# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Maochun Hong' _publ_contact_author_email hmc@fjirsm.ac.cn _publ_section_title ; 2D Sheet-like architectures constructed from main group metal ions, 4,4'-bpno and 1,2-alternate p-sulfonatothiacalix[4]arene ; _publ_author_name 'Maochun Hong' # Attachment '- 1 & 2.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 817407' #TrackingRef '- 1 & 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N2 O15 Pb S4' _chemical_formula_weight 891.86 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' N N 0.0061 0.0033 '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' Pb Pb -3.3944 10.1111 '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' H H 0.0000 0.0000 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.729(3) _cell_length_b 11.682(4) _cell_length_c 15.591(5) _cell_angle_alpha 98.598(4) _cell_angle_beta 90.922(2) _cell_angle_gamma 110.883(4) _cell_volume 1464.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4560 _cell_measurement_theta_min 2.1220 _cell_measurement_theta_max 27.4816 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 6.121 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3740 _exptl_absorpt_correction_T_max 0.5796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Saturn724+ _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12672 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6632 _reflns_number_gt 5595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0429P)^2^+4.5348P] 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 6632 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Pb1 Pb 0.26616(3) -0.01380(3) 0.443179(16) 0.04596(10) Uani 1 1 d . . . S1 S 0.5312(2) 0.13918(16) -0.05601(11) 0.0441(4) Uani 1 1 d . . . S2 S 0.6882(2) 0.54374(15) 0.21001(10) 0.0386(3) Uani 1 1 d . . . S3 S 0.22422(19) 0.09461(16) 0.24295(10) 0.0379(3) Uani 1 1 d . . . S4 S 0.1870(2) 0.67451(18) 0.33863(11) 0.0512(5) Uani 1 1 d . . . O1 O 0.6998(7) 0.4030(5) 0.0287(3) 0.0477(12) Uani 1 1 d . . . H1 H 0.761(11) 0.471(9) 0.052(5) 0.07(3) Uiso 1 1 d . . . O2 O 0.6855(6) 0.7230(5) 0.0833(3) 0.0491(12) Uani 1 1 d . . . H2 H 0.758(9) 0.679(7) 0.091(5) 0.05(2) Uiso 1 1 d . . . O3 O 0.3225(6) 0.0486(6) 0.2944(4) 0.0655(16) Uani 1 1 d . . . O4 O 0.1033(6) -0.0028(5) 0.1831(3) 0.0575(14) Uani 1 1 d . . . O5 O 0.1542(7) 0.1722(5) 0.2975(4) 0.0658(16) Uani 1 1 d . . . O6 O 0.1034(12) 0.5534(6) 0.3502(5) 0.128(4) Uani 1 1 d . . . O7 O 0.0712(10) 0.7281(11) 0.3103(6) 0.133(4) Uani 1 1 d . . . O8 O 0.2843(8) 0.7568(7) 0.4107(4) 0.093(3) Uani 1 1 d . . . O9 O 0.5634(5) 0.0374(5) 0.4325(3) 0.0432(11) Uani 1 1 d . . . O10 O 1.0846(5) 0.3675(4) -0.0635(3) 0.0417(10) Uani 1 1 d . . . O11 O 0.3886(10) 0.2036(8) 0.5257(5) 0.107(3) Uani 1 1 d . . . O12 O 0.0126(12) -0.1051(16) 0.5544(7) 0.213(8) Uani 1 1 d . . . N1 N 0.6463(6) 0.0849(5) 0.3652(3) 0.0377(12) Uani 1 1 d . . . N2 N 1.0334(6) 0.3244(5) 0.0098(3) 0.0349(11) Uani 1 1 d . . . C1 C 0.5890(7) 0.3384(6) 0.0790(4) 0.0330(12) Uani 1 1 d . . . C2 C 0.4976(8) 0.2147(6) 0.0455(4) 0.0347(13) Uani 1 1 d . . . C3 C 0.3821(7) 0.1417(6) 0.0947(4) 0.0347(13) Uani 1 1 d . . . H3 H 0.3186 0.0600 0.0712 0.042 Uiso 1 1 calc R . . C4 C 0.3613(7) 0.1904(6) 0.1785(4) 0.0337(13) Uani 1 1 d . . . C5 C 0.4528(7) 0.3134(6) 0.2130(4) 0.0347(13) Uani 1 1 d . . . H5 H 0.4386 0.3458 0.2693 0.042 Uiso 1 1 calc R . . C6 C 0.5660(8) 0.3889(6) 0.1636(4) 0.0341(13) Uani 1 1 d . . . C7 C 0.5479(7) 0.6216(5) 0.2009(4) 0.0330(12) Uani 1 1 d . . . C8 C 0.4290(8) 0.6133(6) 0.2597(4) 0.0413(15) Uani 1 1 d . . . H8 H 0.4212 0.5652 0.3030 0.050 Uiso 1 1 calc R . . C9 C 0.3216(8) 0.6754(6) 0.2550(4) 0.0429(16) Uani 1 1 d . . . C10 C 0.3304(8) 0.7465(6) 0.1897(4) 0.0411(15) Uani 1 1 d . . . H10 H 0.2553 0.7856 0.1848 0.049 Uiso 1 1 calc R . . C11 C 0.4525(8) 0.7583(6) 0.1317(4) 0.0362(13) Uani 1 1 d . . . C12 C 0.5646(8) 0.6998(6) 0.1385(4) 0.0362(13) Uani 1 1 d . . . C13 C 0.7025(9) 0.2077(7) 0.3669(4) 0.0479(17) Uani 1 1 d . . . H13 H 0.6840 0.2600 0.4133 0.058 Uiso 1 1 calc R . . C14 C 0.7881(9) 0.2561(7) 0.2990(4) 0.0480(17) Uani 1 1 d . . . H14 H 0.8284 0.3416 0.3002 0.058 Uiso 1 1 calc R . . C15 C 0.8146(7) 0.1794(6) 0.2292(4) 0.0351(13) Uani 1 1 d . . . C16 C 0.9008(8) 0.2300(6) 0.1549(4) 0.0373(13) Uani 1 1 d . . . C17 C 0.9883(8) 0.3558(6) 0.1585(4) 0.0429(16) Uani 1 1 d . . . H17 H 1.0028 0.4102 0.2106 0.052 Uiso 1 1 calc R . . C18 C 1.0542(9) 0.4004(6) 0.0849(4) 0.0477(17) Uani 1 1 d . . . H18 H 1.1139 0.4848 0.0881 0.057 Uiso 1 1 calc R . . C19 C 0.9585(9) 0.2023(7) 0.0049(4) 0.0488(17) Uani 1 1 d . . . H19 H 0.9517 0.1495 -0.0471 0.059 Uiso 1 1 calc R . . C20 C 0.8914(9) 0.1540(7) 0.0767(4) 0.0507(18) Uani 1 1 d . . . H20 H 0.8387 0.0686 0.0726 0.061 Uiso 1 1 calc R . . C21 C 0.7539(9) 0.0543(6) 0.2307(4) 0.0461(17) Uani 1 1 d . . . H21 H 0.7705 0.0000 0.1850 0.055 Uiso 1 1 calc R . . C22 C 0.6679(9) 0.0080(7) 0.2994(4) 0.0466(17) Uani 1 1 d . . . H22 H 0.6253 -0.0772 0.2993 0.056 Uiso 1 1 calc R . . O13 O -0.0985(17) -0.1379(12) 0.3085(12) 0.220(7) Uani 1 1 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 Pb1 0.04208(16) 0.05777(19) 0.03543(15) 0.01334(11) 0.00802(10) 0.01255(12) S1 0.0640(11) 0.0366(9) 0.0377(8) 0.0111(7) 0.0196(8) 0.0227(8) S2 0.0409(8) 0.0361(8) 0.0322(7) 0.0102(6) 0.0017(6) 0.0044(7) S3 0.0366(8) 0.0433(9) 0.0313(7) 0.0161(7) 0.0077(6) 0.0074(7) S4 0.0531(10) 0.0474(10) 0.0389(9) 0.0014(7) 0.0229(8) 0.0026(8) O1 0.056(3) 0.040(3) 0.038(2) 0.013(2) 0.020(2) 0.003(2) O2 0.055(3) 0.061(3) 0.044(3) 0.030(2) 0.026(2) 0.027(3) O3 0.051(3) 0.089(4) 0.066(3) 0.056(3) 0.012(3) 0.019(3) O4 0.055(3) 0.050(3) 0.044(3) 0.008(2) 0.008(2) -0.009(2) O5 0.058(3) 0.066(4) 0.066(3) 0.008(3) 0.037(3) 0.013(3) O6 0.182(8) 0.047(4) 0.112(6) -0.001(4) 0.111(6) -0.009(4) O7 0.097(6) 0.245(12) 0.105(6) 0.072(7) 0.060(5) 0.100(7) O8 0.068(4) 0.124(6) 0.049(3) -0.038(4) 0.017(3) 0.008(4) O9 0.035(2) 0.063(3) 0.032(2) 0.023(2) 0.0149(18) 0.012(2) O10 0.038(2) 0.047(3) 0.038(2) 0.022(2) 0.0130(18) 0.007(2) O11 0.111(6) 0.091(6) 0.115(6) -0.031(5) -0.026(5) 0.053(5) O12 0.094(6) 0.46(2) 0.130(8) 0.192(12) 0.047(6) 0.100(10) N1 0.036(3) 0.052(3) 0.027(2) 0.018(2) 0.010(2) 0.014(2) N2 0.031(3) 0.041(3) 0.028(2) 0.015(2) 0.0073(19) 0.003(2) C1 0.034(3) 0.034(3) 0.031(3) 0.013(2) 0.006(2) 0.009(3) C2 0.047(4) 0.034(3) 0.025(3) 0.007(2) 0.009(2) 0.015(3) C3 0.037(3) 0.028(3) 0.037(3) 0.016(2) 0.006(2) 0.005(2) C4 0.039(3) 0.038(3) 0.030(3) 0.018(3) 0.008(2) 0.015(3) C5 0.039(3) 0.032(3) 0.033(3) 0.010(2) 0.009(2) 0.011(3) C6 0.043(3) 0.030(3) 0.031(3) 0.012(2) 0.007(2) 0.012(3) C7 0.041(3) 0.024(3) 0.028(3) 0.004(2) 0.007(2) 0.004(2) C8 0.056(4) 0.033(3) 0.024(3) 0.003(2) 0.011(3) 0.004(3) C9 0.050(4) 0.035(3) 0.032(3) 0.001(3) 0.021(3) 0.002(3) C10 0.048(4) 0.034(3) 0.037(3) -0.002(3) 0.011(3) 0.012(3) C11 0.044(3) 0.030(3) 0.028(3) 0.003(2) 0.014(3) 0.006(3) C12 0.043(3) 0.036(3) 0.025(3) 0.007(2) 0.011(2) 0.008(3) C13 0.060(4) 0.047(4) 0.039(4) 0.016(3) 0.023(3) 0.019(3) C14 0.056(4) 0.043(4) 0.046(4) 0.018(3) 0.018(3) 0.014(3) C15 0.030(3) 0.042(3) 0.027(3) 0.013(3) 0.005(2) 0.002(3) C16 0.039(3) 0.039(3) 0.029(3) 0.009(3) 0.005(2) 0.007(3) C17 0.053(4) 0.034(3) 0.030(3) 0.006(3) 0.011(3) 0.000(3) C18 0.058(4) 0.032(3) 0.046(4) 0.017(3) 0.018(3) 0.005(3) C19 0.057(4) 0.040(4) 0.037(3) 0.008(3) 0.016(3) 0.002(3) C20 0.057(4) 0.045(4) 0.037(3) 0.009(3) 0.016(3) 0.001(3) C21 0.053(4) 0.039(4) 0.033(3) 0.006(3) 0.017(3) 0.000(3) C22 0.053(4) 0.044(4) 0.033(3) 0.013(3) 0.014(3) 0.003(3) O13 0.181(12) 0.143(11) 0.38(2) 0.134(13) 0.132(14) 0.066(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 Pb1 O9 2.460(4) . ? Pb1 O11 2.509(7) . ? Pb1 O9 2.532(4) 2_656 ? Pb1 O3 2.537(5) . ? Pb1 O8 2.713(8) 1_545 ? Pb1 O12 2.835(8) . ? S1 C2 1.776(6) . ? S1 C11 1.776(6) 2_665 ? S2 C6 1.772(6) . ? S2 C7 1.782(7) . ? S3 O4 1.440(5) . ? S3 O5 1.448(6) . ? S3 O3 1.451(5) . ? S3 C4 1.764(6) . ? S4 O6 1.382(6) . ? S4 O8 1.405(6) . ? S4 O7 1.459(9) . ? S4 C9 1.767(6) . ? O1 C1 1.343(7) . ? O1 H1 0.81(9) . ? O2 C12 1.351(7) . ? O2 H2 0.96(8) . ? O8 Pb1 2.713(8) 1_565 ? O9 N1 1.358(6) . ? O9 Pb1 2.532(4) 2_656 ? O10 N2 1.337(6) . ? N1 C22 1.320(9) . ? N1 C13 1.337(9) . ? N2 C18 1.327(9) . ? N2 C19 1.331(8) . ? C1 C2 1.392(8) . ? C1 C6 1.410(8) . ? C2 C3 1.392(8) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.390(9) . ? C5 C6 1.398(8) . ? C5 H5 0.9300 . ? C7 C8 1.383(8) . ? C7 C12 1.406(8) . ? C8 C9 1.381(10) . ? C8 H8 0.9300 . ? C9 C10 1.395(9) . ? C10 C11 1.391(8) . ? C10 H10 0.9300 . ? C11 C12 1.390(9) . ? C11 S1 1.776(6) 2_665 ? C13 C14 1.379(9) . ? C13 H13 0.9300 . ? C14 C15 1.380(9) . ? C14 H14 0.9300 . ? C15 C21 1.369(9) . ? C15 C16 1.475(7) . ? C16 C20 1.378(9) . ? C16 C17 1.385(9) . ? C17 C18 1.380(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.375(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.383(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? 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 O9 Pb1 O11 76.9(2) . . ? O9 Pb1 O9 60.67(15) . 2_656 ? O11 Pb1 O9 77.3(2) . 2_656 ? O9 Pb1 O3 74.72(15) . . ? O11 Pb1 O3 95.1(3) . . ? O9 Pb1 O3 135.36(15) 2_656 . ? O9 Pb1 O8 78.45(18) . 1_545 ? O11 Pb1 O8 146.8(2) . 1_545 ? O9 Pb1 O8 71.37(18) 2_656 1_545 ? O3 Pb1 O8 99.5(2) . 1_545 ? O9 Pb1 O12 141.7(2) . . ? O11 Pb1 O12 97.0(4) . . ? O9 Pb1 O12 81.0(2) 2_656 . ? O3 Pb1 O12 143.5(2) . . ? O8 Pb1 O12 88.8(4) 1_545 . ? C2 S1 C11 106.8(3) . 2_665 ? C6 S2 C7 101.6(3) . . ? O4 S3 O5 112.8(3) . . ? O4 S3 O3 112.8(4) . . ? O5 S3 O3 111.4(4) . . ? O4 S3 C4 106.1(3) . . ? O5 S3 C4 107.0(3) . . ? O3 S3 C4 106.1(3) . . ? O6 S4 O8 116.8(5) . . ? O6 S4 O7 109.9(6) . . ? O8 S4 O7 107.4(6) . . ? O6 S4 C9 109.3(4) . . ? O8 S4 C9 105.9(3) . . ? O7 S4 C9 107.0(4) . . ? C1 O1 H1 115(6) . . ? C12 O2 H2 113(4) . . ? S3 O3 Pb1 126.9(3) . . ? S4 O8 Pb1 116.9(5) . 1_565 ? N1 O9 Pb1 124.1(3) . . ? N1 O9 Pb1 116.5(3) . 2_656 ? Pb1 O9 Pb1 119.33(15) . 2_656 ? C22 N1 C13 121.8(5) . . ? C22 N1 O9 118.9(5) . . ? C13 N1 O9 119.2(5) . . ? C18 N2 C19 120.7(5) . . ? C18 N2 O10 121.5(5) . . ? C19 N2 O10 117.8(5) . . ? O1 C1 C2 117.1(5) . . ? O1 C1 C6 123.2(6) . . ? C2 C1 C6 119.7(5) . . ? C1 C2 C3 120.2(5) . . ? C1 C2 S1 122.8(4) . . ? C3 C2 S1 116.8(5) . . ? C4 C3 C2 120.3(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 S3 120.1(5) . . ? C5 C4 S3 119.8(4) . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.4(6) . . ? C5 C6 S2 119.9(5) . . ? C1 C6 S2 120.6(4) . . ? C8 C7 C12 119.1(6) . . ? C8 C7 S2 120.1(5) . . ? C12 C7 S2 120.6(5) . . ? C9 C8 C7 121.0(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.1(6) . . ? C8 C9 S4 118.8(5) . . ? C10 C9 S4 120.8(6) . . ? C11 C10 C9 119.3(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 120.5(6) . . ? C12 C11 S1 122.0(4) . 2_665 ? C10 C11 S1 117.2(5) . 2_665 ? O2 C12 C11 116.5(5) . . ? O2 C12 C7 123.8(6) . . ? C11 C12 C7 119.7(5) . . ? N1 C13 C14 119.3(6) . . ? N1 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 120.9(7) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C21 C15 C14 117.4(5) . . ? C21 C15 C16 121.4(6) . . ? C14 C15 C16 121.2(6) . . ? C20 C16 C17 116.8(6) . . ? C20 C16 C15 121.0(6) . . ? C17 C16 C15 122.1(6) . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N2 C18 C17 120.9(6) . . ? N2 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? N2 C19 C20 120.1(6) . . ? N2 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C16 121.2(7) . . ? C19 C20 H20 119.4 . . ? C16 C20 H20 119.4 . . ? C15 C21 C22 120.6(6) . . ? C15 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? N1 C22 C21 120.0(6) . . ? N1 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O10 0.81(9) 1.87(9) 2.638(7) 159(8) 2_765 O2 H2 O10 0.96(8) 1.69(8) 2.584(7) 154(7) 2_765 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.123 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.144 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.486 0.500 0.500 154.2 38.8 _platon_squeeze_details ; ? ; ###END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 817408' #TrackingRef '- 1 & 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Ba N2 O15 S4' _chemical_formula_weight 822.01 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3202(2) _cell_length_b 11.3884(2) _cell_length_c 15.0678(5) _cell_angle_alpha 77.526(12) _cell_angle_beta 83.585(13) _cell_angle_gamma 69.775(10) _cell_volume 1464.09(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2461 _cell_measurement_theta_min 2.1597 _cell_measurement_theta_max 27.4294 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.717 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6734 _exptl_absorpt_correction_T_max 0.7827 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12587 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6683 _reflns_number_gt 5569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0523P)^2^+0.7420P] 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 6683 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.26408(3) 0.23061(3) 0.457093(17) 0.03470(10) Uani 1 1 d . . . S1 S 0.41943(11) 0.68820(10) -0.03849(7) 0.0313(2) Uani 1 1 d . . . O1 O 0.2879(4) 0.9194(3) 0.0469(2) 0.0376(7) Uani 1 1 d . . . H1 H 0.256(5) 0.980(5) 0.066(3) 0.032(14) Uiso 1 1 d . . . N1 N 0.5645(5) 0.3717(5) 0.3790(3) 0.0486(11) Uani 1 1 d . . . C1 C 0.2489(4) 0.8204(4) 0.0958(3) 0.0267(8) Uani 1 1 d . . . S2 S 0.09055(10) 0.96974(9) 0.22032(6) 0.0260(2) Uani 1 1 d . . . O2 O -0.0911(3) 1.2014(3) 0.0807(2) 0.0360(7) Uani 1 1 d . . . H2 H 0.000(7) 1.173(6) 0.095(4) 0.062(18) Uiso 1 1 d . . . N2 N 0.7639(4) 0.7667(3) -0.0028(2) 0.0326(8) Uani 1 1 d . . . C2 C 0.3025(4) 0.7058(4) 0.0624(3) 0.0265(8) Uani 1 1 d . . . S3 S 0.15479(14) 0.46463(11) 0.25678(7) 0.0377(3) Uani 1 1 d . . . O3 O 0.0841(6) 0.4903(4) 0.3427(3) 0.0835(15) Uani 1 1 d . . . C3 C 0.2715(4) 0.5998(4) 0.1120(3) 0.0292(8) Uani 1 1 d . . . H3 H 0.3081 0.5239 0.0903 0.035 Uiso 1 1 calc R . . S4 S -0.47659(11) 0.94785(10) 0.32781(7) 0.0296(2) Uani 1 1 d . . . O4 O 0.3085(5) 0.3664(4) 0.2735(3) 0.0718(13) Uani 1 1 d . . . C4 C 0.1864(4) 0.6043(4) 0.1942(3) 0.0286(8) Uani 1 1 d . . . O5 O 0.0712(4) 0.4266(4) 0.2014(2) 0.0542(9) Uani 1 1 d . . . C5 C 0.1298(4) 0.7168(4) 0.2251(3) 0.0295(8) Uani 1 1 d . . . H5 H 0.0715 0.7204 0.2794 0.035 Uiso 1 1 calc R . . O6 O -0.3786(3) 0.8225(3) 0.3690(2) 0.0467(8) Uani 1 1 d . . . C6 C 0.1583(4) 0.8264(4) 0.1763(3) 0.0263(8) Uani 1 1 d . . . O7 O -0.6005(4) 0.9429(4) 0.2818(2) 0.0528(10) Uani 1 1 d . . . C7 C -0.1098(4) 1.0262(4) 0.2005(3) 0.0252(8) Uani 1 1 d . . . O8 O -0.5244(5) 1.0287(4) 0.3951(3) 0.0636(11) Uani 1 1 d . . . C8 C -0.2046(4) 0.9685(4) 0.2570(3) 0.0270(8) Uani 1 1 d . . . H8 H -0.1625 0.8987 0.3025 0.032 Uiso 1 1 calc R . . O9 O 0.5216(5) 0.2971(4) 0.4514(2) 0.0646(12) Uani 1 1 d . . . C9 C -0.3609(4) 1.0139(4) 0.2461(3) 0.0268(8) Uani 1 1 d . . . O10 O 0.7930(3) 0.8430(3) -0.0786(2) 0.0361(7) Uani 1 1 d . . . C10 C -0.4233(4) 1.1161(4) 0.1768(3) 0.0273(8) Uani 1 1 d . . . H10 H -0.5280 1.1451 0.1683 0.033 Uiso 1 1 calc R . . O11 O 0.2086(5) 0.4396(4) 0.5538(3) 0.0683(12) Uani 1 1 d . . . C11 C -0.3303(4) 1.1754(4) 0.1201(3) 0.0258(8) Uani 1 1 d . . . O12 O 0.1707(8) 0.0156(5) 0.5305(4) 0.108(2) Uani 1 1 d . . . C12 C -0.1725(4) 1.1333(4) 0.1332(2) 0.0242(8) Uani 1 1 d . . . O13 O -0.0237(4) 0.3030(4) 0.5402(3) 0.0649(11) Uani 1 1 d . . . C13 C 0.4888(6) 0.4976(6) 0.3636(3) 0.0494(13) Uani 1 1 d . . . H13 H 0.4085 0.5324 0.4029 0.059 Uiso 1 1 calc R . . O14 O 0.1185(5) 0.1811(4) 0.3198(3) 0.0692(12) Uani 1 1 d . . . C14 C 0.5306(5) 0.5740(5) 0.2899(3) 0.0446(11) Uani 1 1 d . . . H14 H 0.4775 0.6612 0.2794 0.054 Uiso 1 1 calc R . . O15 O 0.7488(5) 0.1928(5) 0.5666(3) 0.0822(15) Uani 1 1 d . . . C15 C 0.6500(5) 0.5250(4) 0.2307(3) 0.0340(9) Uani 1 1 d . . . C16 C 0.6945(5) 0.6081(4) 0.1497(3) 0.0328(9) Uani 1 1 d . . . C17 C 0.6488(7) 0.7392(5) 0.1432(3) 0.0511(13) Uani 1 1 d . . . H17 H 0.5930 0.7753 0.1915 0.061 Uiso 1 1 calc R . . C18 C 0.6839(6) 0.8161(5) 0.0679(3) 0.0494(13) Uani 1 1 d . . . H18 H 0.6521 0.9037 0.0654 0.059 Uiso 1 1 calc R . . C19 C 0.8123(5) 0.6404(4) 0.0003(3) 0.0325(9) Uani 1 1 d . . . H19 H 0.8688 0.6072 -0.0488 0.039 Uiso 1 1 calc R . . C20 C 0.7787(5) 0.5594(4) 0.0758(3) 0.0350(9) Uani 1 1 d . . . H20 H 0.8126 0.4720 0.0773 0.042 Uiso 1 1 calc R . . C21 C 0.7258(6) 0.3953(5) 0.2492(3) 0.0502(12) Uani 1 1 d . . . H21 H 0.8077 0.3585 0.2115 0.060 Uiso 1 1 calc R . . C22 C 0.6795(7) 0.3204(6) 0.3239(4) 0.0577(14) Uani 1 1 d . . . H22 H 0.7299 0.2328 0.3357 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.03713(16) 0.03908(17) 0.03026(15) -0.00636(11) 0.00503(10) -0.01768(12) S1 0.0258(5) 0.0294(5) 0.0259(5) 0.0040(4) 0.0051(4) -0.0006(4) O1 0.0475(19) 0.0244(17) 0.0372(18) -0.0009(14) 0.0130(14) -0.0147(14) N1 0.051(2) 0.072(3) 0.033(2) 0.014(2) -0.0095(18) -0.046(2) C1 0.0224(18) 0.025(2) 0.029(2) 0.0017(16) -0.0016(14) -0.0072(15) S2 0.0218(4) 0.0289(5) 0.0273(5) -0.0039(4) -0.0026(3) -0.0088(4) O2 0.0241(15) 0.0361(17) 0.0416(17) 0.0078(13) 0.0028(12) -0.0127(13) N2 0.0328(18) 0.034(2) 0.0324(19) -0.0007(15) 0.0002(14) -0.0167(15) C2 0.0256(18) 0.026(2) 0.0225(19) -0.0011(15) 0.0038(14) -0.0063(15) S3 0.0561(7) 0.0371(6) 0.0255(5) 0.0018(4) -0.0006(4) -0.0273(5) O3 0.156(5) 0.067(3) 0.045(2) -0.016(2) 0.041(3) -0.069(3) C3 0.034(2) 0.022(2) 0.027(2) 0.0013(16) 0.0010(15) -0.0072(16) S4 0.0254(5) 0.0358(6) 0.0244(5) 0.0022(4) 0.0029(4) -0.0123(4) O4 0.059(2) 0.046(2) 0.098(3) 0.029(2) -0.028(2) -0.0200(19) C4 0.032(2) 0.031(2) 0.0201(19) 0.0012(16) 0.0028(15) -0.0118(16) O5 0.069(2) 0.057(2) 0.048(2) 0.0075(17) -0.0190(17) -0.041(2) C5 0.0279(19) 0.036(2) 0.0225(19) -0.0002(16) 0.0034(15) -0.0123(17) O6 0.0362(17) 0.049(2) 0.0448(19) 0.0186(16) -0.0043(14) -0.0176(15) C6 0.0230(18) 0.027(2) 0.0260(19) -0.0012(16) -0.0030(14) -0.0062(15) O7 0.0359(17) 0.085(3) 0.0402(19) 0.0135(18) -0.0072(14) -0.0367(18) C7 0.0225(17) 0.0240(19) 0.0268(19) -0.0023(15) -0.0010(14) -0.0064(14) O8 0.075(3) 0.071(3) 0.051(2) -0.025(2) 0.0323(19) -0.034(2) C8 0.0250(18) 0.027(2) 0.0267(19) -0.0005(16) -0.0022(14) -0.0087(15) O9 0.074(3) 0.091(3) 0.040(2) 0.0240(19) -0.0097(17) -0.061(2) C9 0.0262(19) 0.028(2) 0.0247(19) 0.0007(16) 0.0002(14) -0.0104(15) O10 0.0390(16) 0.0339(17) 0.0340(16) 0.0055(13) 0.0036(12) -0.0190(13) C10 0.0229(18) 0.031(2) 0.0233(19) -0.0011(16) 0.0018(14) -0.0068(15) O11 0.083(3) 0.048(2) 0.069(3) -0.017(2) -0.018(2) -0.008(2) C11 0.0260(18) 0.024(2) 0.0223(18) 0.0016(15) -0.0016(14) -0.0056(15) O12 0.200(6) 0.078(4) 0.068(3) -0.010(3) 0.021(3) -0.082(4) C12 0.0229(18) 0.027(2) 0.0220(18) -0.0034(15) 0.0040(14) -0.0089(15) O13 0.053(2) 0.057(3) 0.078(3) -0.014(2) 0.0240(19) -0.0190(19) C13 0.048(3) 0.067(4) 0.037(3) -0.001(2) 0.006(2) -0.032(3) O14 0.108(3) 0.052(2) 0.063(3) -0.005(2) -0.025(2) -0.043(2) C14 0.042(3) 0.052(3) 0.040(3) 0.000(2) 0.003(2) -0.023(2) O15 0.060(3) 0.113(4) 0.069(3) 0.032(3) -0.012(2) -0.050(3) C15 0.036(2) 0.040(3) 0.031(2) -0.0043(19) -0.0011(17) -0.0195(19) C16 0.036(2) 0.039(2) 0.028(2) -0.0008(18) -0.0008(16) -0.0215(19) C17 0.078(4) 0.042(3) 0.039(3) -0.013(2) 0.020(2) -0.032(3) C18 0.070(3) 0.032(3) 0.049(3) -0.011(2) 0.019(2) -0.025(2) C19 0.033(2) 0.031(2) 0.031(2) -0.0025(18) 0.0037(16) -0.0114(17) C20 0.038(2) 0.032(2) 0.034(2) -0.0013(18) 0.0012(17) -0.0137(18) C21 0.058(3) 0.046(3) 0.043(3) 0.001(2) 0.009(2) -0.022(2) C22 0.071(4) 0.045(3) 0.056(3) 0.008(3) 0.001(3) -0.030(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 Ba1 O8 2.725(4) 1_645 ? Ba1 O9 2.743(3) . ? Ba1 O13 2.759(4) . ? Ba1 O6 2.804(3) 2_566 ? Ba1 O12 2.840(5) . ? Ba1 O14 2.846(4) . ? Ba1 O11 2.921(4) . ? Ba1 O4 2.925(4) . ? Ba1 O3 3.090(5) . ? Ba1 S3 3.5476(12) . ? S1 C11 1.768(4) 2_575 ? S1 C2 1.774(4) . ? O1 C1 1.345(5) . ? O1 H1 0.76(5) . ? N1 C22 1.326(7) . ? N1 C13 1.342(7) . ? N1 O9 1.345(5) . ? C1 C6 1.399(5) . ? C1 C2 1.409(6) . ? S2 C6 1.778(4) . ? S2 C7 1.789(4) . ? O2 C12 1.346(4) . ? O2 H2 0.83(6) . ? N2 O10 1.340(4) . ? N2 C18 1.342(6) . ? N2 C19 1.342(6) . ? C2 C3 1.380(5) . ? S3 O5 1.423(3) . ? S3 O3 1.427(4) . ? S3 O4 1.489(4) . ? S3 C4 1.767(4) . ? C3 C4 1.394(5) . ? C3 H3 0.9300 . ? S4 O7 1.435(3) . ? S4 O8 1.447(4) . ? S4 O6 1.449(3) . ? S4 C9 1.763(4) . ? C4 C5 1.368(6) . ? C5 C6 1.400(5) . ? C5 H5 0.9300 . ? O6 Ba1 2.804(3) 2_566 ? C7 C8 1.389(5) . ? C7 C12 1.401(5) . ? O8 Ba1 2.725(4) 1_465 ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C9 C10 1.388(5) . ? C10 C11 1.388(5) . ? C10 H10 0.9300 . ? C11 C12 1.403(5) . ? C11 S1 1.768(4) 2_575 ? C13 C14 1.365(6) . ? C13 H13 0.9300 . ? C14 C15 1.383(6) . ? C14 H14 0.9300 . ? C15 C21 1.379(7) . ? C15 C16 1.488(6) . ? C16 C17 1.388(7) . ? C16 C20 1.391(6) . ? C17 C18 1.359(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.383(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.384(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? 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 O9 79.99(13) 1_645 . ? O8 Ba1 O13 141.59(12) 1_645 . ? O9 Ba1 O13 135.41(14) . . ? O8 Ba1 O6 96.97(12) 1_645 2_566 ? O9 Ba1 O6 68.75(9) . 2_566 ? O13 Ba1 O6 86.63(12) . 2_566 ? O8 Ba1 O12 73.62(15) 1_645 . ? O9 Ba1 O12 137.75(17) . . ? O13 Ba1 O12 69.01(15) . . ? O6 Ba1 O12 82.22(14) 2_566 . ? O8 Ba1 O14 74.48(13) 1_645 . ? O9 Ba1 O14 131.76(12) . . ? O13 Ba1 O14 85.41(14) . . ? O6 Ba1 O14 153.55(11) 2_566 . ? O12 Ba1 O14 71.37(14) . . ? O8 Ba1 O11 146.63(13) 1_645 . ? O9 Ba1 O11 69.05(14) . . ? O13 Ba1 O11 66.49(13) . . ? O6 Ba1 O11 60.84(11) 2_566 . ? O12 Ba1 O11 122.45(14) . . ? O14 Ba1 O11 136.31(12) . . ? O8 Ba1 O4 82.96(12) 1_645 . ? O9 Ba1 O4 71.34(11) . . ? O13 Ba1 O4 118.14(12) . . ? O6 Ba1 O4 139.43(10) 2_566 . ? O12 Ba1 O4 134.99(14) . . ? O14 Ba1 O4 65.49(12) . . ? O11 Ba1 O4 98.12(13) . . ? O8 Ba1 O3 127.24(11) 1_645 . ? O9 Ba1 O3 92.76(12) . . ? O13 Ba1 O3 74.11(12) . . ? O6 Ba1 O3 128.98(11) 2_566 . ? O12 Ba1 O3 129.49(17) . . ? O14 Ba1 O3 72.45(12) . . ? O11 Ba1 O3 68.15(11) . . ? O4 Ba1 O3 46.07(11) . . ? O8 Ba1 S3 103.69(9) 1_645 . ? O9 Ba1 S3 87.44(8) . . ? O13 Ba1 S3 93.92(9) . . ? O6 Ba1 S3 145.17(7) 2_566 . ? O12 Ba1 S3 130.31(13) . . ? O14 Ba1 S3 60.69(8) . . ? O11 Ba1 S3 87.49(9) . . ? O4 Ba1 S3 24.24(8) . . ? O3 Ba1 S3 23.56(8) . . ? C11 S1 C2 105.33(18) 2_575 . ? C1 O1 H1 114(4) . . ? C22 N1 C13 121.1(4) . . ? C22 N1 O9 119.9(5) . . ? C13 N1 O9 119.0(5) . . ? O1 C1 C6 123.6(4) . . ? O1 C1 C2 117.1(3) . . ? C6 C1 C2 119.3(3) . . ? C6 S2 C7 102.83(18) . . ? C12 O2 H2 110(4) . . ? O10 N2 C18 120.5(4) . . ? O10 N2 C19 119.0(4) . . ? C18 N2 C19 120.5(4) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 S1 117.8(3) . . ? C1 C2 S1 122.7(3) . . ? O5 S3 O3 116.3(3) . . ? O5 S3 O4 110.2(3) . . ? O3 S3 O4 107.9(3) . . ? O5 S3 C4 107.3(2) . . ? O3 S3 C4 108.2(2) . . ? O4 S3 C4 106.5(2) . . ? O5 S3 Ba1 110.30(15) . . ? O3 S3 Ba1 59.9(2) . . ? O4 S3 Ba1 53.74(17) . . ? C4 S3 Ba1 141.81(14) . . ? S3 O3 Ba1 96.5(2) . . ? C2 C3 C4 121.3(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O7 S4 O8 114.0(2) . . ? O7 S4 O6 112.6(2) . . ? O8 S4 O6 109.5(2) . . ? O7 S4 C9 107.91(19) . . ? O8 S4 C9 106.1(2) . . ? O6 S4 C9 106.32(18) . . ? S3 O4 Ba1 102.0(2) . . ? C5 C4 C3 119.3(4) . . ? C5 C4 S3 121.2(3) . . ? C3 C4 S3 119.5(3) . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? S4 O6 Ba1 122.8(2) . 2_566 ? C1 C6 C5 119.6(4) . . ? C1 C6 S2 120.1(3) . . ? C5 C6 S2 120.2(3) . . ? C8 C7 C12 120.1(3) . . ? C8 C7 S2 119.2(3) . . ? C12 C7 S2 120.5(3) . . ? S4 O8 Ba1 149.0(3) . 1_465 ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N1 O9 Ba1 123.1(3) . . ? C8 C9 C10 119.7(3) . . ? C8 C9 S4 118.2(3) . . ? C10 C9 S4 121.9(3) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 S1 117.8(3) . 2_575 ? C12 C11 S1 121.8(3) . 2_575 ? O2 C12 C7 124.0(3) . . ? O2 C12 C11 117.1(3) . . ? C7 C12 C11 118.9(3) . . ? N1 C13 C14 119.5(5) . . ? N1 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 121.5(5) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C21 C15 C14 117.2(4) . . ? C21 C15 C16 121.2(4) . . ? C14 C15 C16 121.6(4) . . ? C17 C16 C20 116.8(4) . . ? C17 C16 C15 121.3(4) . . ? C20 C16 C15 121.9(4) . . ? C18 C17 C16 121.5(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? N2 C18 C17 120.5(5) . . ? N2 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? N2 C19 C20 120.6(4) . . ? N2 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C16 120.2(4) . . ? C19 C20 H20 119.9 . . ? C16 C20 H20 119.9 . . ? C15 C21 C22 119.7(5) . . ? C15 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? N1 C22 C21 120.9(5) . . ? N1 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.277 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.109 ###END