Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email wqpang@mail.jlu.edu.cn _publ_contact_author_name 'Prof Wenqin Pang' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name W.Pang G.Li Z.Shi Y.Xing data_sad _database_code_CSD 196729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H22 La2 N2 O22 S4' _chemical_formula_weight 832.28 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' 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' La La -0.2871 2.4523 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.9220(8) _cell_length_b 31.639(4) _cell_length_c 9.6388(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.020(3) _cell_angle_gamma 90.00 _cell_volume 2038.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 4.654 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3053 _exptl_absorpt_correction_T_max 0.3888 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5905 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2916 _reflns_number_gt 2295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0089P)^2^+6.2270P] 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 2916 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _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 La1 La 0.25437(6) 0.681015(14) 0.31031(5) 0.01331(12) Uani 1 1 d . . . La2 La -0.36075(6) 0.568195(15) 0.22306(5) 0.01565(13) Uani 1 1 d . . . S1 S -0.2456(3) 0.67093(6) 0.2519(2) 0.0166(5) Uani 1 1 d . . . S2 S 0.2774(3) 0.75208(7) 0.0708(2) 0.0159(4) Uani 1 1 d . . . S3 S 0.4149(3) 0.60128(6) 0.5258(2) 0.0160(4) Uani 1 1 d . . . S4 S -0.9104(3) 0.58274(6) 0.0784(2) 0.0150(4) Uani 1 1 d . . . O1 O -0.1281(7) 0.70175(17) 0.1905(5) 0.0201(13) Uani 1 1 d . . . O2 O -0.0992(8) 0.64272(18) 0.3498(5) 0.0281(14) Uani 1 1 d . . . O3 O -0.3735(7) 0.69330(16) 0.3283(5) 0.0216(13) Uani 1 1 d . . . O4 O -0.3737(8) 0.64416(17) 0.1382(5) 0.0264(14) Uani 1 1 d . . . O5 O 0.2959(7) 0.76094(17) 0.2245(5) 0.0222(13) Uani 1 1 d . . . O6 O 0.2511(7) 0.70585(16) 0.0549(5) 0.0200(13) Uani 1 1 d . . . O7 O 0.4523(7) 0.76710(17) 0.0256(5) 0.0224(13) Uani 1 1 d . . . O8 O 0.1020(7) 0.77443(16) -0.0225(5) 0.0207(13) Uani 1 1 d . . . O9 O 0.4605(7) 0.60772(17) 0.3825(5) 0.0223(13) Uani 1 1 d . . . O10 O 0.3104(8) 0.64115(16) 0.5460(5) 0.0245(13) Uani 1 1 d . . . O11 O 0.2837(7) 0.56500(17) 0.5203(6) 0.0265(13) Uani 1 1 d . . . O12 O 0.5975(7) 0.59557(17) 0.6380(5) 0.0250(14) Uani 1 1 d . . . O13 O -0.7243(7) 0.55731(17) 0.1000(5) 0.0222(13) Uani 1 1 d . . . O14 O -0.8599(8) 0.62635(16) 0.1208(5) 0.0233(13) Uani 1 1 d . . . O15 O -1.0236(7) 0.58069(16) -0.0731(5) 0.0216(13) Uani 1 1 d . . . O16 O -1.0307(7) 0.56393(17) 0.1693(5) 0.0229(13) Uani 1 1 d . . . O1W O -0.1106(8) 0.5509(2) 0.4501(6) 0.0325(16) Uani 1 1 d D . . O2W O -0.3066(8) 0.49561(19) 0.1239(6) 0.0275(14) Uani 1 1 d D . . O3W O -0.4316(8) 0.57480(19) -0.0593(6) 0.0244(14) Uani 1 1 d D . . O4W O -0.4808(8) 0.50794(19) 0.3467(6) 0.0288(14) Uani 1 1 d D . . O5W O -0.1310(9) 0.5174(2) 0.7081(6) 0.0292(14) Uani 1 1 d D . . O6W O -0.6737(9) 0.6463(2) -0.1485(6) 0.0334(15) Uani 1 1 d D . . C1 C -1.1347(11) 0.6838(3) -0.2990(8) 0.0242(19) Uani 1 1 d . . . H1A H -1.2487 0.6935 -0.3736 0.080 Uiso 1 1 calc . . . H1B H -1.0290 0.7046 -0.2873 0.080 Uiso 1 1 calc . . . C2 C -1.1939(11) 0.6786(2) -0.1588(8) 0.0204(19) Uani 1 1 d . . . H2A H -1.3028 0.6585 -0.1714 0.080 Uiso 1 1 calc . . . H2B H -1.0813 0.6679 -0.0850 0.080 Uiso 1 1 calc . . . N1 N -1.0645(9) 0.6427(2) -0.3411(6) 0.0244(17) Uani 1 1 d . . . H1C H -1.0305 0.6456 -0.4235 0.080 Uiso 1 1 calc . . . H1D H -1.1621 0.6236 -0.3520 0.080 Uiso 1 1 calc . . . H1E H -0.9588 0.6340 -0.2730 0.080 Uiso 1 1 calc . . . N2 N -1.2575(9) 0.7202(2) -0.1139(7) 0.0281(18) Uani 1 1 d . . . H2C H -1.2915 0.7173 -0.0315 0.080 Uiso 1 1 calc . . . H2D H -1.3620 0.7297 -0.1813 0.080 Uiso 1 1 calc . . . H2E H -1.1570 0.7385 -0.1022 0.080 Uiso 1 1 calc . . . H1WA H -0.125(15) 0.535(3) 0.521(8) 0.080 Uiso 1 1 d D . . H1WB H 0.019(8) 0.547(3) 0.470(11) 0.080 Uiso 1 1 d D . . H2WA H -0.269(15) 0.487(3) 0.052(8) 0.080 Uiso 1 1 d D . . H2WB H -0.395(12) 0.487(3) 0.161(11) 0.080 Uiso 1 1 d D . . H3WA H -0.536(11) 0.559(3) -0.090(10) 0.080 Uiso 1 1 d D . . H3WB H -0.322(10) 0.575(3) -0.084(11) 0.080 Uiso 1 1 d D . . H4WA H -0.608(8) 0.502(4) 0.311(10) 0.080 Uiso 1 1 d D . . H4WB H -0.441(16) 0.484(2) 0.388(10) 0.080 Uiso 1 1 d D . . H5WA H -0.093(16) 0.531(3) 0.786(8) 0.080 Uiso 1 1 d D . . H5WB H -0.045(13) 0.499(3) 0.736(11) 0.080 Uiso 1 1 d D . . H6WA H -0.598(14) 0.621(2) -0.114(10) 0.080 Uiso 1 1 d D . . H6WB H -0.664(16) 0.639(3) -0.232(7) 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 La1 0.0140(2) 0.0133(3) 0.0133(2) 0.0002(2) 0.00482(18) 0.0001(2) La2 0.0134(2) 0.0175(3) 0.0173(2) 0.0002(2) 0.00630(18) 0.0013(2) S1 0.0148(10) 0.0176(12) 0.0185(10) -0.0018(9) 0.0065(8) 0.0020(9) S2 0.0151(10) 0.0202(12) 0.0135(10) 0.0032(9) 0.0056(8) -0.0014(9) S3 0.0144(10) 0.0187(12) 0.0156(10) 0.0022(9) 0.0053(8) 0.0005(9) S4 0.0136(10) 0.0150(12) 0.0170(10) -0.0017(9) 0.0050(8) -0.0006(8) O1 0.012(3) 0.024(3) 0.026(3) 0.000(3) 0.006(2) -0.005(2) O2 0.032(3) 0.032(4) 0.020(3) 0.008(3) 0.007(3) 0.009(3) O3 0.015(3) 0.022(3) 0.031(3) -0.007(3) 0.012(2) -0.002(2) O4 0.032(3) 0.021(3) 0.024(3) -0.007(3) 0.003(3) -0.006(3) O5 0.028(3) 0.025(3) 0.013(3) 0.001(2) 0.004(2) 0.001(3) O6 0.028(3) 0.016(3) 0.017(3) 0.001(2) 0.008(2) -0.001(3) O7 0.018(3) 0.027(3) 0.024(3) 0.003(3) 0.008(2) -0.001(3) O8 0.018(3) 0.023(3) 0.020(3) 0.009(3) 0.002(2) 0.003(2) O9 0.026(3) 0.025(4) 0.020(3) 0.002(3) 0.014(2) 0.006(3) O10 0.037(3) 0.018(3) 0.022(3) 0.002(3) 0.014(3) 0.012(3) O11 0.018(3) 0.020(3) 0.040(3) 0.009(3) 0.005(3) -0.004(3) O12 0.016(3) 0.030(4) 0.022(3) 0.004(3) -0.007(2) -0.002(3) O13 0.014(3) 0.028(4) 0.025(3) 0.001(3) 0.007(2) 0.007(2) O14 0.030(3) 0.014(3) 0.027(3) -0.003(3) 0.009(3) -0.003(3) O15 0.020(3) 0.024(4) 0.020(3) -0.006(2) 0.003(2) -0.001(2) O16 0.021(3) 0.028(4) 0.024(3) 0.001(3) 0.015(2) 0.000(3) O1W 0.017(3) 0.047(5) 0.030(4) 0.014(3) 0.001(3) -0.007(3) O2W 0.029(3) 0.028(4) 0.029(4) -0.011(3) 0.014(3) -0.003(3) O3W 0.022(3) 0.031(4) 0.022(3) -0.004(3) 0.010(3) -0.009(3) O4W 0.024(3) 0.025(4) 0.039(4) 0.010(3) 0.010(3) -0.001(3) O5W 0.028(4) 0.027(4) 0.030(3) 0.000(3) 0.003(3) 0.003(3) O6W 0.031(4) 0.043(4) 0.025(3) 0.002(3) 0.004(3) 0.009(3) C1 0.026(5) 0.025(5) 0.024(4) 0.003(4) 0.011(4) 0.000(4) C2 0.025(5) 0.018(5) 0.021(4) 0.001(4) 0.011(4) 0.000(4) N1 0.018(4) 0.034(5) 0.022(4) -0.003(3) 0.006(3) -0.001(3) N2 0.026(4) 0.030(5) 0.027(4) -0.002(3) 0.005(3) 0.002(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 La1 O14 2.491(5) 1_655 ? La1 O10 2.539(5) . ? La1 O8 2.565(5) 4_576 ? La1 O3 2.566(5) 1_655 ? La1 O6 2.579(5) . ? La1 O1 2.681(5) . ? La1 O5 2.699(5) . ? La1 O9 2.717(5) . ? La1 O7 2.721(5) 4_576 ? La1 O2 2.844(5) . ? La1 S2 3.256(2) . ? La1 S2 3.256(2) 4_576 ? La2 O16 2.474(5) 1_655 ? La2 O1W 2.474(6) . ? La2 O4W 2.501(6) . ? La2 O13 2.512(5) . ? La2 O4 2.533(5) . ? La2 O9 2.538(5) 1_455 ? La2 O2W 2.552(6) . ? La2 O3W 2.646(5) . ? La2 S1 3.341(2) . ? La2 H2WB 2.62(11) . ? S1 O3 1.472(5) . ? S1 O4 1.484(5) . ? S1 O1 1.487(5) . ? S1 O2 1.490(5) . ? S2 O7 1.468(5) . ? S2 O6 1.477(5) . ? S2 O5 1.480(5) . ? S2 O8 1.489(5) . ? S2 La1 3.256(2) 4_575 ? S3 O12 1.446(5) . ? S3 O11 1.456(5) . ? S3 O10 1.492(5) . ? S3 O9 1.509(5) . ? S4 O14 1.456(5) . ? S4 O15 1.468(5) . ? S4 O16 1.481(5) . ? S4 O13 1.487(5) . ? O3 La1 2.566(4) 1_455 ? O7 La1 2.721(5) 4_575 ? O8 La1 2.565(5) 4_575 ? O9 La2 2.538(5) 1_655 ? O14 La1 2.491(5) 1_455 ? O16 La2 2.474(5) 1_455 ? O1W H1WA 0.88(5) . ? O1W H1WB 0.87(5) . ? O2W H2WA 0.85(5) . ? O2W H2WB 0.83(5) . ? O3W H3WA 0.87(5) . ? O3W H3WB 0.85(5) . ? O4W H4WA 0.88(5) . ? O4W H4WB 0.85(5) . ? O5W H5WA 0.84(5) . ? O5W H5WB 0.84(5) . ? O6W H6WA 0.95(5) . ? O6W H6WB 0.85(5) . ? C1 N1 1.481(10) . ? C1 C2 1.520(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.488(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? 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 O14 La1 O10 104.89(17) 1_655 . ? O14 La1 O8 137.57(16) 1_655 4_576 ? O10 La1 O8 72.73(16) . 4_576 ? O14 La1 O3 106.10(16) 1_655 1_655 ? O10 La1 O3 95.56(16) . 1_655 ? O8 La1 O3 116.33(15) 4_576 1_655 ? O14 La1 O6 65.74(16) 1_655 . ? O10 La1 O6 165.27(16) . . ? O8 La1 O6 121.95(16) 4_576 . ? O3 La1 O6 77.21(16) 1_655 . ? O14 La1 O1 76.31(16) 1_655 . ? O10 La1 O1 114.32(16) . . ? O8 La1 O1 67.37(15) 4_576 . ? O3 La1 O1 148.64(15) 1_655 . ? O6 La1 O1 75.58(15) . . ? O14 La1 O5 117.69(15) 1_655 . ? O10 La1 O5 137.39(16) . . ? O8 La1 O5 76.78(15) 4_576 . ? O3 La1 O5 72.19(16) 1_655 . ? O6 La1 O5 52.93(15) . . ? O1 La1 O5 79.07(15) . . ? O14 La1 O9 68.97(16) 1_655 . ? O10 La1 O9 53.03(15) . . ? O8 La1 O9 125.62(15) 4_576 . ? O3 La1 O9 70.16(16) 1_655 . ? O6 La1 O9 112.24(15) . . ? O1 La1 O9 135.52(16) . . ? O5 La1 O9 141.96(15) . . ? O14 La1 O7 168.40(16) 1_655 4_576 ? O10 La1 O7 71.78(16) . 4_576 ? O8 La1 O7 52.92(15) 4_576 4_576 ? O3 La1 O7 63.83(14) 1_655 4_576 ? O6 La1 O7 114.98(16) . 4_576 ? O1 La1 O7 115.26(15) . 4_576 ? O5 La1 O7 66.17(15) . 4_576 ? O9 La1 O7 101.09(15) . 4_576 ? O14 La1 O2 71.43(16) 1_655 . ? O10 La1 O2 66.77(16) . . ? O8 La1 O2 68.99(16) 4_576 . ? O3 La1 O2 159.92(16) 1_655 . ? O6 La1 O2 117.57(15) . . ? O1 La1 O2 51.24(15) . . ? O5 La1 O2 127.15(15) . . ? O9 La1 O2 90.87(15) . . ? O7 La1 O2 115.82(14) 4_576 . ? O14 La1 S2 91.39(12) 1_655 . ? O10 La1 S2 162.43(13) . . ? O8 La1 S2 99.76(12) 4_576 . ? O3 La1 S2 73.18(12) 1_655 . ? O6 La1 S2 26.19(12) . . ? O1 La1 S2 75.51(11) . . ? O5 La1 S2 26.75(10) . . ? O9 La1 S2 130.69(10) . . ? O7 La1 S2 90.96(11) 4_576 . ? O2 La1 S2 126.24(11) . . ? O14 La1 S2 163.64(12) 1_655 4_576 ? O10 La1 S2 70.57(12) . 4_576 ? O8 La1 S2 26.38(11) 4_576 4_576 ? O3 La1 S2 90.11(11) 1_655 4_576 ? O6 La1 S2 121.65(12) . 4_576 ? O1 La1 S2 91.07(11) . 4_576 ? O5 La1 S2 68.87(11) . 4_576 ? O9 La1 S2 116.09(11) . 4_576 ? O7 La1 S2 26.55(10) 4_576 4_576 ? O2 La1 S2 92.60(11) . 4_576 ? S2 La1 S2 95.522(16) . 4_576 ? O16 La2 O1W 72.58(17) 1_655 . ? O16 La2 O4W 119.80(18) 1_655 . ? O1W La2 O4W 69.69(19) . . ? O16 La2 O13 139.48(16) 1_655 . ? O1W La2 O13 140.62(17) . . ? O4W La2 O13 72.82(18) . . ? O16 La2 O4 86.64(18) 1_655 . ? O1W La2 O4 116.98(19) . . ? O4W La2 O4 152.70(18) . . ? O13 La2 O4 91.73(17) . . ? O16 La2 O9 140.83(17) 1_655 1_455 ? O1W La2 O9 84.99(18) . 1_455 ? O4W La2 O9 79.22(18) . 1_455 ? O13 La2 O9 76.55(16) . 1_455 ? O4 La2 O9 75.29(16) . 1_455 ? O16 La2 O2W 68.85(17) 1_655 . ? O1W La2 O2W 89.7(2) . . ? O4W La2 O2W 65.91(19) . . ? O13 La2 O2W 85.77(17) . . ? O4 La2 O2W 136.82(17) . . ? O9 La2 O2W 144.30(17) 1_455 . ? O16 La2 O3W 73.97(16) 1_655 . ? O1W La2 O3W 145.89(17) . . ? O4W La2 O3W 123.66(19) . . ? O13 La2 O3W 68.24(15) . . ? O4 La2 O3W 67.11(17) . . ? O9 La2 O3W 126.47(17) 1_455 . ? O2W La2 O3W 72.06(19) . . ? O16 La2 S1 81.78(13) 1_655 . ? O1W La2 S1 92.55(15) . . ? O4W La2 S1 143.45(15) . . ? O13 La2 S1 111.15(13) . . ? O4 La2 S1 24.70(12) . . ? O9 La2 S1 67.26(12) 1_455 . ? O2W La2 S1 148.37(12) . . ? O3W La2 S1 89.16(13) . . ? O16 La2 H2WB 86.2(14) 1_655 . ? O1W La2 H2WB 89(2) . . ? O4W La2 H2WB 48.9(14) . . ? O13 La2 H2WB 75(2) . . ? O4 La2 H2WB 149(2) . . ? O9 La2 H2WB 126.0(12) 1_455 . ? O2W La2 H2WB 18.4(11) . . ? O3W La2 H2WB 82(2) . . ? S1 La2 H2WB 166.7(12) . . ? O3 S1 O4 108.8(3) . . ? O3 S1 O1 110.2(3) . . ? O4 S1 O1 111.4(3) . . ? O3 S1 O2 111.7(3) . . ? O4 S1 O2 107.7(3) . . ? O1 S1 O2 107.0(3) . . ? O3 S1 La2 110.4(2) . . ? O4 S1 La2 45.5(2) . . ? O1 S1 La2 138.4(2) . . ? O2 S1 La2 65.0(2) . . ? O3 S1 La1 126.5(2) . . ? O4 S1 La1 124.6(2) . . ? O1 S1 La1 50.3(2) . . ? O2 S1 La1 56.7(2) . . ? La2 S1 La1 108.55(5) . . ? O7 S2 O6 112.2(3) . . ? O7 S2 O5 111.8(3) . . ? O6 S2 O5 105.5(3) . . ? O7 S2 O8 105.9(3) . . ? O6 S2 O8 110.4(3) . . ? O5 S2 O8 111.1(3) . . ? O7 S2 La1 129.0(2) . . ? O6 S2 La1 50.40(19) . . ? O5 S2 La1 55.1(2) . . ? O8 S2 La1 125.0(2) . . ? O7 S2 La1 56.0(2) . 4_575 ? O6 S2 La1 125.7(2) . 4_575 ? O5 S2 La1 128.5(2) . 4_575 ? O8 S2 La1 49.93(19) . 4_575 ? La1 S2 La1 173.75(7) . 4_575 ? O12 S3 O11 110.2(3) . . ? O12 S3 O10 111.6(3) . . ? O11 S3 O10 110.7(3) . . ? O12 S3 O9 110.6(3) . . ? O11 S3 O9 110.5(3) . . ? O10 S3 O9 103.2(3) . . ? O12 S3 La1 131.1(2) . . ? O11 S3 La1 118.6(2) . . ? O10 S3 La1 48.29(19) . . ? O9 S3 La1 55.4(2) . . ? O14 S4 O15 110.4(3) . . ? O14 S4 O16 110.2(3) . . ? O15 S4 O16 109.5(3) . . ? O14 S4 O13 109.7(3) . . ? O15 S4 O13 109.6(3) . . ? O16 S4 O13 107.4(3) . . ? S1 O1 La1 104.4(3) . . ? S1 O2 La1 97.3(3) . . ? S1 O3 La1 128.1(3) . 1_455 ? S1 O4 La2 109.8(3) . . ? S2 O5 La1 98.1(3) . . ? S2 O6 La1 103.4(2) . . ? S2 O7 La1 97.5(2) . 4_575 ? S2 O8 La1 103.7(2) . 4_575 ? S3 O9 La2 137.6(3) . 1_655 ? S3 O9 La1 97.4(2) . . ? La2 O9 La1 124.86(18) 1_655 . ? S3 O10 La1 105.7(2) . . ? S4 O13 La2 135.9(3) . . ? S4 O14 La1 150.7(3) . 1_455 ? S4 O16 La2 142.5(3) . 1_455 ? La2 O1W H1WA 128(7) . . ? La2 O1W H1WB 132(7) . . ? H1WA O1W H1WB 94(9) . . ? La2 O2W H2WA 135(7) . . ? La2 O2W H2WB 86(8) . . ? H2WA O2W H2WB 133(10) . . ? La2 O3W H3WA 103(7) . . ? La2 O3W H3WB 111(7) . . ? H3WA O3W H3WB 129(10) . . ? La2 O4W H4WA 114(7) . . ? La2 O4W H4WB 141(7) . . ? H4WA O4W H4WB 99(10) . . ? H5WA O5W H5WB 92(10) . . ? H6WA O6W H6WB 87(9) . . ? N1 C1 C2 109.4(6) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 109.4(6) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? 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 N1 H1C O2 0.89 2.11 2.926(8) 151.3 1_454 N1 H1C O10 0.89 2.46 3.064(8) 125.8 1_454 N1 H1D O12 0.89 1.87 2.737(8) 165.2 1_354 N1 H1E O6W 0.89 2.06 2.859(8) 148.3 . N2 H2C O1 0.89 2.20 2.896(8) 134.7 1_455 N2 H2C O7 0.89 2.54 3.073(8) 119.3 1_355 N2 H2D O5 0.89 2.32 3.138(8) 151.8 4_375 N2 H2E O8 0.89 2.09 2.962(8) 165.3 1_455 O1W H1WA O5W 0.88(5) 1.90(6) 2.740(8) 161(10) . O1W H1WB O11 0.87(5) 1.86(6) 2.674(7) 154(10) . O2W H2WA O13 0.85(5) 2.02(7) 2.783(7) 149(10) 3_465 O2W H2WB O4W 0.83(5) 2.13(9) 2.749(8) 132(10) . O2W H2WB O3W 0.83(5) 2.38(10) 2.837(8) 116(9) 3_465 O3W H3WA O2W 0.87(5) 2.02(6) 2.837(8) 156(10) 3_465 O3W H3WB O15 0.85(5) 2.05(6) 2.868(7) 161(10) 1_655 O4W H4WA O5W 0.88(5) 1.87(6) 2.722(8) 163(10) 3_466 O4W H4WB O11 0.85(5) 1.98(5) 2.815(8) 166(10) 3_566 O5W H5WA O15 0.84(5) 2.06(6) 2.862(8) 159(11) 1_656 O5W H5WB O16 0.84(5) 2.18(7) 2.931(8) 149(10) 3_466 O5W H5WB O2W 0.84(5) 2.47(9) 3.070(8) 130(10) 3_566 O6W H6WA O3W 0.95(5) 1.86(5) 2.814(9) 173(9) . O6W H6WB O10 0.85(5) 2.10(6) 2.923(7) 161(10) 1_454 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.557 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.141 #============================================================ END