.049(5) 0.051(5) -0.020(4) -0.010(4) 0.000(3) C26 0.029(5) 0.028(4) 0.039(5) -0.015(3) -0.005(4) 0.010(3) C27 0.026(5) 0.033(4) 0.036(4) -0.015(3) -0.003(4) 0.006(3) C28 0.024(4) 0.041(4) 0.037(4) -0.020(4) -0.006(4) 0.003(3) C29 0.037(5) 0.038(4) 0.028(4) -0.013(3) -0.002(4) 0.003(4) C30 0.021(4) 0.043(4) 0.034(4) -0.009(4) 0.008(3) -0.003(4) C31 0.032(5) 0.037(4) 0.056(5) -0.019(4) -0.010(4) -0.004(4) C32 0.027(5) 0.046(5) 0.034(4) -0.017(4) -0.001(4) 0.006(4) C33 0.041(6) 0.057(6) 0.064(7) -0.002(5) 0.015(5) -0.002(4) C34 0.080(9) 0.106(9) 0.066(8) -0.011(7) 0.032(7) -0.031(7) O17 0.069(5) 0.060(4) 0.041(4) -0.015(3) -0.003(3) 0.018(3) O18 0.067(6) 0.164(9) 0.078(6) -0.065(6) -0.013(5) 0.048(6) O19 0.153(12) 0.151(10) 0.222(15) -0.054(9) -0.056(11) -0.017(9) O20 0.042(4) 0.050(3) 0.040(3) -0.015(3) 0.012(3) 0.000(3) O21 0.107(7) 0.075(5) 0.050(5) -0.015(4) 0.011(4) -0.027(5) O22 0.142(10) 0.085(7) 0.082(6) 0.005(5) 0.033(7) 0.041(6) O23 0.083(6) 0.074(5) 0.059(5) -0.001(4) 0.002(4) 0.025(4) O25 0.140(17) 0.040(8) 0.151(18) -0.018(9) -0.019(14) -0.009(9) O25' 0.13(2) 0.43(6) 0.26(4) 0.23(4) 0.07(3) 0.02(3) O24' 0.16(2) 0.141(17) 0.134(19) -0.090(15) 0.001(16) 0.013(15) O24 0.23(2) 0.037(8) 0.076(11) 0.008(7) -0.084(13) -0.028(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ba1 O18 2.738(9) . ? Ba1 O22 2.740(10) . ? Ba1 O23 2.768(9) . ? Ba1 O17 2.872(8) 2_767 ? Ba1 O20 2.877(6) 2_667 ? Ba1 O19 2.909(12) . ? Ba1 O21 2.916(9) . ? Ba1 O20 2.962(7) . ? Ba1 O17 3.067(8) . ? Ba1 O21 3.176(11) 2_667 ? Ba1 Ba1 4.409(6) 2_667 ? Ba1 H22A 2.6(2) . ? S1 O8 1.427(8) . ? S1 O7 1.459(7) . ? S1 O6 1.465(8) . ? S1 C12 1.754(8) . ? S2 O15 1.427(7) . ? S2 O16 1.438(7) . ? S2 O14 1.448(7) . ? S2 C29 1.752(8) . ? O1 C1 1.345(9) . ? O1 C9 1.352(9) . ? O2 C3 1.255(8) . ? O3 C5 1.339(9) . ? O3 H3 0.8200 . ? O4 C7 1.337(9) . ? O4 C16 1.403(11) . ? O5 C13 1.355(9) . ? O5 C17 1.448(12) . ? O9 C18 1.354(9) . ? O9 C26 1.375(9) . ? O10 C20 1.220(9) . ? O11 C22 1.328(9) . ? O11 H11 0.8200 . ? O12 C24 1.349(10) . ? O12 C33 1.402(11) . ? O13 C30 1.356(9) . ? O13 C34 1.459(12) . ? C1 C2 1.338(11) . ? C1 H1 0.9300 . ? C2 C10 1.472(10) . ? C2 C3 1.477(10) . ? C3 C4 1.432(10) . ? C4 C9 1.413(10) . ? C4 C5 1.417(10) . ? C5 C6 1.379(10) . ? C6 C7 1.395(11) . ? C6 H6 0.9300 . ? C7 C8 1.377(11) . ? C8 C9 1.366(11) . ? C8 H8 0.9300 . ? C10 C11 1.380(10) . ? C10 C15 1.385(11) . ? C11 C12 1.368(10) . ? C11 H11A 0.9300 . ? C12 C13 1.418(12) . ? C13 C14 1.377(11) . ? C14 C15 1.354(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.327(11) . ? C18 H18 0.9300 . ? C19 C20 1.476(11) . ? C19 C27 1.482(11) . ? C20 C21 1.427(10) . ? C21 C26 1.414(11) . ? C21 C22 1.426(11) . ? C22 C23 1.370(11) . ? C23 C24 1.410(12) . ? C23 H23 0.9300 . ? C24 C25 1.378(12) . ? C25 C26 1.343(11) . ? C25 H25 0.9300 . ? C27 C32 1.371(11) . ? C27 C28 1.391(10) . ? C28 C29 1.369(10) . ? C28 H28 0.9300 . ? C29 C30 1.389(11) . ? C30 C31 1.395(11) . ? C31 C32 1.376(11) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? O17 Ba1 2.872(8) 2_767 ? O17 H17D 0.85(2) . ? O17 H17E 0.87(2) . ? O18 H18A 0.86(2) . ? O18 H18B 0.85(2) . ? O20 Ba1 2.877(6) 2_667 ? O20 H20A 0.84(2) . ? O20 H20B 0.84(2) . ? O21 Ba1 3.176(10) 2_667 ? O21 H21A 0.86(2) . ? O21 H21B 0.86(2) . ? O22 H22A 0.86(2) . ? O22 H22B 0.86(2) . ? O23 H23A 0.86(2) . ? O23 H23B 0.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O18 Ba1 O22 126.4(3) . . ? O18 Ba1 O23 71.9(3) . . ? O22 Ba1 O23 71.6(3) . . ? O18 Ba1 O17 126.7(3) . 2_767 ? O22 Ba1 O17 79.7(3) . 2_767 ? O23 Ba1 O17 76.6(3) . 2_767 ? O18 Ba1 O20 145.3(2) . 2_667 ? O22 Ba1 O20 72.2(3) . 2_667 ? O23 Ba1 O20 140.5(2) . 2_667 ? O17 Ba1 O20 82.1(2) 2_767 2_667 ? O18 Ba1 O19 64.4(4) . . ? O22 Ba1 O19 69.4(4) . . ? O23 Ba1 O19 75.3(4) . . ? O17 Ba1 O19 143.4(3) 2_767 . ? O20 Ba1 O19 105.7(3) 2_667 . ? O18 Ba1 O21 105.9(3) . . ? O22 Ba1 O21 127.3(3) . . ? O23 Ba1 O21 139.8(3) . . ? O17 Ba1 O21 73.6(2) 2_767 . ? O20 Ba1 O21 59.87(19) 2_667 . ? O19 Ba1 O21 141.6(3) . . ? O18 Ba1 O20 65.0(2) . . ? O22 Ba1 O20 138.0(3) . . ? O23 Ba1 O20 136.8(2) . . ? O17 Ba1 O20 129.4(2) 2_767 . ? O20 Ba1 O20 81.9(2) 2_667 . ? O19 Ba1 O20 87.2(3) . . ? O21 Ba1 O20 56.9(2) . . ? O18 Ba1 O17 66.6(3) . . ? O22 Ba1 O17 135.3(3) . . ? O23 Ba1 O17 74.9(2) . . ? O17 Ba1 O17 64.3(2) 2_767 . ? O20 Ba1 O17 124.10(19) 2_667 . ? O19 Ba1 O17 128.2(3) . . ? O21 Ba1 O17 68.1(2) . . ? O20 Ba1 O17 86.6(2) . . ? O18 Ba1 O21 95.7(2) . 2_667 ? O22 Ba1 O21 81.9(3) . 2_667 ? O23 Ba1 O21 132.7(2) . 2_667 ? O17 Ba1 O21 136.6(2) 2_767 2_667 ? O20 Ba1 O21 54.8(2) 2_667 2_667 ? O19 Ba1 O21 58.7(3) . 2_667 ? O21 Ba1 O21 87.4(2) . 2_667 ? O20 Ba1 O21 56.1(2) . 2_667 ? O17 Ba1 O21 142.7(2) . 2_667 ? O18 Ba1 Ba1 104.60(19) . 2_667 ? O22 Ba1 Ba1 107.4(2) . 2_667 ? O23 Ba1 Ba1 173.5(2) . 2_667 ? O17 Ba1 Ba1 109.68(17) 2_767 2_667 ? O20 Ba1 Ba1 41.69(14) 2_667 2_667 ? O19 Ba1 Ba1 98.3(3) . 2_667 ? O21 Ba1 Ba1 46.03(18) . 2_667 ? O20 Ba1 Ba1 40.25(12) . 2_667 ? O17 Ba1 Ba1 109.05(18) . 2_667 ? O21 Ba1 Ba1 41.35(16) 2_667 2_667 ? O18 Ba1 H22A 127(4) . . ? O22 Ba1 H22A 18(2) . . ? O23 Ba1 H22A 61(4) . . ? O17 Ba1 H22A 64(2) 2_767 . ? O20 Ba1 H22A 80(4) 2_667 . ? O19 Ba1 H22A 82(3) . . ? O21 Ba1 H22A 125(4) . . ? O20 Ba1 H22A 155.7(15) . . ? O17 Ba1 H22A 117(2) . . ? O21 Ba1 H22A 99.9(10) 2_667 . ? Ba1 Ba1 H22A 120(3) 2_667 . ? O8 S1 O7 112.3(4) . . ? O8 S1 O6 115.3(5) . . ? O7 S1 O6 110.7(5) . . ? O8 S1 C12 106.0(4) . . ? O7 S1 C12 106.5(4) . . ? O6 S1 C12 105.3(4) . . ? O15 S2 O16 113.6(5) . . ? O15 S2 O14 109.8(5) . . ? O16 S2 O14 112.7(4) . . ? O15 S2 C29 108.5(4) . . ? O16 S2 C29 105.8(4) . . ? O14 S2 C29 106.0(4) . . ? C1 O1 C9 119.1(6) . . ? C5 O3 H3 109.5 . . ? C7 O4 C16 120.3(7) . . ? C13 O5 C17 117.9(7) . . ? C18 O9 C26 117.9(6) . . ? C22 O11 H11 109.5 . . ? C24 O12 C33 119.6(7) . . ? C30 O13 C34 118.5(7) . . ? C2 C1 O1 127.3(7) . . ? C2 C1 H1 116.4 . . ? O1 C1 H1 116.4 . . ? C1 C2 C10 120.5(7) . . ? C1 C2 C3 116.4(7) . . ? C10 C2 C3 123.0(7) . . ? O2 C3 C4 121.0(7) . . ? O2 C3 C2 122.7(6) . . ? C4 C3 C2 116.3(6) . . ? C9 C4 C5 115.8(7) . . ? C9 C4 C3 121.0(7) . . ? C5 C4 C3 123.1(7) . . ? O3 C5 C6 119.5(7) . . ? O3 C5 C4 119.4(6) . . ? C6 C5 C4 121.0(7) . . ? C5 C6 C7 120.2(7) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? O4 C7 C8 115.8(8) . . ? O4 C7 C6 123.7(7) . . ? C8 C7 C6 120.5(7) . . ? C9 C8 C7 118.9(8) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? O1 C9 C8 116.7(7) . . ? O1 C9 C4 119.8(6) . . ? C8 C9 C4 123.5(7) . . ? C11 C10 C15 116.6(7) . . ? C11 C10 C2 119.9(7) . . ? C15 C10 C2 123.4(7) . . ? C12 C11 C10 122.6(8) . . ? C12 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? C11 C12 C13 120.0(7) . . ? C11 C12 S1 119.7(6) . . ? C13 C12 S1 120.3(6) . . ? O5 C13 C14 125.7(8) . . ? O5 C13 C12 117.7(8) . . ? C14 C13 C12 116.6(7) . . ? C15 C14 C13 122.3(8) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C10 121.8(8) . . ? C14 C15 H15 119.1 . . ? C10 C15 H15 119.1 . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O9 127.3(8) . . ? C19 C18 H18 116.3 . . ? O9 C18 H18 116.3 . . ? C18 C19 C20 118.6(7) . . ? C18 C19 C27 120.7(7) . . ? C20 C19 C27 120.7(7) . . ? O10 C20 C21 123.4(8) . . ? O10 C20 C19 123.0(7) . . ? C21 C20 C19 113.6(7) . . ? C26 C21 C22 115.1(7) . . ? C26 C21 C20 123.6(7) . . ? C22 C21 C20 121.2(7) . . ? O11 C22 C23 119.2(7) . . ? O11 C22 C21 119.8(7) . . ? C23 C22 C21 121.0(7) . . ? C22 C23 C24 119.8(8) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? O12 C24 C25 116.4(8) . . ? O12 C24 C23 122.6(8) . . ? C25 C24 C23 121.0(7) . . ? C26 C25 C24 118.0(8) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 O9 116.1(7) . . ? C25 C26 C21 125.2(8) . . ? O9 C26 C21 118.7(7) . . ? C32 C27 C28 117.0(7) . . ? C32 C27 C19 124.1(7) . . ? C28 C27 C19 118.8(7) . . ? C29 C28 C27 122.3(7) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 120.2(7) . . ? C28 C29 S2 119.8(6) . . ? C30 C29 S2 120.0(6) . . ? O13 C30 C29 117.5(7) . . ? O13 C30 C31 124.6(7) . . ? C29 C30 C31 117.9(7) . . ? C32 C31 C30 120.7(7) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C27 C32 C31 121.8(7) . . ? C27 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? O12 C33 H33A 109.5 . . ? O12 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O12 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C34 H34A 109.5 . . ? O13 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O13 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Ba1 O17 Ba1 115.7(2) 2_767 . ? Ba1 O17 H17D 113(8) 2_767 . ? Ba1 O17 H17D 104(9) . . ? Ba1 O17 H17E 52(8) 2_767 . ? Ba1 O17 H17E 166(8) . . ? H17D O17 H17E 78(10) . . ? Ba1 O18 H18A 125(10) . . ? Ba1 O18 H18B 121(10) . . ? H18A O18 H18B 115(10) . . ? Ba1 O20 Ba1 98.1(2) 2_667 . ? Ba1 O20 H20A 129(8) 2_667 . ? Ba1 O20 H20A 111(7) . . ? Ba1 O20 H20B 156(6) 2_667 . ? Ba1 O20 H20B 90(7) . . ? H20A O20 H20B 67(7) . . ? Ba1 O21 Ba1 92.6(2) . 2_667 ? Ba1 O21 H21A 132(10) . . ? Ba1 O21 H21A 103(10) 2_667 . ? Ba1 O21 H21B 112(9) . . ? Ba1 O21 H21B 127(10) 2_667 . ? H21A O21 H21B 95(10) . . ? Ba1 O22 H22A 74(10) . . ? Ba1 O22 H22B 117(10) . . ? H22A O22 H22B 147(10) . . ? Ba1 O23 H23A 114(10) . . ? Ba1 O23 H23B 116(10) . . ? H23A O23 H23B 128(10) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.653 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.127 data_031217a _database_code_depnum_ccdc_archive 'CCDC 865947' #TrackingRef '- 1 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 Ba O18 S2, 4(H2 O) ' _chemical_formula_sum 'C30 H34 Ba O22 S2' _chemical_formula_weight 948.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9077(19) _cell_length_b 39.210(11) _cell_length_c 13.137(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.785(4) _cell_angle_gamma 90.00 _cell_volume 3540.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18156 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.1043 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6142 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6264 _refine_ls_number_parameters 575 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.003 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 Ba1 Ba 0.83787(5) 0.538078(10) 0.63306(3) 0.03855(13) Uani 1 1 d D . . O1 O 0.7082(6) 0.73063(11) 1.0847(3) 0.0409(11) Uani 1 1 d . . . O2 O 1.2159(6) 0.68443(11) 1.0282(3) 0.0504(12) Uani 1 1 d . . . O3 O 0.9890(7) 0.84040(11) 1.0772(3) 0.0602(13) Uani 1 1 d . . . H3 H 0.8787 0.8458 1.0888 0.090 Uiso 1 1 calc R . . O4 O 0.8746(9) 0.53579(13) 1.0879(4) 0.0822(17) Uani 1 1 d . . . H4 H 0.9283 0.5266 1.0423 0.123 Uiso 1 1 calc R . . O5 O 1.2651(17) 0.5825(3) 0.8947(11) 0.115(5) Uani 0.50 1 d PDU . . O5' O 1.0643(18) 0.5808(3) 0.8119(7) 0.062(3) Uani 0.50 1 d PDU . . O6 O 0.9565(19) 0.5621(4) 0.8197(9) 0.099(5) Uani 0.50 1 d PDU . . O6' O 0.9187(17) 0.5334(3) 0.8750(10) 0.105(4) Uani 0.50 1 d PDU . . O7 O 1.1345(19) 0.5320(3) 0.9551(9) 0.073(4) Uani 0.50 1 d PDU . . O7' O 1.2354(15) 0.5469(3) 0.9460(8) 0.069(4) Uani 0.50 1 d PDU . . O8 O 0.0252(6) 0.71835(11) 0.3429(3) 0.0519(12) Uani 1 1 d . . . O9 O 0.5540(6) 0.68014(11) 0.2924(3) 0.0502(12) Uani 1 1 d . . . O10 O 0.2374(7) 0.83233(11) 0.3094(3) 0.0556(13) Uani 1 1 d . . . H10 H 0.1252 0.8363 0.3212 0.083 Uiso 1 1 calc R . . O11 O 0.3309(7) 0.52744(11) 0.2905(4) 0.0472(13) Uani 1 1 d . . . O12 O 0.4701(6) 0.54330(13) 0.5275(3) 0.0618(14) Uani 1 1 d . . . O13 O 0.1836(6) 0.57131(11) 0.5771(3) 0.0449(11) Uani 1 1 d . . . O14 O 0.1532(6) 0.52086(11) 0.4782(3) 0.0474(11) Uani 1 1 d . . . O15 O 0.7966(10) 0.60978(15) 0.6340(5) 0.099(2) Uani 1 1 d D . . O16 O 0.5224(10) 0.5511(2) 0.7503(6) 0.122(3) Uani 1 1 d D . . O17 O 1.1540(8) 0.49901(12) 0.7200(3) 0.0602(14) Uani 1 1 d D . . O18 O 0.7658(7) 0.55587(13) 0.4130(4) 0.0609(14) Uani 1 1 d D . . S1 S 1.0749(3) 0.56303(5) 0.90465(15) 0.0607(6) Uani 1 1 d D . . S2 S 0.2661(2) 0.55113(4) 0.50087(12) 0.0358(4) Uani 1 1 d . . . C1 C 0.7249(10) 0.69671(17) 1.0784(4) 0.0413(16) Uani 1 1 d . . . H1 H 0.6134 0.6840 1.0856 0.050 Uiso 1 1 calc R . . C2 C 0.8862(9) 0.67916(16) 1.0627(4) 0.0345(15) Uani 1 1 d . . . C3 C 1.0625(9) 0.69893(16) 1.0465(4) 0.0352(15) Uani 1 1 d . . . C4 C 1.0440(9) 0.73506(15) 1.0534(4) 0.0331(14) Uani 1 1 d . . . C5 C 1.1970(9) 0.75755(18) 1.0410(5) 0.0459(17) Uani 1 1 d . . . H5 H 1.3161 0.7486 1.0268 0.055 Uiso 1 1 calc R . . C6 C 1.1788(10) 0.79211(18) 1.0488(5) 0.0501(18) Uani 1 1 d . . . H6 H 1.2844 0.8062 1.0407 0.060 Uiso 1 1 calc R . . C7 C 0.9999(11) 0.80625(17) 1.0691(5) 0.0459(17) Uani 1 1 d . . . C8 C 0.8429(9) 0.78532(17) 1.0811(4) 0.0421(16) Uani 1 1 d . . . H8 H 0.7238 0.7944 1.0946 0.051 Uiso 1 1 calc R . . C9 C 0.8673(9) 0.75018(16) 1.0724(4) 0.0346(15) Uani 1 1 d . . . C10 C 0.8835(9) 0.64140(16) 1.0655(4) 0.0372(15) Uani 1 1 d . . . C11 C 0.9642(9) 0.62172(16) 0.9923(4) 0.0380(15) Uani 1 1 d . . . H11 H 1.0187 0.6325 0.9390 0.046 Uiso 1 1 calc R . . C12 C 0.9649(9) 0.58629(16) 0.9972(4) 0.0397(16) Uani 1 1 d . . . C13 C 0.8801(10) 0.57060(17) 1.0761(5) 0.0458(17) Uani 1 1 d . . . C14 C 0.7995(10) 0.58944(17) 1.1485(5) 0.0488(18) Uani 1 1 d . . . H14 H 0.7441 0.5786 1.2014 0.059 Uiso 1 1 calc R . . C15 C 0.8002(8) 0.62501(17) 1.1432(5) 0.0414(16) Uani 1 1 d . . . H15 H 0.7442 0.6377 1.1923 0.050 Uiso 1 1 calc R . . C16 C 0.0581(10) 0.68444(16) 0.3391(5) 0.0444(17) Uani 1 1 d . . . H16 H -0.0430 0.6699 0.3519 0.053 Uiso 1 1 calc R . . C17 C 0.2297(9) 0.67002(15) 0.3178(4) 0.0339(14) Uani 1 1 d . . . C18 C 0.3933(9) 0.69201(16) 0.3045(4) 0.0380(15) Uani 1 1 d . . . C19 C 0.3536(9) 0.72850(16) 0.3051(4) 0.0367(15) Uani 1 1 d . . . C20 C 0.4953(9) 0.75310(17) 0.2893(4) 0.0416(16) Uani 1 1 d . . . H20 H 0.6199 0.7461 0.2779 0.050 Uiso 1 1 calc R . . C21 C 0.4543(10) 0.78678(16) 0.2903(5) 0.0443(17) Uani 1 1 d . . . H21 H 0.5495 0.8026 0.2782 0.053 Uiso 1 1 calc R . . C22 C 0.2675(11) 0.79798(17) 0.3097(4) 0.0435(17) Uani 1 1 d . . . C23 C 0.1289(10) 0.77525(17) 0.3277(4) 0.0434(17) Uani 1 1 d . . . H23 H 0.0065 0.7826 0.3420 0.052 Uiso 1 1 calc R . . C24 C 0.1716(9) 0.74029(16) 0.3247(4) 0.0360(15) Uani 1 1 d . . . C25 C 0.2485(8) 0.63223(15) 0.3114(4) 0.0338(14) Uani 1 1 d . . . C26 C 0.2315(8) 0.61109(16) 0.3947(4) 0.0352(15) Uani 1 1 d . . . H26 H 0.2007 0.6205 0.4560 0.042 Uiso 1 1 calc R . . C27 C 0.2597(8) 0.57626(15) 0.3882(4) 0.0297(14) Uani 1 1 d . . . C28 C 0.3026(8) 0.56176(16) 0.2954(4) 0.0356(15) Uani 1 1 d . . . C29 C 0.3190(8) 0.58334(16) 0.2143(5) 0.0366(15) Uani 1 1 d . . . H29 H 0.3458 0.5742 0.1519 0.044 Uiso 1 1 calc R . . C30 C 0.2970(9) 0.61775(16) 0.2230(4) 0.0387(16) Uani 1 1 d . . . H30 H 0.3155 0.6317 0.1674 0.046 Uiso 1 1 calc R . . H11A H 0.362(10) 0.5262(18) 0.235(5) 0.06(3) Uiso 1 1 d . . . H31 H 0.820(9) 0.6183(6) 0.6976(15) 0.080 Uiso 1 1 d D . . H32 H 0.688(6) 0.6199(16) 0.604(4) 0.080 Uiso 1 1 d D . . H33 H 0.454(10) 0.5317(10) 0.756(6) 0.080 Uiso 1 1 d D . . H34 H 0.483(10) 0.5664(11) 0.796(4) 0.080 Uiso 1 1 d D . . H35 H 1.167(10) 0.4936(14) 0.7866(12) 0.080 Uiso 1 1 d D . . H36 H 1.120(11) 0.4805(10) 0.682(3) 0.080 Uiso 1 1 d D . . H37 H 0.831(8) 0.5396(9) 0.3827(17) 0.080 Uiso 1 1 d D . . H38 H 0.801(10) 0.5767(6) 0.393(5) 0.080 Uiso 1 1 d D . . O22 O 0.5631(11) 0.49014(18) 0.8952(4) 0.113(2) Uani 1 1 d D . . H45 H 0.656(6) 0.4833(16) 0.944(4) 0.080 Uiso 1 1 d D . . H46 H 0.612(8) 0.5080(13) 0.863(5) 0.080 Uiso 1 1 d D . . O19 O 0.7457(7) 0.62640(14) 0.4143(4) 0.0721(15) Uani 1 1 d D . . H39 H 0.663(8) 0.6405(11) 0.377(5) 0.080 Uiso 1 1 d D . . H40 H 0.704(9) 0.6048(5) 0.406(5) 0.080 Uiso 1 1 d D . . O21 O 0.1980(9) 0.63942(17) 0.6754(4) 0.0896(18) Uani 1 1 d D . . H43 H 0.083(5) 0.644(2) 0.640(4) 0.080 Uiso 1 1 d D . . H44 H 0.192(8) 0.641(2) 0.7430(10) 0.080 Uiso 1 1 d D . . O20 O 0.3975(8) 0.64910(15) 0.8818(5) 0.0868(18) Uani 1 1 d D . . H41 H 0.377(11) 0.6268(4) 0.893(5) 0.080 Uiso 1 1 d D . . H42 H 0.340(9) 0.6622(11) 0.926(4) 0.080 Uiso 1 1 d D . . 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 Ba1 0.0337(2) 0.0357(2) 0.0458(2) 0.0039(2) 0.00176(15) 0.0016(2) O1 0.038(3) 0.034(3) 0.052(3) -0.002(2) 0.010(2) 0.004(2) O2 0.044(3) 0.041(3) 0.068(3) -0.003(2) 0.015(2) 0.008(2) O3 0.066(3) 0.032(3) 0.081(3) -0.003(3) -0.002(3) 0.001(2) O4 0.141(5) 0.034(3) 0.076(3) 0.006(3) 0.029(3) -0.001(3) O5 0.099(7) 0.105(8) 0.158(9) -0.048(7) 0.091(7) -0.024(6) O5' 0.091(7) 0.050(6) 0.047(6) 0.005(5) 0.021(5) 0.021(5) O6 0.106(8) 0.134(9) 0.054(6) -0.038(7) -0.013(6) 0.040(7) O6' 0.118(8) 0.085(8) 0.114(8) -0.049(7) 0.026(7) -0.013(7) O7 0.097(8) 0.049(7) 0.077(6) 0.001(5) 0.032(6) 0.022(6) O7' 0.057(6) 0.091(8) 0.057(6) 0.004(6) -0.003(5) 0.028(6) O8 0.045(3) 0.040(3) 0.072(3) 0.000(3) 0.014(2) -0.006(2) O9 0.040(3) 0.047(3) 0.064(3) -0.001(2) 0.010(2) 0.000(2) O10 0.068(3) 0.036(3) 0.062(3) 0.004(2) 0.005(3) 0.007(2) O11 0.068(3) 0.028(3) 0.049(3) -0.006(2) 0.021(3) 0.003(2) O12 0.032(2) 0.089(4) 0.063(3) 0.030(3) -0.003(2) 0.011(3) O13 0.045(3) 0.044(3) 0.047(3) 0.002(2) 0.012(2) 0.000(2) O14 0.050(3) 0.038(3) 0.055(3) 0.005(2) 0.009(2) -0.010(2) O15 0.100(5) 0.064(4) 0.125(5) -0.022(4) -0.027(4) 0.031(3) O16 0.090(5) 0.167(8) 0.119(6) -0.018(6) 0.055(4) 0.016(5) O17 0.079(4) 0.058(3) 0.043(3) 0.002(2) -0.001(3) 0.020(3) O18 0.058(3) 0.061(4) 0.066(3) -0.006(3) 0.015(3) 0.010(3) S1 0.0879(16) 0.0490(13) 0.0463(11) -0.0025(10) 0.0120(11) 0.0303(12) S2 0.0324(9) 0.0354(10) 0.0401(9) 0.0057(7) 0.0071(7) -0.0010(7) C1 0.047(4) 0.039(4) 0.039(4) -0.004(3) 0.009(3) -0.004(3) C2 0.036(4) 0.036(4) 0.031(3) -0.001(3) 0.006(3) 0.001(3) C3 0.044(4) 0.033(4) 0.028(3) 0.003(3) 0.005(3) 0.002(3) C4 0.039(4) 0.031(4) 0.028(3) 0.003(3) -0.001(3) -0.003(3) C5 0.037(4) 0.053(5) 0.047(4) 0.004(4) 0.003(3) 0.007(4) C6 0.047(4) 0.044(5) 0.058(4) 0.005(4) -0.002(4) -0.006(4) C7 0.066(5) 0.028(4) 0.042(4) -0.001(3) -0.005(4) -0.002(4) C8 0.046(4) 0.042(4) 0.037(4) -0.002(3) -0.004(3) 0.001(3) C9 0.042(4) 0.032(4) 0.030(3) -0.001(3) 0.002(3) 0.002(3) C10 0.040(4) 0.036(4) 0.034(4) 0.001(3) -0.001(3) 0.009(3) C11 0.049(4) 0.033(4) 0.032(3) 0.002(3) 0.006(3) 0.007(3) C12 0.052(4) 0.031(4) 0.035(4) 0.002(3) 0.004(3) 0.007(3) C13 0.058(5) 0.028(4) 0.052(4) 0.004(3) 0.008(4) -0.003(3) C14 0.064(5) 0.036(4) 0.049(4) 0.002(3) 0.019(4) -0.007(4) C15 0.038(4) 0.042(4) 0.046(4) 0.001(3) 0.013(3) 0.000(3) C16 0.053(4) 0.027(4) 0.053(4) -0.003(3) 0.005(3) 0.001(3) C17 0.046(4) 0.029(4) 0.026(3) -0.002(3) -0.001(3) 0.002(3) C18 0.037(4) 0.033(4) 0.045(4) 0.004(3) 0.002(3) 0.000(3) C19 0.044(4) 0.038(4) 0.027(3) 0.004(3) -0.002(3) -0.008(3) C20 0.043(4) 0.043(4) 0.039(4) 0.000(3) 0.005(3) -0.002(3) C21 0.062(5) 0.029(4) 0.043(4) 0.001(3) 0.009(3) -0.004(3) C22 0.070(5) 0.027(4) 0.034(4) 0.003(3) 0.008(3) -0.004(4) C23 0.052(4) 0.039(4) 0.039(4) -0.006(3) 0.001(3) 0.006(3) C24 0.043(4) 0.030(4) 0.034(3) 0.005(3) 0.002(3) 0.001(3) C25 0.035(4) 0.026(4) 0.040(4) -0.001(3) 0.000(3) -0.003(3) C26 0.028(3) 0.041(4) 0.036(3) -0.001(3) 0.001(3) -0.009(3) C27 0.026(3) 0.025(4) 0.039(3) 0.001(3) 0.006(3) -0.008(3) C28 0.036(4) 0.032(4) 0.038(4) -0.002(3) -0.001(3) -0.005(3) C29 0.034(4) 0.040(4) 0.037(4) -0.001(3) 0.008(3) -0.001(3) C30 0.049(4) 0.032(4) 0.035(3) 0.004(3) 0.005(3) -0.007(3) O22 0.179(7) 0.097(6) 0.063(4) -0.007(4) 0.012(4) 0.045(5) O19 0.063(4) 0.057(4) 0.096(4) 0.016(3) 0.006(3) 0.002(3) O21 0.106(5) 0.076(4) 0.088(4) -0.003(4) 0.018(4) -0.019(4) O20 0.079(4) 0.076(4) 0.113(5) -0.031(4) 0.044(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ba1 O6 2.677(10) . ? Ba1 O14 2.738(4) 3_666 ? Ba1 O12 2.777(4) . ? Ba1 O17 2.814(5) . ? Ba1 O15 2.826(6) . ? Ba1 O16 2.839(5) . ? Ba1 O13 2.880(4) 1_655 ? Ba1 O18 2.967(5) . ? Ba1 O11 3.034(5) 3_666 ? Ba1 O5' 3.168(12) . ? Ba1 O6' 3.177(13) . ? Ba1 O14 3.199(4) 1_655 ? O1 C1 1.338(7) . ? O1 C9 1.363(7) . ? O2 C3 1.247(7) . ? O3 C7 1.346(7) . ? O3 H3 0.8200 . ? O4 C13 1.375(7) . ? O4 H4 0.8200 . ? O5 S1 1.537(10) . ? O5 O7' 1.572(16) . ? O5 O5' 1.676(16) . ? O5' O6 1.058(15) . ? O5' S1 1.400(9) . ? O6 S1 1.316(9) . ? O6 O6' 1.380(16) . ? O6' S1 1.607(10) . ? O6' O7 1.737(17) . ? O7 O7' 0.927(13) . ? O7 S1 1.426(9) . ? O7' S1 1.342(9) . ? O8 C16 1.351(7) . ? O8 C24 1.367(7) . ? O9 C18 1.229(7) . ? O10 C22 1.363(7) . ? O10 H10 0.8200 . ? O11 C28 1.362(7) . ? O11 Ba1 3.034(5) 3_666 ? O11 H11A 0.78(6) . ? O12 S2 1.450(4) . ? O13 S2 1.438(4) . ? O13 Ba1 2.880(4) 1_455 ? O14 S2 1.435(4) . ? O14 Ba1 2.738(4) 3_666 ? O14 Ba1 3.199(4) 1_455 ? O15 H31 0.900(10) . ? O15 H32 0.904(11) . ? O16 H33 0.900(11) . ? O16 H34 0.905(11) . ? O17 H35 0.896(11) . ? O17 H36 0.897(11) . ? O18 H37 0.898(11) . ? O18 H38 0.901(11) . ? S1 C12 1.753(6) . ? S2 C27 1.775(6) . ? S2 Ba1 3.6144(17) 1_455 ? C1 C2 1.343(8) . ? C1 H1 0.9300 . ? C2 C3 1.477(8) . ? C2 C10 1.481(8) . ? C3 C4 1.426(8) . ? C4 C5 1.398(8) . ? C4 C9 1.402(8) . ? C5 C6 1.366(9) . ? C5 H5 0.9300 . ? C6 C7 1.405(9) . ? C6 H6 0.9300 . ? C7 C8 1.382(9) . ? C8 C9 1.394(8) . ? C8 H8 0.9300 . ? C10 C15 1.381(8) . ? C10 C11 1.392(8) . ? C11 C12 1.391(8) . ? C11 H11 0.9300 . ? C12 C13 1.385(8) . ? C13 C14 1.367(8) . ? C14 C15 1.396(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.367(8) . ? C16 H16 0.9300 . ? C17 C18 1.446(8) . ? C17 C25 1.491(8) . ? C18 C19 1.457(8) . ? C19 C24 1.388(8) . ? C19 C20 1.405(8) . ? C20 C21 1.351(8) . ? C20 H20 0.9300 . ? C21 C22 1.411(9) . ? C21 H21 0.9300 . ? C22 C23 1.346(8) . ? C23 C24 1.404(8) . ? C23 H23 0.9300 . ? C25 C30 1.364(7) . ? C25 C26 1.388(8) . ? C26 C27 1.383(8) . ? C26 H26 0.9300 . ? C27 C28 1.403(8) . ? C28 C29 1.375(8) . ? C29 C30 1.364(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O22 H45 0.905(11) . ? O22 H46 0.900(11) . ? O19 H39 0.900(11) . ? O19 H40 0.899(11) . ? O21 H43 0.899(11) . ? O21 H44 0.896(11) . ? O20 H41 0.901(11) . ? O20 H42 0.897(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ba1 O14 139.9(3) . 3_666 ? O6 Ba1 O12 127.7(3) . . ? O14 Ba1 O12 82.21(14) 3_666 . ? O6 Ba1 O17 70.5(3) . . ? O14 Ba1 O17 72.48(13) 3_666 . ? O12 Ba1 O17 151.23(15) . . ? O6 Ba1 O15 70.6(4) . . ? O14 Ba1 O15 148.18(16) 3_666 . ? O12 Ba1 O15 80.87(17) . . ? O17 Ba1 O15 127.89(17) . . ? O6 Ba1 O16 67.7(3) . . ? O14 Ba1 O16 120.1(2) 3_666 . ? O12 Ba1 O16 62.88(19) . . ? O17 Ba1 O16 119.0(2) . . ? O15 Ba1 O16 74.7(2) . . ? O6 Ba1 O13 83.7(4) . 1_655 ? O14 Ba1 O13 100.46(12) 3_666 1_655 ? O12 Ba1 O13 125.41(12) . 1_655 ? O17 Ba1 O13 73.76(14) . 1_655 ? O15 Ba1 O13 68.75(17) . 1_655 ? O16 Ba1 O13 139.4(2) . 1_655 ? O6 Ba1 O18 144.6(4) . . ? O14 Ba1 O18 71.88(13) 3_666 . ? O12 Ba1 O18 55.99(12) . . ? O17 Ba1 O18 124.80(13) . . ? O15 Ba1 O18 76.31(16) . . ? O16 Ba1 O18 115.09(19) . . ? O13 Ba1 O18 72.95(13) 1_655 . ? O6 Ba1 O11 95.0(4) . 3_666 ? O14 Ba1 O11 59.48(12) 3_666 3_666 ? O12 Ba1 O11 82.25(14) . 3_666 ? O17 Ba1 O11 73.32(14) . 3_666 ? O15 Ba1 O11 143.00(17) . 3_666 ? O16 Ba1 O11 68.3(2) . 3_666 ? O13 Ba1 O11 145.47(12) 1_655 3_666 ? O18 Ba1 O11 119.30(14) . 3_666 ? O6 Ba1 O5' 18.5(4) . . ? O14 Ba1 O5' 143.7(2) 3_666 . ? O12 Ba1 O5' 133.6(2) . . ? O17 Ba1 O5' 71.5(2) . . ? O15 Ba1 O5' 60.8(2) . . ? O16 Ba1 O5' 81.5(3) . . ? O13 Ba1 O5' 65.8(2) 1_655 . ? O18 Ba1 O5' 128.3(2) . . ? O11 Ba1 O5' 112.33(19) 3_666 . ? O6 Ba1 O6' 25.5(4) . . ? O14 Ba1 O6' 118.3(2) 3_666 . ? O12 Ba1 O6' 124.3(2) . . ? O17 Ba1 O6' 60.7(2) . . ? O15 Ba1 O6' 93.5(3) . . ? O16 Ba1 O6' 62.3(3) . . ? O13 Ba1 O6' 102.4(2) 1_655 . ? O18 Ba1 O6' 169.7(2) . . ? O11 Ba1 O6' 69.8(2) 3_666 . ? O5' Ba1 O6' 42.7(2) . . ? O6 Ba1 O14 119.4(3) . 1_655 ? O14 Ba1 O14 55.17(14) 3_666 1_655 ? O12 Ba1 O14 110.19(12) . 1_655 ? O17 Ba1 O14 65.98(12) . 1_655 ? O15 Ba1 O14 106.75(16) . 1_655 ? O16 Ba1 O14 172.83(19) . 1_655 ? O13 Ba1 O14 45.40(11) 1_655 1_655 ? O18 Ba1 O14 59.20(12) . 1_655 ? O11 Ba1 O14 109.93(12) 3_666 1_655 ? O5' Ba1 O14 105.5(2) . 1_655 ? O6' Ba1 O14 124.2(2) . 1_655 ? C1 O1 C9 118.4(5) . . ? C7 O3 H3 109.5 . . ? C13 O4 H4 109.5 . . ? S1 O5 O7' 51.1(4) . . ? S1 O5 O5' 51.4(5) . . ? O7' O5 O5' 96.2(7) . . ? O6 O5' S1 62.9(7) . . ? O6 O5' O5 120.6(10) . . ? S1 O5' O5 59.1(5) . . ? O6 O5' Ba1 53.5(9) . . ? S1 O5' Ba1 111.1(6) . . ? O5 O5' Ba1 144.8(6) . . ? O5' O6 S1 71.3(8) . . ? O5' O6 O6' 142.2(13) . . ? S1 O6 O6' 73.2(8) . . ? O5' O6 Ba1 108.0(12) . . ? S1 O6 Ba1 153.3(8) . . ? O6' O6 Ba1 97.9(9) . . ? O6 O6' S1 51.6(5) . . ? O6 O6' O7 98.5(8) . . ? S1 O6' O7 50.3(4) . . ? O6 O6' Ba1 56.6(7) . . ? S1 O6' Ba1 104.3(6) . . ? O7 O6' Ba1 131.4(6) . . ? O7' O7 S1 65.6(8) . . ? O7' O7 O6' 120.9(12) . . ? S1 O7 O6' 60.1(6) . . ? O7 O7' S1 75.4(9) . . ? O7 O7' O5 138.4(12) . . ? S1 O7' O5 63.1(6) . . ? C16 O8 C24 118.9(5) . . ? C22 O10 H10 109.5 . . ? C28 O11 Ba1 139.4(4) . 3_666 ? C28 O11 H11A 99(5) . . ? Ba1 O11 H11A 114(5) 3_666 . ? S2 O12 Ba1 162.6(3) . . ? S2 O13 Ba1 109.0(2) . 1_455 ? S2 O14 Ba1 140.2(2) . 3_666 ? S2 O14 Ba1 94.8(2) . 1_455 ? Ba1 O14 Ba1 124.83(14) 3_666 1_455 ? Ba1 O15 H31 111.5(17) . . ? Ba1 O15 H32 121(5) . . ? H31 O15 H32 108(5) . . ? Ba1 O16 H33 109(4) . . ? Ba1 O16 H34 140(4) . . ? H33 O16 H34 108(3) . . ? Ba1 O17 H35 122(5) . . ? Ba1 O17 H36 94(5) . . ? H35 O17 H36 110(3) . . ? Ba1 O18 H37 102.9(16) . . ? Ba1 O18 H38 119(5) . . ? H37 O18 H38 110(3) . . ? O6 S1 O7' 138.4(8) . . ? O6 S1 O5' 45.7(7) . . ? O7' S1 O5' 123.7(7) . . ? O6 S1 O7 119.8(8) . . ? O7' S1 O7 39.0(7) . . ? O5' S1 O7 144.8(6) . . ? O6 S1 O5 113.9(8) . . ? O7' S1 O5 65.8(7) . . ? O5' S1 O5 69.4(7) . . ? O7 S1 O5 104.7(7) . . ? O6 S1 O6' 55.3(7) . . ? O7' S1 O6' 105.3(7) . . ? O5' S1 O6' 100.1(7) . . ? O7 S1 O6' 69.6(7) . . ? O5 S1 O6' 153.9(6) . . ? O6 S1 C12 109.1(6) . . ? O7' S1 C12 111.2(5) . . ? O5' S1 C12 110.9(5) . . ? O7 S1 C12 104.3(5) . . ? O5 S1 C12 103.5(5) . . ? O6' S1 C12 102.6(5) . . ? O14 S2 O13 110.8(3) . . ? O14 S2 O12 111.7(3) . . ? O13 S2 O12 113.1(3) . . ? O14 S2 C27 108.6(3) . . ? O13 S2 C27 107.3(3) . . ? O12 S2 C27 105.1(3) . . ? O14 S2 Ba1 61.88(17) . 1_455 ? O13 S2 Ba1 48.88(17) . 1_455 ? O12 S2 Ba1 132.59(18) . 1_455 ? C27 S2 Ba1 121.77(19) . 1_455 ? O1 C1 C2 126.6(6) . . ? O1 C1 H1 116.7 . . ? C2 C1 H1 116.7 . . ? C1 C2 C3 117.5(6) . . ? C1 C2 C10 119.7(6) . . ? C3 C2 C10 122.7(5) . . ? O2 C3 C4 123.3(6) . . ? O2 C3 C2 121.2(6) . . ? C4 C3 C2 115.6(6) . . ? C5 C4 C9 115.9(6) . . ? C5 C4 C3 123.1(6) . . ? C9 C4 C3 121.1(6) . . ? C6 C5 C4 122.7(6) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C7 119.7(7) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? O3 C7 C8 122.1(7) . . ? O3 C7 C6 117.7(6) . . ? C8 C7 C6 120.2(6) . . ? C7 C8 C9 118.3(6) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? O1 C9 C8 116.1(6) . . ? O1 C9 C4 120.7(5) . . ? C8 C9 C4 123.2(6) . . ? C15 C10 C11 118.6(6) . . ? C15 C10 C2 119.4(5) . . ? C11 C10 C2 122.0(6) . . ? C12 C11 C10 121.5(6) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 118.6(6) . . ? C13 C12 S1 122.2(5) . . ? C11 C12 S1 119.2(5) . . ? C14 C13 O4 116.1(6) . . ? C14 C13 C12 120.9(6) . . ? O4 C13 C12 123.0(6) . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 120.4(6) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O8 C16 C17 124.6(6) . . ? O8 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? C16 C17 C18 118.8(6) . . ? C16 C17 C25 120.3(6) . . ? C18 C17 C25 120.8(6) . . ? O9 C18 C17 121.1(6) . . ? O9 C18 C19 123.1(6) . . ? C17 C18 C19 115.8(6) . . ? C24 C19 C20 117.2(6) . . ? C24 C19 C18 120.2(6) . . ? C20 C19 C18 122.6(6) . . ? C21 C20 C19 121.3(6) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.2(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 O10 122.9(6) . . ? C23 C22 C21 120.4(6) . . ? O10 C22 C21 116.7(6) . . ? C22 C23 C24 119.1(6) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? O8 C24 C19 121.5(6) . . ? O8 C24 C23 116.6(6) . . ? C19 C24 C23 121.8(6) . . ? C30 C25 C26 118.1(6) . . ? C30 C25 C17 119.5(5) . . ? C26 C25 C17 122.3(5) . . ? C27 C26 C25 121.1(5) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 S2 119.2(4) . . ? C28 C27 S2 120.6(5) . . ? O11 C28 C29 123.2(6) . . ? O11 C28 C27 119.1(6) . . ? C29 C28 C27 117.7(6) . . ? C30 C29 C28 121.7(6) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C25 121.5(6) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? H45 O22 H46 107(3) . . ? H39 O19 H40 110(3) . . ? H43 O21 H44 111(3) . . ? H41 O20 H42 111(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.957 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.088 # Attachment '- 2 cif.txt' data_040226a _database_code_depnum_ccdc_archive 'CCDC 865948' #TrackingRef '- 2 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Ba O18 S2, 8(H2 O) ' _chemical_formula_sum 'C32 H46 Ba O26 S2' _chemical_formula_weight 1048.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.752(7) _cell_length_b 9.780(8) _cell_length_c 15.148(13) _cell_angle_alpha 77.246(13) _cell_angle_beta 84.484(14) _cell_angle_gamma 70.415(12) _cell_volume 1055.0(16) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1505 _cell_measurement_theta_min 2.823 _cell_measurement_theta_max 24.343 _exptl_crystal_description plate _exptl_crystal_colour white _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4478 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3462 _reflns_number_gt 2682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3731 _refine_ls_number_parameters 316 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ba1 Ba 1.0000 0.0000 1.0000 0.03871(19) Uani 1 2 d S . . O1 O 0.7666(6) 0.8047(4) 0.4034(2) 0.0459(10) Uani 1 1 d . . . O2 O 0.6703(5) 0.8198(4) 0.6707(3) 0.0448(10) Uani 1 1 d . . . O3 O 0.8545(6) 1.2740(4) 0.3364(3) 0.0506(11) Uani 1 1 d . . . O4 O 0.7687(5) 0.1556(4) 0.8112(3) 0.0439(10) Uani 1 1 d D . . O5 O 1.1570(5) 0.1050(4) 0.8203(2) 0.0372(9) Uani 1 1 d . . . O6 O 0.9965(5) 0.2896(4) 0.9056(2) 0.0433(9) Uani 1 1 d . . . O7 O 1.2094(5) 0.3419(4) 0.7849(3) 0.0453(10) Uani 1 1 d . . . O8 O 0.6710(6) 0.2023(6) 1.0288(3) 0.0718(14) Uani 1 1 d D . . O9 O 1.1944(8) 0.1365(5) 1.0694(4) 0.0793(17) Uani 1 1 d D . . O10 O 0.5418(5) 0.0141(5) 0.7901(3) 0.0462(10) Uani 1 1 d D . . O11 O 0.4229(6) 0.4177(5) 0.8958(3) 0.0541(11) Uani 1 1 d D . . O12 O 0.5430(6) 0.6582(5) 0.8288(3) 0.0526(11) Uani 1 1 d D . . O13 O 0.8077(6) 0.5646(5) 0.9549(3) 0.0564(11) Uani 1 1 d D . . S1 S 1.08032(17) 0.26425(14) 0.81798(9) 0.0320(3) Uani 1 1 d . . . C1 C 0.7571(8) 0.6859(6) 0.4675(4) 0.0418(14) Uani 1 1 d . . . H1 H 0.7661 0.6006 0.4471 0.050 Uiso 1 1 calc R . . C2 C 0.7363(7) 0.6788(6) 0.5561(4) 0.0332(12) Uani 1 1 d . . . C3 C 0.7098(7) 0.8139(6) 0.5900(4) 0.0328(12) Uani 1 1 d . . . C4 C 0.7371(7) 0.9355(6) 0.5234(3) 0.0321(12) Uani 1 1 d . . . C5 C 0.7407(7) 1.0667(6) 0.5469(4) 0.0403(14) Uani 1 1 d . . . H5 H 0.7167 1.0787 0.6066 0.048 Uiso 1 1 calc R . . C6 C 0.7787(7) 1.1754(6) 0.4836(4) 0.0418(14) Uani 1 1 d . . . H6 H 0.7823 1.2601 0.5007 0.050 Uiso 1 1 calc R . . C7 C 0.8128(7) 1.1619(6) 0.3924(4) 0.0381(13) Uani 1 1 d . . . C8 C 0.8049(7) 1.0372(6) 0.3671(4) 0.0376(13) Uani 1 1 d . . . H8 H 0.8249 1.0271 0.3070 0.045 Uiso 1 1 calc R . . C9 C 0.7670(7) 0.9281(6) 0.4323(4) 0.0339(13) Uani 1 1 d . . . C10 C 0.7420(7) 0.5379(5) 0.6210(3) 0.0314(12) Uani 1 1 d . . . C11 C 0.8865(7) 0.4697(5) 0.6790(3) 0.0311(12) Uani 1 1 d . . . H11 H 0.9785 0.5120 0.6758 0.037 Uiso 1 1 calc R . . C12 C 0.8993(7) 0.3410(5) 0.7418(3) 0.0285(11) Uani 1 1 d . . . C13 C 0.7579(7) 0.2791(5) 0.7466(4) 0.0311(12) Uani 1 1 d . . . C14 C 0.6136(7) 0.3467(6) 0.6884(4) 0.0357(13) Uani 1 1 d . . . H14 H 0.5212 0.3049 0.6911 0.043 Uiso 1 1 calc R . . C15 C 0.6042(7) 0.4751(6) 0.6265(4) 0.0376(13) Uani 1 1 d . . . H15 H 0.5052 0.5198 0.5882 0.045 Uiso 1 1 calc R . . C16 C 0.9083(10) 1.2594(7) 0.2456(4) 0.0600(18) Uani 1 1 d . . . H16A H 0.9342 1.3468 0.2133 0.090 Uiso 1 1 calc R . . H16B H 0.8110 1.2470 0.2168 0.090 Uiso 1 1 calc R . . H16C H 1.0160 1.1745 0.2454 0.090 Uiso 1 1 calc R . . H16 H 0.683(7) 0.113(7) 0.810(5) 0.080 Uiso 1 1 d D . . H17 H 0.612(7) 0.229(7) 1.080(2) 0.080 Uiso 1 1 d D . . H18 H 0.598(7) 0.251(7) 0.981(2) 0.080 Uiso 1 1 d D . . H19 H 1.257(8) 0.100(6) 1.121(3) 0.080 Uiso 1 1 d D . . H20 H 1.169(9) 0.2353(15) 1.056(4) 0.080 Uiso 1 1 d D . . H21 H 0.4197(19) 0.053(7) 0.796(4) 0.080 Uiso 1 1 d D . . H22 H 0.571(7) -0.022(7) 0.739(3) 0.080 Uiso 1 1 d D . . H23 H 0.339(6) 0.433(8) 0.941(3) 0.080 Uiso 1 1 d D . . H24 H 0.373(7) 0.414(8) 0.846(2) 0.080 Uiso 1 1 d D . . H25 H 0.516(9) 0.575(4) 0.832(4) 0.080 Uiso 1 1 d D . . H26 H 0.580(9) 0.692(6) 0.7727(18) 0.080 Uiso 1 1 d D . . H27 H 0.736(6) 0.580(7) 0.908(3) 0.080 Uiso 1 1 d D . . H28 H 0.916(4) 0.496(6) 0.948(4) 0.080 Uiso 1 1 d D . . 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 Ba1 0.0420(3) 0.0328(3) 0.0466(3) -0.0121(2) 0.0033(2) -0.0174(2) O1 0.074(3) 0.039(2) 0.033(2) -0.0093(18) -0.0038(19) -0.028(2) O2 0.060(3) 0.043(2) 0.038(2) -0.0164(19) 0.0081(19) -0.021(2) O3 0.068(3) 0.042(2) 0.047(3) 0.000(2) 0.003(2) -0.032(2) O4 0.046(2) 0.034(2) 0.057(3) 0.0007(19) -0.007(2) -0.0244(18) O5 0.038(2) 0.030(2) 0.045(2) -0.0083(17) -0.0013(16) -0.0125(16) O6 0.060(3) 0.039(2) 0.035(2) -0.0119(17) -0.0003(18) -0.0186(19) O7 0.041(2) 0.044(2) 0.059(3) 0.000(2) -0.0091(19) -0.0288(19) O8 0.066(3) 0.070(3) 0.052(3) -0.008(3) 0.009(2) 0.008(2) O9 0.115(4) 0.045(3) 0.087(4) 0.010(3) -0.058(3) -0.038(3) O10 0.039(2) 0.051(3) 0.061(3) -0.024(2) -0.0016(19) -0.022(2) O11 0.060(3) 0.064(3) 0.049(3) -0.019(2) -0.001(2) -0.028(2) O12 0.065(3) 0.052(3) 0.050(3) -0.015(2) 0.013(2) -0.032(2) O13 0.053(3) 0.050(3) 0.070(3) -0.022(2) -0.005(2) -0.015(2) S1 0.0353(8) 0.0276(7) 0.0371(8) -0.0070(6) -0.0036(6) -0.0145(6) C1 0.060(4) 0.032(3) 0.039(4) -0.010(3) 0.000(3) -0.021(3) C2 0.038(3) 0.031(3) 0.034(3) -0.007(2) -0.005(2) -0.014(2) C3 0.029(3) 0.034(3) 0.036(3) -0.010(3) -0.002(2) -0.009(2) C4 0.032(3) 0.034(3) 0.032(3) -0.008(2) -0.003(2) -0.012(2) C5 0.046(3) 0.040(3) 0.041(3) -0.014(3) 0.001(3) -0.018(3) C6 0.044(3) 0.033(3) 0.053(4) -0.009(3) 0.001(3) -0.018(3) C7 0.038(3) 0.036(3) 0.044(4) -0.007(3) -0.004(3) -0.018(3) C8 0.041(3) 0.041(3) 0.032(3) -0.004(3) -0.002(2) -0.018(3) C9 0.031(3) 0.030(3) 0.044(3) -0.005(3) -0.007(2) -0.013(2) C10 0.038(3) 0.028(3) 0.034(3) -0.014(2) 0.003(2) -0.014(2) C11 0.034(3) 0.026(3) 0.039(3) -0.010(2) 0.001(2) -0.016(2) C12 0.035(3) 0.022(3) 0.032(3) -0.007(2) 0.001(2) -0.013(2) C13 0.039(3) 0.023(3) 0.038(3) -0.009(2) 0.003(2) -0.017(2) C14 0.035(3) 0.034(3) 0.047(3) -0.013(3) -0.003(3) -0.019(2) C15 0.040(3) 0.037(3) 0.040(3) -0.013(3) -0.004(3) -0.013(3) C16 0.080(5) 0.054(4) 0.052(4) 0.005(3) -0.003(4) -0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ba1 O8 2.720(4) . ? Ba1 O8 2.720(4) 2_757 ? Ba1 O9 2.726(5) . ? Ba1 O9 2.726(5) 2_757 ? Ba1 O6 2.869(4) 2_757 ? Ba1 O6 2.869(4) . ? Ba1 O5 2.985(4) 2_757 ? Ba1 O5 2.985(4) . ? Ba1 O4 3.308(4) 2_757 ? Ba1 O4 3.308(4) . ? Ba1 S1 3.503(2) 2_757 ? Ba1 S1 3.503(2) . ? O1 C1 1.358(6) . ? O1 C9 1.373(6) . ? O2 C3 1.240(6) . ? O3 C7 1.342(7) . ? O3 C16 1.422(7) . ? O4 C13 1.360(6) . ? O4 H16 0.900(10) . ? O5 S1 1.462(4) . ? O6 S1 1.455(4) . ? O7 S1 1.440(4) . ? O8 H17 0.898(10) . ? O8 H18 0.897(10) . ? O9 H19 0.898(10) . ? O9 H20 0.897(10) . ? O10 H21 0.898(10) . ? O10 H22 0.898(10) . ? O11 H23 0.894(10) . ? O11 H24 0.893(10) . ? O12 H25 0.895(10) . ? O12 H26 0.896(10) . ? O13 H27 0.898(10) . ? O13 H28 0.896(10) . ? S1 C12 1.757(5) . ? C1 C2 1.327(7) . ? C1 H1 0.9300 . ? C2 C3 1.466(7) . ? C2 C10 1.495(7) . ? C3 C4 1.441(7) . ? C4 C9 1.391(7) . ? C4 C5 1.415(7) . ? C5 C6 1.357(8) . ? C5 H5 0.9300 . ? C6 C7 1.408(8) . ? C6 H6 0.9300 . ? C7 C8 1.378(7) . ? C8 C9 1.375(8) . ? C8 H8 0.9300 . ? C10 C11 1.379(7) . ? C10 C15 1.388(7) . ? C11 C12 1.380(7) . ? C11 H11 0.9300 . ? C12 C13 1.409(7) . ? C13 C14 1.379(7) . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ba1 O8 180.000(1) . 2_757 ? O8 Ba1 O9 93.80(19) . . ? O8 Ba1 O9 86.20(19) 2_757 . ? O8 Ba1 O9 86.20(19) . 2_757 ? O8 Ba1 O9 93.80(19) 2_757 2_757 ? O9 Ba1 O9 180.0 . 2_757 ? O8 Ba1 O6 109.52(15) . 2_757 ? O8 Ba1 O6 70.48(14) 2_757 2_757 ? O9 Ba1 O6 118.07(13) . 2_757 ? O9 Ba1 O6 61.93(13) 2_757 2_757 ? O8 Ba1 O6 70.48(14) . . ? O8 Ba1 O6 109.52(14) 2_757 . ? O9 Ba1 O6 61.93(13) . . ? O9 Ba1 O6 118.07(13) 2_757 . ? O6 Ba1 O6 180.000(1) 2_757 . ? O8 Ba1 O5 70.55(13) . 2_757 ? O8 Ba1 O5 109.45(12) 2_757 2_757 ? O9 Ba1 O5 94.04(15) . 2_757 ? O9 Ba1 O5 85.96(15) 2_757 2_757 ? O6 Ba1 O5 48.03(10) 2_757 2_757 ? O6 Ba1 O5 131.97(10) . 2_757 ? O8 Ba1 O5 109.45(13) . . ? O8 Ba1 O5 70.55(12) 2_757 . ? O9 Ba1 O5 85.96(15) . . ? O9 Ba1 O5 94.04(15) 2_757 . ? O6 Ba1 O5 131.97(10) 2_757 . ? O6 Ba1 O5 48.03(10) . . ? O5 Ba1 O5 180.000(1) 2_757 . ? O8 Ba1 O4 111.99(13) . 2_757 ? O8 Ba1 O4 68.01(13) 2_757 2_757 ? O9 Ba1 O4 57.88(12) . 2_757 ? O9 Ba1 O4 122.12(12) 2_757 2_757 ? O6 Ba1 O4 60.20(10) 2_757 2_757 ? O6 Ba1 O4 119.80(10) . 2_757 ? O5 Ba1 O4 54.47(11) 2_757 2_757 ? O5 Ba1 O4 125.53(11) . 2_757 ? O8 Ba1 O4 68.01(13) . . ? O8 Ba1 O4 111.99(13) 2_757 . ? O9 Ba1 O4 122.12(12) . . ? O9 Ba1 O4 57.88(12) 2_757 . ? O6 Ba1 O4 119.80(10) 2_757 . ? O6 Ba1 O4 60.20(10) . . ? O5 Ba1 O4 125.53(11) 2_757 . ? O5 Ba1 O4 54.47(11) . . ? O4 Ba1 O4 180.0 2_757 . ? O8 Ba1 S1 91.63(12) . 2_757 ? O8 Ba1 S1 88.37(12) 2_757 2_757 ? O9 Ba1 S1 105.33(12) . 2_757 ? O9 Ba1 S1 74.67(12) 2_757 2_757 ? O6 Ba1 S1 23.84(7) 2_757 2_757 ? O6 Ba1 S1 156.16(7) . 2_757 ? O5 Ba1 S1 24.41(7) 2_757 2_757 ? O5 Ba1 S1 155.59(7) . 2_757 ? O4 Ba1 S1 51.51(8) 2_757 2_757 ? O4 Ba1 S1 128.49(8) . 2_757 ? O8 Ba1 S1 88.37(12) . . ? O8 Ba1 S1 91.63(12) 2_757 . ? O9 Ba1 S1 74.67(12) . . ? O9 Ba1 S1 105.33(12) 2_757 . ? O6 Ba1 S1 156.16(7) 2_757 . ? O6 Ba1 S1 23.84(7) . . ? O5 Ba1 S1 155.59(7) 2_757 . ? O5 Ba1 S1 24.41(7) . . ? O4 Ba1 S1 128.49(8) 2_757 . ? O4 Ba1 S1 51.51(8) . . ? S1 Ba1 S1 180.0 2_757 . ? C1 O1 C9 117.6(4) . . ? C7 O3 C16 118.2(5) . . ? C13 O4 Ba1 133.9(3) . . ? C13 O4 H16 116(4) . . ? Ba1 O4 H16 109(4) . . ? S1 O5 Ba1 98.04(17) . . ? S1 O6 Ba1 103.30(19) . . ? Ba1 O8 H17 132(4) . . ? Ba1 O8 H18 119(4) . . ? H17 O8 H18 109(5) . . ? Ba1 O9 H19 125(4) . . ? Ba1 O9 H20 122(4) . . ? H19 O9 H20 109(5) . . ? H21 O10 H22 110(5) . . ? H23 O11 H24 111(3) . . ? H25 O12 H26 112(3) . . ? H27 O13 H28 110(5) . . ? O7 S1 O6 114.1(2) . . ? O7 S1 O5 113.0(2) . . ? O6 S1 O5 109.7(2) . . ? O7 S1 C12 105.6(2) . . ? O6 S1 C12 105.1(2) . . ? O5 S1 C12 108.9(2) . . ? O7 S1 Ba1 141.51(16) . . ? O6 S1 Ba1 52.85(16) . . ? O5 S1 Ba1 57.55(15) . . ? C12 S1 Ba1 112.74(18) . . ? C2 C1 O1 126.7(5) . . ? C2 C1 H1 116.6 . . ? O1 C1 H1 116.6 . . ? C1 C2 C3 118.0(5) . . ? C1 C2 C10 121.9(5) . . ? C3 C2 C10 120.1(5) . . ? O2 C3 C4 123.5(5) . . ? O2 C3 C2 121.5(5) . . ? C4 C3 C2 115.0(5) . . ? C9 C4 C5 116.3(5) . . ? C9 C4 C3 121.5(5) . . ? C5 C4 C3 122.2(5) . . ? C6 C5 C4 120.9(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? O3 C7 C8 124.8(5) . . ? O3 C7 C6 115.8(5) . . ? C8 C7 C6 119.4(5) . . ? C9 C8 C7 118.8(5) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? O1 C9 C8 116.0(5) . . ? O1 C9 C4 120.3(5) . . ? C8 C9 C4 123.6(5) . . ? C11 C10 C15 118.7(5) . . ? C11 C10 C2 119.1(5) . . ? C15 C10 C2 122.2(5) . . ? C10 C11 C12 122.4(5) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 118.2(4) . . ? C11 C12 S1 120.4(4) . . ? C13 C12 S1 121.3(4) . . ? O4 C13 C14 122.9(5) . . ? O4 C13 C12 117.5(4) . . ? C14 C13 C12 119.6(5) . . ? C15 C14 C13 121.0(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C10 120.2(5) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.248 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.106 # Attachment '- 4 cif.txt' data_y1809 _database_code_depnum_ccdc_archive 'CCDC 865949' #TrackingRef '- 4 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Ba O28 S2' _chemical_formula_weight 1104.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2370(10) _cell_length_b 8.3220(10) _cell_length_c 37.233(7) _cell_angle_alpha 93.160(10) _cell_angle_beta 93.700(10) _cell_angle_gamma 90.820(10) _cell_volume 2234.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 15.24 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6040 _exptl_absorpt_correction_T_max 0.7973 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.71 _diffrn_reflns_number 9024 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8293 _reflns_number_gt 6226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+3.5921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8293 _refine_ls_number_parameters 648 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Ba Ba 0.36487(4) 0.70319(4) 0.762943(8) 0.03680(10) Uani 1 1 d . . . S1 S 0.75179(17) 0.85957(14) 0.84101(3) 0.0302(3) Uani 1 1 d . . . S2 S 0.78781(18) 0.92659(15) 0.65809(3) 0.0334(3) Uani 1 1 d . . . O1 O 0.8629(4) 0.9608(3) 1.04167(7) 0.0281(7) Uani 1 1 d . . . O2 O 1.0523(5) 0.5584(4) 1.11821(9) 0.0415(9) Uani 1 1 d . . . H2O H 1.0526 0.4602 1.1190 0.050 Uiso 1 1 calc R . . O3 O 0.8983(5) 0.3206(4) 1.07079(9) 0.0344(7) Uani 1 1 d . . . O4 O 0.7489(5) 0.4055(3) 1.00428(8) 0.0356(8) Uani 1 1 d . . . H4O H 0.7049 0.4475 0.9863 0.043 Uiso 1 1 calc R . . O5 O 0.6797(5) 0.6311(4) 0.96122(8) 0.0348(8) Uani 1 1 d . . . O6 O 0.5282(5) 1.1562(4) 0.84602(9) 0.0468(10) Uani 1 1 d . . . O7 O 0.5852(6) 0.7906(5) 0.82248(10) 0.0562(11) Uani 1 1 d . . . O8 O 0.8781(5) 0.7375(4) 0.85296(9) 0.0451(9) Uani 1 1 d . . . O9 O 0.8418(5) 0.9772(4) 0.82036(9) 0.0455(9) Uani 1 1 d . . . O17 O 0.6380(4) 0.9426(3) 0.45732(8) 0.0294(7) Uani 1 1 d . . . O18 O 0.4553(6) 0.5019(4) 0.37892(9) 0.0449(9) Uani 1 1 d . . . H18O H 0.4277 0.4064 0.3799 0.054 Uiso 1 1 calc R . . O19 O 0.5966(5) 0.2877(4) 0.42722(9) 0.0340(7) Uani 1 1 d . . . O20 O 0.7436(5) 0.4063(4) 0.49401(8) 0.0369(8) Uani 1 1 d . . . H20O H 0.7885 0.4570 0.5121 0.044 Uiso 1 1 calc R . . O21 O 0.8186(5) 0.6546(4) 0.53707(8) 0.0362(8) Uani 1 1 d . . . O22 O 0.9656(5) 1.2480(4) 0.65222(9) 0.0444(9) Uani 1 1 d . . . O23 O 0.6684(8) 0.7925(5) 0.64828(10) 0.0738(15) Uani 1 1 d . . . O24 O 0.6995(8) 1.0387(5) 0.68164(12) 0.0832(17) Uani 1 1 d . . . O25 O 0.9631(7) 0.8849(8) 0.67447(14) 0.103(2) Uani 1 1 d . . . C1 C 0.8747(6) 0.7992(5) 1.04688(11) 0.0248(9) Uani 1 1 d . . . C2 C 0.9561(7) 0.7598(5) 1.07975(12) 0.0307(10) Uani 1 1 d . . . H2 H 1.0025 0.8394 1.0966 0.037 Uiso 1 1 calc R . . C3 C 0.9665(6) 0.5984(5) 1.08689(12) 0.0296(10) Uani 1 1 d . . . C4 C 0.8896(6) 0.4798(5) 1.06165(11) 0.0261(9) Uani 1 1 d . . . C5 C 0.8148(6) 0.5204(5) 1.02872(11) 0.0254(9) Uani 1 1 d . . . C6 C 0.8077(6) 0.6851(5) 1.02045(11) 0.0227(9) Uani 1 1 d . . . C7 C 0.7366(6) 0.7329(5) 0.98537(11) 0.0243(9) Uani 1 1 d . . . C8 C 0.7382(6) 0.9059(5) 0.98076(11) 0.0236(9) Uani 1 1 d . . . C9 C 0.7970(6) 1.0057(5) 1.00892(11) 0.0258(9) Uani 1 1 d . . . H9 H 0.7920 1.1156 1.0056 0.031 Uiso 1 1 calc R . . C10 C 0.6798(6) 0.9725(5) 0.94587(11) 0.0236(9) Uani 1 1 d . . . C11 C 0.5841(6) 1.1167(5) 0.94392(12) 0.0283(10) Uani 1 1 d . . . H11 H 0.5521 1.1703 0.9651 0.034 Uiso 1 1 calc R . . C12 C 0.5356(7) 1.1822(6) 0.91135(12) 0.0333(11) Uani 1 1 d . . . H12 H 0.4731 1.2790 0.9110 0.040 Uiso 1 1 calc R . . C13 C 0.5794(6) 1.1044(5) 0.87948(12) 0.0303(10) Uani 1 1 d . . . C14 C 0.6806(6) 0.9622(5) 0.88070(11) 0.0264(9) Uani 1 1 d . . . C15 C 0.7285(6) 0.8983(5) 0.91361(11) 0.0239(9) Uani 1 1 d . . . H15 H 0.7949 0.8035 0.9141 0.029 Uiso 1 1 calc R . . C16 C 0.7377(8) 0.2695(6) 1.08803(14) 0.0426(12) Uani 1 1 d . . . H16B H 0.7255 0.3355 1.1097 0.051 Uiso 1 1 calc R . . H16C H 0.7505 0.1592 1.0939 0.051 Uiso 1 1 calc R . . H16A H 0.6296 0.2796 1.0720 0.051 Uiso 1 1 calc R . . C17 C 0.4518(10) 1.3122(7) 0.84431(16) 0.0658(19) Uani 1 1 d . . . H17A H 0.3372 1.3147 0.8560 0.079 Uiso 1 1 calc R . . H17B H 0.4293 1.3370 0.8196 0.079 Uiso 1 1 calc R . . H17C H 0.5371 1.3902 0.8563 0.079 Uiso 1 1 calc R . . C18 C 0.6244(6) 0.7786(5) 0.45136(11) 0.0241(9) Uani 1 1 d . . . C19 C 0.5456(6) 0.7225(5) 0.41822(11) 0.0296(10) Uani 1 1 d . . . H19 H 0.5009 0.7928 0.4013 0.036 Uiso 1 1 calc R . . C20 C 0.5359(6) 0.5582(6) 0.41127(12) 0.0308(10) Uani 1 1 d . . . C21 C 0.6079(6) 0.4515(5) 0.43621(12) 0.0284(10) Uani 1 1 d . . . C22 C 0.6804(6) 0.5102(5) 0.46948(11) 0.0272(9) Uani 1 1 d . . . C23 C 0.6893(6) 0.6786(5) 0.47795(11) 0.0234(9) Uani 1 1 d . . . C24 C 0.7601(6) 0.7430(5) 0.51327(11) 0.0257(9) Uani 1 1 d . . . C25 C 0.7613(6) 0.9188(5) 0.51818(11) 0.0238(9) Uani 1 1 d . . . C26 C 0.7014(6) 1.0050(5) 0.49005(11) 0.0283(10) Uani 1 1 d . . . H26 H 0.7041 1.1165 0.4936 0.034 Uiso 1 1 calc R . . C27 C 0.8214(6) 1.0045(5) 0.55296(11) 0.0246(9) Uani 1 1 d . . . C28 C 0.9088(6) 1.1552(5) 0.55445(12) 0.0284(10) Uani 1 1 d . . . H28 H 0.9360 1.2003 0.5331 0.034 Uiso 1 1 calc R . . C29 C 0.9564(7) 1.2398(6) 0.58702(12) 0.0329(10) Uani 1 1 d . . . H29 H 1.0127 1.3410 0.5872 0.039 Uiso 1 1 calc R . . C30 C 0.9204(6) 1.1743(5) 0.61915(12) 0.0295(10) Uani 1 1 d . . . C31 C 0.8342(6) 1.0223(5) 0.61800(11) 0.0251(9) Uani 1 1 d . . . C32 C 0.7847(6) 0.9396(5) 0.58548(11) 0.0258(9) Uani 1 1 d . . . H32 H 0.7262 0.8393 0.5853 0.031 Uiso 1 1 calc R . . C33 C 0.7592(8) 0.2299(6) 0.41065(15) 0.0451(13) Uani 1 1 d . . . H33A H 0.7788 0.2894 0.3898 0.054 Uiso 1 1 calc R . . H33B H 0.7424 0.1178 0.4035 0.054 Uiso 1 1 calc R . . H33C H 0.8648 0.2441 0.4276 0.054 Uiso 1 1 calc R . . C34 C 1.0393(10) 1.4078(7) 0.65360(16) 0.0610(18) Uani 1 1 d . . . H34A H 1.1573 1.4076 0.6432 0.073 Uiso 1 1 calc R . . H34B H 1.0543 1.4489 0.6782 0.073 Uiso 1 1 calc R . . H34C H 0.9560 1.4748 0.6403 0.073 Uiso 1 1 calc R . . O10 O 0.2135(6) 0.9615(6) 0.80099(13) 0.0654(12) Uani 1 1 d D . . H10A H 0.285(7) 1.008(9) 0.8163(14) 0.098 Uiso 1 1 d D . . H10B H 0.108(4) 0.962(9) 0.8080(17) 0.098 Uiso 1 1 d D . . O11 O 0.0056(6) 0.7345(8) 0.73810(14) 0.0832(17) Uani 1 1 d D . . H11A H -0.032(12) 0.774(10) 0.7193(14) 0.125 Uiso 1 1 d D . . H11B H -0.073(10) 0.683(10) 0.748(2) 0.125 Uiso 1 1 d D . . O12 O 0.3067(8) 0.3862(7) 0.74043(17) 0.0871(17) Uani 1 1 d D . . H12A H 0.224(9) 0.322(8) 0.744(2) 0.131 Uiso 1 1 d D . . H12B H 0.358(11) 0.353(10) 0.7225(16) 0.131 Uiso 1 1 d D . . O13 O 0.1429(6) 0.5721(5) 0.81114(12) 0.0546(10) Uani 1 1 d D . . H13A H 0.083(8) 0.488(4) 0.8124(19) 0.082 Uiso 1 1 d D . . H13B H 0.091(8) 0.646(5) 0.8219(17) 0.082 Uiso 1 1 d D . . O14 O 0.5869(9) 0.9657(7) 0.75207(12) 0.0870(17) Uani 1 1 d D . . H14A H 0.603(13) 1.024(8) 0.7354(13) 0.130 Uiso 1 1 d D . . H14B H 0.636(12) 1.008(9) 0.7708(11) 0.130 Uiso 1 1 d D . . O15 O 0.7012(7) 0.5390(6) 0.75392(13) 0.0664(12) Uani 1 1 d D . . H15A H 0.684(12) 0.495(9) 0.7337(10) 0.100 Uiso 1 1 d D . . H15B H 0.720(12) 0.517(10) 0.7752(7) 0.100 Uiso 1 1 d D . . O16 O 0.3354(8) 0.7716(9) 0.69062(14) 0.097(2) Uani 1 1 d D . . H16D H 0.430(8) 0.771(13) 0.679(2) 0.146 Uiso 1 1 d D . . H16E H 0.311(17) 0.868(4) 0.692(3) 0.146 Uiso 1 1 d D . . O26 O 0.0377(7) 0.1412(6) 0.74039(13) 0.0778(14) Uani 1 1 d . . . O27 O 0.5900(9) 0.3571(6) 0.69055(13) 0.0801(15) Uani 1 1 d D . . H27A H 0.616(13) 0.261(3) 0.688(3) 0.120 Uiso 1 1 d D . . H27B H 0.557(13) 0.416(9) 0.6744(17) 0.120 Uiso 1 1 d D . . O28 O 0.8803(9) 0.3147(7) 0.79788(18) 0.0931(17) Uani 1 1 d D . . H28A H 0.893(14) 0.299(12) 0.8195(7) 0.140 Uiso 1 1 d D . . H28B H 0.799(11) 0.253(10) 0.788(2) 0.140 Uiso 1 1 d D . . 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 Ba 0.03310(16) 0.0513(2) 0.02586(15) 0.00279(12) 0.00018(11) 0.00115(12) S1 0.0404(6) 0.0358(6) 0.0149(5) 0.0025(4) 0.0021(5) 0.0099(5) S2 0.0457(7) 0.0366(6) 0.0179(5) 0.0043(5) 0.0007(5) -0.0053(5) O1 0.0456(19) 0.0199(15) 0.0184(14) 0.0005(12) -0.0004(13) 0.0015(13) O2 0.061(2) 0.0343(18) 0.0283(17) 0.0098(15) -0.0125(16) 0.0004(18) O3 0.0419(19) 0.0260(16) 0.0368(18) 0.0125(14) 0.0043(15) 0.0056(14) O4 0.057(2) 0.0216(16) 0.0267(17) -0.0014(13) -0.0060(16) 0.0014(15) O5 0.056(2) 0.0243(16) 0.0234(16) 0.0005(13) -0.0062(15) -0.0002(15) O6 0.065(2) 0.049(2) 0.0280(18) 0.0132(16) -0.0005(17) 0.0314(19) O7 0.059(3) 0.074(3) 0.033(2) -0.0112(19) -0.0056(18) -0.004(2) O8 0.070(3) 0.043(2) 0.0240(17) 0.0021(15) 0.0094(17) 0.0290(19) O9 0.058(2) 0.045(2) 0.0377(19) 0.0171(16) 0.0186(17) 0.0142(18) O17 0.0456(19) 0.0221(15) 0.0201(15) 0.0021(12) -0.0022(14) 0.0035(14) O18 0.069(3) 0.0329(19) 0.0293(18) -0.0035(15) -0.0169(17) -0.0023(18) O19 0.0417(19) 0.0249(16) 0.0346(18) -0.0059(14) 0.0041(15) -0.0011(14) O20 0.059(2) 0.0262(17) 0.0250(16) 0.0038(13) -0.0055(16) 0.0034(16) O21 0.057(2) 0.0289(17) 0.0221(16) 0.0029(13) -0.0057(15) 0.0087(15) O22 0.066(2) 0.042(2) 0.0237(17) -0.0081(15) 0.0003(16) -0.0199(18) O23 0.132(4) 0.060(3) 0.0267(19) 0.0020(18) 0.001(2) -0.055(3) O24 0.155(5) 0.051(3) 0.050(3) 0.001(2) 0.060(3) -0.005(3) O25 0.059(3) 0.179(6) 0.081(4) 0.096(4) -0.003(3) 0.013(3) C1 0.028(2) 0.022(2) 0.024(2) 0.0008(17) 0.0021(18) 0.0044(17) C2 0.040(3) 0.031(2) 0.021(2) 0.0007(18) -0.0012(19) 0.000(2) C3 0.033(2) 0.033(2) 0.023(2) 0.0071(19) 0.0004(19) 0.003(2) C4 0.033(2) 0.024(2) 0.023(2) 0.0068(18) 0.0029(18) 0.0056(18) C5 0.030(2) 0.026(2) 0.021(2) -0.0013(17) 0.0034(18) 0.0049(18) C6 0.024(2) 0.022(2) 0.022(2) 0.0004(17) 0.0032(17) 0.0074(17) C7 0.029(2) 0.025(2) 0.019(2) -0.0002(17) 0.0043(17) 0.0036(18) C8 0.028(2) 0.024(2) 0.020(2) 0.0012(17) 0.0040(17) 0.0053(17) C9 0.035(2) 0.023(2) 0.020(2) 0.0061(17) 0.0033(18) 0.0052(18) C10 0.027(2) 0.023(2) 0.021(2) 0.0025(17) 0.0022(17) 0.0017(17) C11 0.033(2) 0.028(2) 0.024(2) -0.0032(18) 0.0045(19) 0.0089(19) C12 0.037(3) 0.031(2) 0.033(2) 0.007(2) 0.002(2) 0.015(2) C13 0.033(2) 0.032(2) 0.027(2) 0.0084(19) 0.0008(19) 0.012(2) C14 0.031(2) 0.029(2) 0.020(2) 0.0029(18) 0.0017(18) 0.0026(19) C15 0.028(2) 0.024(2) 0.020(2) 0.0023(17) -0.0003(17) 0.0048(17) C16 0.055(3) 0.033(3) 0.041(3) 0.009(2) 0.008(3) -0.004(2) C17 0.094(5) 0.062(4) 0.046(3) 0.026(3) 0.006(3) 0.041(4) C18 0.029(2) 0.023(2) 0.021(2) -0.0007(17) 0.0045(18) 0.0050(18) C19 0.036(3) 0.031(2) 0.020(2) 0.0014(18) -0.0056(19) 0.005(2) C20 0.036(3) 0.032(2) 0.023(2) -0.0048(19) -0.0031(19) 0.001(2) C21 0.035(2) 0.024(2) 0.026(2) -0.0019(18) 0.0052(19) -0.0010(19) C22 0.030(2) 0.028(2) 0.023(2) 0.0028(18) 0.0011(18) 0.0029(19) C23 0.025(2) 0.026(2) 0.019(2) -0.0004(17) 0.0036(17) 0.0012(17) C24 0.029(2) 0.027(2) 0.021(2) 0.0024(18) 0.0032(18) 0.0064(18) C25 0.028(2) 0.025(2) 0.019(2) -0.0008(17) 0.0047(17) 0.0016(18) C26 0.040(3) 0.023(2) 0.021(2) -0.0023(18) 0.0023(19) 0.0008(19) C27 0.027(2) 0.027(2) 0.019(2) -0.0003(17) 0.0029(17) 0.0018(18) C28 0.034(2) 0.030(2) 0.022(2) 0.0023(18) 0.0033(19) -0.0022(19) C29 0.040(3) 0.029(2) 0.031(2) 0.000(2) 0.007(2) -0.008(2) C30 0.035(2) 0.031(2) 0.022(2) -0.0032(19) 0.0009(19) -0.003(2) C31 0.028(2) 0.028(2) 0.019(2) 0.0015(17) 0.0021(17) 0.0012(18) C32 0.031(2) 0.025(2) 0.021(2) 0.0003(17) 0.0017(18) 0.0018(18) C33 0.061(4) 0.034(3) 0.042(3) -0.002(2) 0.012(3) 0.011(3) C34 0.088(5) 0.052(4) 0.040(3) -0.016(3) 0.000(3) -0.025(3) O10 0.045(2) 0.071(3) 0.077(3) -0.023(2) 0.004(2) 0.009(2) O11 0.043(3) 0.149(5) 0.062(3) 0.055(3) -0.010(2) -0.004(3) O12 0.082(4) 0.081(4) 0.097(4) -0.037(3) 0.031(3) -0.022(3) O13 0.067(3) 0.049(2) 0.052(2) 0.010(2) 0.026(2) 0.011(2) O14 0.113(4) 0.105(4) 0.042(3) 0.021(3) -0.007(3) -0.052(3) O15 0.052(3) 0.081(3) 0.066(3) -0.005(3) 0.003(3) 0.005(2) O16 0.062(3) 0.190(6) 0.043(3) 0.030(4) 0.010(2) -0.016(4) O26 0.101(4) 0.067(3) 0.062(3) -0.006(2) -0.003(3) -0.018(3) O27 0.118(4) 0.076(4) 0.049(3) 0.006(3) 0.015(3) 0.029(3) O28 0.098(5) 0.076(4) 0.107(5) 0.025(3) 0.004(4) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ba O7 2.705(4) . ? Ba O11 2.724(4) . ? Ba O12 2.742(5) . ? Ba O13 2.744(4) . ? Ba O14 2.757(5) . ? Ba O16 2.778(5) . ? Ba O10 2.786(4) . ? Ba O15 2.838(5) . ? S1 O7 1.445(4) . ? S1 O8 1.445(3) . ? S1 O9 1.450(4) . ? S1 C14 1.775(4) . ? S2 O23 1.419(4) . ? S2 O25 1.427(5) . ? S2 O24 1.431(4) . ? S2 C31 1.779(4) . ? O1 C9 1.355(5) . ? O1 C1 1.372(5) . ? O2 C3 1.346(5) . ? O2 H2O 0.8200 . ? O3 C4 1.387(5) . ? O3 C16 1.434(6) . ? O4 C5 1.344(5) . ? O4 H4O 0.8200 . ? O5 C7 1.247(5) . ? O6 C13 1.371(5) . ? O6 C17 1.421(6) . ? O17 C26 1.348(5) . ? O17 C18 1.372(5) . ? O18 C20 1.360(5) . ? O18 H18O 0.8200 . ? O19 C21 1.385(5) . ? O19 C33 1.440(6) . ? O20 C22 1.355(5) . ? O20 H20O 0.8200 . ? O21 C24 1.240(5) . ? O22 C30 1.363(5) . ? O22 C34 1.423(6) . ? C1 C2 1.382(6) . ? C1 C6 1.388(6) . ? C2 C3 1.386(6) . ? C2 H2 0.9300 . ? C3 C4 1.408(6) . ? C4 C5 1.369(6) . ? C5 C6 1.423(6) . ? C6 C7 1.451(6) . ? C7 C8 1.459(6) . ? C8 C9 1.344(6) . ? C8 C10 1.479(6) . ? C9 H9 0.9300 . ? C10 C15 1.388(6) . ? C10 C11 1.398(6) . ? C11 C12 1.383(6) . ? C11 H11 0.9300 . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.402(6) . ? C14 C15 1.388(6) . ? C15 H15 0.9300 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16 H16A 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.380(6) . ? C18 C23 1.391(6) . ? C19 C20 1.377(6) . ? C19 H19 0.9300 . ? C20 C21 1.401(6) . ? C21 C22 1.375(6) . ? C22 C23 1.419(6) . ? C23 C24 1.452(6) . ? C24 C25 1.465(6) . ? C25 C26 1.354(6) . ? C25 C27 1.480(6) . ? C26 H26 0.9300 . ? C27 C32 1.392(6) . ? C27 C28 1.393(6) . ? C28 C29 1.389(6) . ? C28 H28 0.9300 . ? C29 C30 1.380(6) . ? C29 H29 0.9300 . ? C30 C31 1.400(6) . ? C31 C32 1.383(6) . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? O10 H10A 0.818(10) . ? O10 H10B 0.821(11) . ? O11 H11A 0.820(10) . ? O11 H11B 0.819(11) . ? O12 H12A 0.824(11) . ? O12 H12B 0.822(10) . ? O13 H13A 0.821(11) . ? O13 H13B 0.822(10) . ? O14 H14A 0.820(11) . ? O14 H14B 0.820(11) . ? O15 H15A 0.823(10) . ? O15 H15B 0.824(10) . ? O16 H16D 0.821(11) . ? O16 H16E 0.826(11) . ? O27 H27A 0.823(10) . ? O27 H27B 0.821(10) . ? O28 H28A 0.822(10) . ? O28 H28B 0.822(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ba O11 138.44(16) . . ? O7 Ba O12 121.55(18) . . ? O11 Ba O12 83.9(2) . . ? O7 Ba O13 84.04(14) . . ? O11 Ba O13 71.91(14) . . ? O12 Ba O13 73.35(15) . . ? O7 Ba O14 68.37(14) . . ? O11 Ba O14 113.66(19) . . ? O12 Ba O14 141.42(18) . . ? O13 Ba O14 143.55(15) . . ? O7 Ba O16 137.71(17) . . ? O11 Ba O16 68.13(16) . . ? O12 Ba O16 87.1(2) . . ? O13 Ba O16 136.98(16) . . ? O14 Ba O16 70.20(17) . . ? O7 Ba O10 69.74(13) . . ? O11 Ba O10 71.21(18) . . ? O12 Ba O10 143.51(16) . . ? O13 Ba O10 73.78(14) . . ? O14 Ba O10 74.52(18) . . ? O16 Ba O10 106.81(19) . . ? O7 Ba O15 74.77(13) . . ? O11 Ba O15 146.01(18) . . ? O12 Ba O15 67.68(17) . . ? O13 Ba O15 114.40(14) . . ? O14 Ba O15 81.73(19) . . ? O16 Ba O15 91.38(17) . . ? O10 Ba O15 142.55(14) . . ? O7 S1 O8 112.1(2) . . ? O7 S1 O9 112.8(2) . . ? O8 S1 O9 112.0(2) . . ? O7 S1 C14 106.0(2) . . ? O8 S1 C14 106.07(19) . . ? O9 S1 C14 107.3(2) . . ? O23 S2 O25 113.9(4) . . ? O23 S2 O24 110.2(3) . . ? O25 S2 O24 109.5(4) . . ? O23 S2 C31 107.8(2) . . ? O25 S2 C31 106.5(2) . . ? O24 S2 C31 108.8(2) . . ? C9 O1 C1 118.0(3) . . ? C3 O2 H2O 109.5 . . ? C4 O3 C16 112.6(4) . . ? C5 O4 H4O 109.5 . . ? C13 O6 C17 117.5(4) . . ? S1 O7 Ba 153.6(2) . . ? C26 O17 C18 119.2(3) . . ? C20 O18 H18O 109.5 . . ? C21 O19 C33 112.3(4) . . ? C22 O20 H20O 109.5 . . ? C30 O22 C34 117.9(4) . . ? O1 C1 C2 115.6(4) . . ? O1 C1 C6 121.1(4) . . ? C2 C1 C6 123.2(4) . . ? C1 C2 C3 118.1(4) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? O2 C3 C2 118.5(4) . . ? O2 C3 C4 121.2(4) . . ? C2 C3 C4 120.3(4) . . ? C5 C4 O3 121.4(4) . . ? C5 C4 C3 120.9(4) . . ? O3 C4 C3 117.7(4) . . ? O4 C5 C4 120.3(4) . . ? O4 C5 C6 120.1(4) . . ? C4 C5 C6 119.6(4) . . ? C1 C6 C5 117.7(4) . . ? C1 C6 C7 120.8(4) . . ? C5 C6 C7 121.4(4) . . ? O5 C7 C6 121.3(4) . . ? O5 C7 C8 123.4(4) . . ? C6 C7 C8 115.3(4) . . ? C9 C8 C7 118.7(4) . . ? C9 C8 C10 119.8(4) . . ? C7 C8 C10 121.5(4) . . ? C8 C9 O1 125.9(4) . . ? C8 C9 H9 117.1 . . ? O1 C9 H9 117.1 . . ? C15 C10 C11 117.1(4) . . ? C15 C10 C8 120.8(4) . . ? C11 C10 C8 121.9(4) . . ? C12 C11 C10 122.0(4) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O6 C13 C12 124.1(4) . . ? O6 C13 C14 116.9(4) . . ? C12 C13 C14 119.0(4) . . ? C15 C14 C13 120.0(4) . . ? C15 C14 S1 118.2(3) . . ? C13 C14 S1 121.8(3) . . ? C14 C15 C10 121.6(4) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? O3 C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? O6 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O17 C18 C19 116.4(4) . . ? O17 C18 C23 120.0(4) . . ? C19 C18 C23 123.6(4) . . ? C20 C19 C18 117.3(4) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? O18 C20 C19 117.6(4) . . ? O18 C20 C21 120.6(4) . . ? C19 C20 C21 121.8(4) . . ? C22 C21 O19 121.4(4) . . ? C22 C21 C20 119.7(4) . . ? O19 C21 C20 118.8(4) . . ? O20 C22 C21 119.6(4) . . ? O20 C22 C23 120.4(4) . . ? C21 C22 C23 120.1(4) . . ? C18 C23 C22 117.4(4) . . ? C18 C23 C24 121.6(4) . . ? C22 C23 C24 121.0(4) . . ? O21 C24 C23 121.9(4) . . ? O21 C24 C25 123.0(4) . . ? C23 C24 C25 115.0(4) . . ? C26 C25 C24 118.5(4) . . ? C26 C25 C27 119.2(4) . . ? C24 C25 C27 122.3(4) . . ? O17 C26 C25 125.4(4) . . ? O17 C26 H26 117.3 . . ? C25 C26 H26 117.3 . . ? C32 C27 C28 117.6(4) . . ? C32 C27 C25 120.7(4) . . ? C28 C27 C25 121.6(4) . . ? C29 C28 C27 121.8(4) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? O22 C30 C29 123.9(4) . . ? O22 C30 C31 117.6(4) . . ? C29 C30 C31 118.5(4) . . ? C32 C31 C30 121.0(4) . . ? C32 C31 S2 117.4(3) . . ? C30 C31 S2 121.5(3) . . ? C31 C32 C27 120.8(4) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? O19 C33 H33A 109.5 . . ? O19 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O19 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O22 C34 H34A 109.5 . . ? O22 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O22 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Ba O10 H10A 115(5) . . ? Ba O10 H10B 124(5) . . ? H10A O10 H10B 110(6) . . ? Ba O11 H11A 127(7) . . ? Ba O11 H11B 117(7) . . ? H11A O11 H11B 115(9) . . ? Ba O12 H12A 131(6) . . ? Ba O12 H12B 117(6) . . ? H12A O12 H12B 108(8) . . ? Ba O13 H13A 137(4) . . ? Ba O13 H13B 108(4) . . ? H13A O13 H13B 109(6) . . ? Ba O14 H14A 136(6) . . ? Ba O14 H14B 113(5) . . ? H14A O14 H14B 109(7) . . ? Ba O15 H15A 103(6) . . ? Ba O15 H15B 96(6) . . ? H15A O15 H15B 141(9) . . ? Ba O16 H16D 119(8) . . ? Ba O16 H16E 100(8) . . ? H16D O16 H16E 102(10) . . ? H27A O27 H27B 126(9) . . ? H28A O28 H28B 110(9) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 S1 O7 Ba -101.9(6) . . . . ? O9 S1 O7 Ba 25.6(7) . . . . ? C14 S1 O7 Ba 142.8(5) . . . . ? O11 Ba O7 S1 -130.9(5) . . . . ? O12 Ba O7 S1 108.8(6) . . . . ? O13 Ba O7 S1 175.1(6) . . . . ? O14 Ba O7 S1 -29.2(6) . . . . ? O16 Ba O7 S1 -17.0(7) . . . . ? O10 Ba O7 S1 -110.0(6) . . . . ? O15 Ba O7 S1 57.8(6) . . . . ? C9 O1 C1 C2 175.2(4) . . . . ? C9 O1 C1 C6 -5.0(6) . . . . ? O1 C1 C2 C3 178.1(4) . . . . ? C6 C1 C2 C3 -1.8(7) . . . . ? C1 C2 C3 O2 177.3(4) . . . . ? C1 C2 C3 C4 -2.3(7) . . . . ? C16 O3 C4 C5 -90.6(5) . . . . ? C16 O3 C4 C3 91.7(5) . . . . ? O2 C3 C4 C5 -175.1(4) . . . . ? C2 C3 C4 C5 4.5(7) . . . . ? O2 C3 C4 O3 2.6(7) . . . . ? C2 C3 C4 O3 -177.7(4) . . . . ? O3 C4 C5 O4 -0.4(7) . . . . ? C3 C4 C5 O4 177.2(4) . . . . ? O3 C4 C5 C6 179.7(4) . . . . ? C3 C4 C5 C6 -2.6(7) . . . . ? O1 C1 C6 C5 -176.3(4) . . . . ? C2 C1 C6 C5 3.6(7) . . . . ? O1 C1 C6 C7 5.0(6) . . . . ? C2 C1 C6 C7 -175.2(4) . . . . ? O4 C5 C6 C1 178.9(4) . . . . ? C4 C5 C6 C1 -1.3(6) . . . . ? O4 C5 C6 C7 -2.4(6) . . . . ? C4 C5 C6 C7 177.4(4) . . . . ? C1 C6 C7 O5 178.5(4) . . . . ? C5 C6 C7 O5 -0.2(7) . . . . ? C1 C6 C7 C8 -1.2(6) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? O5 C7 C8 C9 177.9(4) . . . . ? C6 C7 C8 C9 -2.4(6) . . . . ? O5 C7 C8 C10 -3.1(7) . . . . ? C6 C7 C8 C10 176.6(4) . . . . ? C7 C8 C9 O1 2.5(7) . . . . ? C10 C8 C9 O1 -176.5(4) . . . . ? C1 O1 C9 C8 1.2(6) . . . . ? C9 C8 C10 C15 138.9(5) . . . . ? C7 C8 C10 C15 -40.1(6) . . . . ? C9 C8 C10 C11 -37.1(6) . . . . ? C7 C8 C10 C11 143.9(4) . . . . ? C15 C10 C11 C12 1.4(7) . . . . ? C8 C10 C11 C12 177.5(4) . . . . ? C10 C11 C12 C13 0.7(7) . . . . ? C17 O6 C13 C12 10.5(8) . . . . ? C17 O6 C13 C14 -170.3(5) . . . . ? C11 C12 C13 O6 176.4(5) . . . . ? C11 C12 C13 C14 -2.7(7) . . . . ? O6 C13 C14 C15 -176.6(4) . . . . ? C12 C13 C14 C15 2.6(7) . . . . ? O6 C13 C14 S1 3.7(6) . . . . ? C12 C13 C14 S1 -177.1(4) . . . . ? O7 S1 C14 C15 109.7(4) . . . . ? O8 S1 C14 C15 -9.6(4) . . . . ? O9 S1 C14 C15 -129.4(4) . . . . ? O7 S1 C14 C13 -70.5(4) . . . . ? O8 S1 C14 C13 170.2(4) . . . . ? O9 S1 C14 C13 50.3(4) . . . . ? C13 C14 C15 C10 -0.5(7) . . . . ? S1 C14 C15 C10 179.3(3) . . . . ? C11 C10 C15 C14 -1.5(7) . . . . ? C8 C10 C15 C14 -177.7(4) . . . . ? C26 O17 C18 C19 175.3(4) . . . . ? C26 O17 C18 C23 -5.1(6) . . . . ? O17 C18 C19 C20 178.0(4) . . . . ? C23 C18 C19 C20 -1.6(7) . . . . ? C18 C19 C20 O18 178.8(4) . . . . ? C18 C19 C20 C21 -2.0(7) . . . . ? C33 O19 C21 C22 -90.7(5) . . . . ? C33 O19 C21 C20 92.2(5) . . . . ? O18 C20 C21 C22 -176.8(4) . . . . ? C19 C20 C21 C22 4.0(7) . . . . ? O18 C20 C21 O19 0.5(7) . . . . ? C19 C20 C21 O19 -178.8(4) . . . . ? O19 C21 C22 O20 0.4(7) . . . . ? C20 C21 C22 O20 177.6(4) . . . . ? O19 C21 C22 C23 -179.7(4) . . . . ? C20 C21 C22 C23 -2.6(7) . . . . ? O17 C18 C23 C22 -176.7(4) . . . . ? C19 C18 C23 C22 2.9(7) . . . . ? O17 C18 C23 C24 4.5(6) . . . . ? C19 C18 C23 C24 -175.9(4) . . . . ? O20 C22 C23 C18 179.1(4) . . . . ? C21 C22 C23 C18 -0.7(6) . . . . ? O20 C22 C23 C24 -2.0(6) . . . . ? C21 C22 C23 C24 178.1(4) . . . . ? C18 C23 C24 O21 -179.8(4) . . . . ? C22 C23 C24 O21 1.4(7) . . . . ? C18 C23 C24 C25 -1.3(6) . . . . ? C22 C23 C24 C25 179.9(4) . . . . ? O21 C24 C25 C26 177.3(4) . . . . ? C23 C24 C25 C26 -1.2(6) . . . . ? O21 C24 C25 C27 -4.1(7) . . . . ? C23 C24 C25 C27 177.3(4) . . . . ? C18 O17 C26 C25 2.7(7) . . . . ? C24 C25 C26 O17 0.5(7) . . . . ? C27 C25 C26 O17 -178.0(4) . . . . ? C26 C25 C27 C32 143.3(4) . . . . ? C24 C25 C27 C32 -35.2(6) . . . . ? C26 C25 C27 C28 -33.8(6) . . . . ? C24 C25 C27 C28 147.7(4) . . . . ? C32 C27 C28 C29 -0.8(7) . . . . ? C25 C27 C28 C29 176.4(4) . . . . ? C27 C28 C29 C30 1.1(7) . . . . ? C34 O22 C30 C29 5.8(8) . . . . ? C34 O22 C30 C31 -174.9(5) . . . . ? C28 C29 C30 O22 178.8(4) . . . . ? C28 C29 C30 C31 -0.5(7) . . . . ? O22 C30 C31 C32 -179.8(4) . . . . ? C29 C30 C31 C32 -0.5(7) . . . . ? O22 C30 C31 S2 -0.9(6) . . . . ? C29 C30 C31 S2 178.4(4) . . . . ? O23 S2 C31 C32 -12.7(5) . . . . ? O25 S2 C31 C32 109.9(5) . . . . ? O24 S2 C31 C32 -132.2(4) . . . . ? O23 S2 C31 C30 168.4(4) . . . . ? O25 S2 C31 C30 -69.0(5) . . . . ? O24 S2 C31 C30 48.9(5) . . . . ? C30 C31 C32 C27 0.8(7) . . . . ? S2 C31 C32 C27 -178.1(3) . . . . ? C28 C27 C32 C31 -0.2(6) . . . . ? C25 C27 C32 C31 -177.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.846 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.102