Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Daniel, Louer' 'Thierry, Bataille' _publ_contact_author_name 'Dr Daniel Louer' _publ_contact_author_address ; Laboratoire de Chimie du Solide et Inorganique Moleculaire UMR CNRS 6511, Inst de Chimie, Univ de Rennes I Avenue du General Leclerc Rennes 35042 cedex FRANCE ; _publ_contact_author_email 'DANIEL.LOUER@UNIV-RENNES1.FR' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Two new diamine templated lanthanum sulfates, La2(H20)2(C4H12N2)(SO4) and La2(H20)2(C2H10N2)3(SO4)6.4H20, with 3D and 2D crystal structures ; data_job _database_code_CSD 190425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'lanthanum ethylenediammonium sulfate hexahydrate' _chemical_melting_point ? _chemical_formula_moiety 'La2 (H2 O)2 (C2 H10 N2)3 (S O4)6 (H2 O)4' _chemical_formula_sum 'C6 H42 La2 N6 O30 S6' _chemical_formula_weight 1148.64 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' 'La' 'La' -0.2871 2.4523 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 6.66050(10) _cell_length_b 26.7013(6) _cell_length_c 10.0256(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.8740(10) _cell_angle_gamma 90.00 _cell_volume 1723.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10689 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 2.922 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7377 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details 'N.W. Alcock (1970). Cryst. Computing, p271)' _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16891 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3953 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0333P)^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 SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3953 _refine_ls_number_parameters 311 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.985 _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 La La 0.45460(4) 0.176035(12) 0.03108(3) 0.01568(12) Uani 1 1 d . . . S1 S 0.5969(2) 0.06344(6) 0.25370(16) 0.0225(4) Uani 1 1 d . . . S2 S 0.47062(18) 0.25125(5) 0.28175(15) 0.0180(3) Uani 1 1 d . . . S3 S 0.96555(19) 0.15610(6) -0.04754(16) 0.0221(4) Uani 1 1 d . . . O11 O 0.4348(6) 0.05217(16) 0.3222(5) 0.0347(11) Uani 1 1 d . . . O12 O 0.8046(5) 0.05323(15) 0.3452(4) 0.0303(10) Uani 1 1 d . . . O13 O 0.5847(6) 0.11754(14) 0.2164(4) 0.0323(11) Uani 1 1 d . . . O14 O 0.5706(6) 0.03288(16) 0.1262(4) 0.0323(11) Uani 1 1 d . . . O21 O 0.5040(5) 0.26298(14) -0.0724(4) 0.0223(9) Uani 1 1 d . . . O22 O 0.4400(5) 0.19428(14) -0.2260(4) 0.0243(9) Uani 1 1 d . . . O23 O 0.6467(5) 0.23598(14) 0.2274(4) 0.0233(9) Uani 1 1 d . . . O24 O 0.2863(5) 0.22527(14) 0.1947(4) 0.0251(10) Uani 1 1 d . . . O31 O 0.8256(5) 0.17679(14) 0.0303(4) 0.0260(10) Uani 1 1 d . . . O32 O 0.0765(5) 0.19762(16) -0.0961(4) 0.0288(10) Uani 1 1 d . . . O33 O 0.1303(5) 0.12615(15) 0.0482(4) 0.0282(10) Uani 1 1 d . . . O34 O 0.8529(6) 0.12594(18) -0.1620(5) 0.0453(13) Uani 1 1 d . . . OW1 O 0.4628(7) 0.09375(16) -0.0932(5) 0.0327(11) Uani 1 1 d D . . H11 H 0.496(11) 0.090(3) -0.179(4) 0.08(3) Uiso 1 1 d D . . H12 H 0.503(10) 0.068(2) -0.027(6) 0.06(2) Uiso 1 1 d D . . N1 N -0.1232(8) 0.6253(2) 1.1443(6) 0.0329(13) Uani 1 1 d D . . HN1A H -0.023(7) 0.5984(16) 1.147(6) 0.038(18) Uiso 1 1 d D . . HN1B H -0.251(7) 0.618(3) 1.073(6) 0.08(3) Uiso 1 1 d D . . HN1C H -0.131(11) 0.629(3) 1.240(3) 0.09(3) Uiso 1 1 d D . . C1 C -0.0519(9) 0.6715(2) 1.0902(7) 0.0296(15) Uani 1 1 d D . . HC1A H -0.151(9) 0.698(2) 1.092(8) 0.08(3) Uiso 1 1 d D . . HC1B H 0.057(8) 0.684(3) 1.167(5) 0.07(3) Uiso 1 1 d D . . C2 C 0.0143(10) 0.6612(3) 0.9613(7) 0.0310(16) Uani 1 1 d D . . HC2A H -0.093(6) 0.648(2) 0.886(4) 0.033(17) Uiso 1 1 d D . . HC2B H 0.124(8) 0.637(2) 0.977(7) 0.07(2) Uiso 1 1 d D . . N2 N 0.0772(7) 0.7079(2) 0.9034(6) 0.0282(13) Uani 1 1 d D . . HN2A H 0.084(9) 0.703(2) 0.809(3) 0.04(2) Uiso 1 1 d D . . HN2B H -0.014(9) 0.7354(19) 0.916(8) 0.08(3) Uiso 1 1 d D . . HN2C H 0.217(5) 0.717(2) 0.957(6) 0.05(2) Uiso 1 1 d D . . N3 N 0.0729(8) 0.4715(2) 0.3473(7) 0.0329(13) Uani 1 1 d D . . HN3A H 0.194(7) 0.493(2) 0.354(7) 0.06(2) Uiso 1 1 d D . . HN3B H 0.096(9) 0.4375(11) 0.379(7) 0.05(2) Uiso 1 1 d D . . HN3C H -0.004(9) 0.472(3) 0.251(3) 0.07(3) Uiso 1 1 d D . . C3 C -0.0547(9) 0.4993(3) 0.4251(7) 0.0360(17) Uani 1 1 d D . . HC3A H -0.188(6) 0.482(2) 0.403(7) 0.06(2) Uiso 1 1 d D . . HC3B H -0.066(10) 0.5328(13) 0.386(7) 0.06(2) Uiso 1 1 d D . . OW2 O 0.2415(7) 0.5315(2) 0.8927(6) 0.0465(13) Uani 1 1 d D . . H21 H 0.229(16) 0.535(4) 0.985(4) 0.14(5) Uiso 1 1 d D . . H22 H 0.295(14) 0.4991(16) 0.882(11) 0.13(4) Uiso 1 1 d D . . OW3 O 0.4668(9) 0.1109(3) 0.5949(8) 0.096(3) Uani 1 1 d D . . H31 H 0.560(11) 0.083(2) 0.618(10) 0.12(4) Uiso 1 1 d D . . H32 H 0.528(13) 0.137(3) 0.657(9) 0.12(4) 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 La 0.01212(16) 0.0183(2) 0.0170(2) 0.00070(17) 0.00447(12) 0.00005(13) S1 0.0226(7) 0.0228(9) 0.0214(9) 0.0026(7) 0.0046(6) 0.0010(6) S2 0.0167(6) 0.0217(8) 0.0161(8) -0.0017(6) 0.0049(6) 0.0002(5) S3 0.0128(6) 0.0265(9) 0.0274(10) -0.0064(7) 0.0057(6) -0.0005(6) O11 0.034(2) 0.040(3) 0.036(3) 0.002(2) 0.018(2) -0.0036(19) O12 0.025(2) 0.032(3) 0.029(3) 0.008(2) 0.0002(18) 0.0009(17) O13 0.046(2) 0.018(2) 0.029(3) 0.004(2) 0.001(2) 0.0005(18) O14 0.039(2) 0.031(3) 0.024(3) -0.005(2) 0.0034(19) 0.0061(19) O21 0.0262(19) 0.023(2) 0.017(2) -0.0030(19) 0.0052(16) 0.0013(16) O22 0.033(2) 0.015(2) 0.025(3) 0.0011(19) 0.0086(18) -0.0043(16) O23 0.0159(18) 0.030(2) 0.026(3) -0.006(2) 0.0096(17) 0.0005(16) O24 0.0173(18) 0.034(3) 0.024(3) -0.014(2) 0.0049(17) -0.0029(16) O31 0.0159(18) 0.036(3) 0.029(3) -0.007(2) 0.0110(16) 0.0001(16) O32 0.0189(19) 0.039(3) 0.030(3) 0.014(2) 0.0083(17) 0.0015(17) O33 0.0151(18) 0.026(2) 0.043(3) 0.007(2) 0.0063(18) 0.0029(16) O34 0.027(2) 0.058(3) 0.048(3) -0.032(3) 0.005(2) -0.001(2) OW1 0.058(3) 0.025(3) 0.019(3) -0.003(2) 0.019(2) 0.006(2) N1 0.036(3) 0.034(4) 0.031(4) 0.006(3) 0.014(3) -0.001(3) C1 0.029(3) 0.028(4) 0.036(4) -0.007(3) 0.014(3) -0.003(3) C2 0.038(4) 0.027(4) 0.033(4) 0.003(3) 0.016(3) -0.001(3) N2 0.025(3) 0.033(3) 0.028(4) 0.006(3) 0.008(2) -0.003(2) N3 0.031(3) 0.026(4) 0.041(4) 0.000(3) 0.007(3) -0.006(2) C3 0.028(4) 0.046(5) 0.031(4) 0.001(4) 0.002(3) 0.006(3) OW2 0.052(3) 0.048(4) 0.036(4) -0.009(3) 0.004(2) 0.003(2) OW3 0.060(4) 0.111(6) 0.095(6) -0.072(5) -0.020(3) 0.034(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 La O13 2.411(4) . ? La O31 2.473(3) . ? La OW1 2.533(4) . ? La O24 2.573(4) . ? La O32 2.579(3) . ? La O33 2.581(3) . ? La O21 2.598(4) . ? La O22 2.600(4) . ? La O23 2.604(4) . ? La S2 3.1885(15) 4_565 ? La S3 3.1931(13) 1_455 ? La S2 3.1973(15) . ? S1 O11 1.452(4) . ? S1 O12 1.476(4) . ? S1 O14 1.488(4) . ? S1 O13 1.489(4) . ? S2 O22 1.468(4) 4_566 ? S2 O21 1.472(4) 4_566 ? S2 O23 1.472(3) . ? S2 O24 1.483(4) . ? S2 La 3.1885(15) 4_566 ? S3 O34 1.445(4) . ? S3 O31 1.469(4) . ? S3 O32 1.482(4) 1_655 ? S3 O33 1.491(4) 1_655 ? S3 La 3.1931(13) 1_655 ? O21 S2 1.472(4) 4_565 ? O22 S2 1.468(4) 4_565 ? O32 S3 1.482(4) 1_455 ? O33 S3 1.491(4) 1_455 ? OW1 H11 0.95(2) . ? OW1 H12 0.95(2) . ? N1 C1 1.474(8) . ? N1 HN1A 0.98(2) . ? N1 HN1B 0.98(2) . ? N1 HN1C 0.98(2) . ? C1 C2 1.494(9) . ? C1 HC1A 0.98(2) . ? C1 HC1B 0.97(2) . ? C2 N2 1.480(8) . ? C2 HC2A 0.96(2) . ? C2 HC2B 0.96(2) . ? N2 HN2A 0.97(2) . ? N2 HN2B 0.98(2) . ? N2 HN2C 0.98(2) . ? N3 C3 1.490(8) . ? N3 HN3A 0.97(2) . ? N3 HN3B 0.96(2) . ? N3 HN3C 0.97(2) . ? C3 C3 1.493(13) 3_566 ? C3 HC3A 0.97(2) . ? C3 HC3B 0.97(2) . ? OW2 H21 0.96(2) . ? OW2 H22 0.95(2) . ? OW3 H31 0.95(2) . ? OW3 H32 0.95(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 O13 La O31 81.14(13) . . ? O13 La OW1 76.61(15) . . ? O31 La OW1 81.82(13) . . ? O13 La O24 88.22(13) . . ? O31 La O24 126.66(12) . . ? OW1 La O24 145.56(13) . . ? O13 La O32 129.62(12) . . ? O31 La O32 147.82(13) . . ? OW1 La O32 95.30(14) . . ? O24 La O32 70.79(12) . . ? O13 La O33 75.86(12) . . ? O31 La O33 149.14(12) . . ? OW1 La O33 73.10(13) . . ? O24 La O33 73.27(12) . . ? O32 La O33 54.58(12) . . ? O13 La O21 146.01(12) . . ? O31 La O21 76.26(12) . . ? OW1 La O21 123.90(13) . . ? O24 La O21 85.32(12) . . ? O32 La O21 79.08(11) . . ? O33 La O21 132.98(11) . . ? O13 La O22 143.10(13) . . ? O31 La O22 77.21(12) . . ? OW1 La O22 71.03(13) . . ? O24 La O22 128.66(12) . . ? O32 La O22 71.63(11) . . ? O33 La O22 110.10(12) . . ? O21 La O22 54.07(12) . . ? O13 La O23 78.82(13) . . ? O31 La O23 72.53(11) . . ? OW1 La O23 146.76(13) . . ? O24 La O23 54.13(10) . . ? O32 La O23 117.67(12) . . ? O33 La O23 121.62(12) . . ? O21 La O23 70.39(12) . . ? O22 La O23 121.34(12) . . ? O13 La S2 157.02(10) . 4_565 ? O31 La S2 76.00(10) . 4_565 ? OW1 La S2 97.65(11) . 4_565 ? O24 La S2 107.24(9) . 4_565 ? O32 La S2 72.62(9) . 4_565 ? O33 La S2 124.30(9) . 4_565 ? O21 La S2 27.09(9) . 4_565 ? O22 La S2 27.01(9) . 4_565 ? O23 La S2 96.28(9) . 4_565 ? O13 La S3 102.96(10) . 1_455 ? O31 La S3 163.20(10) . 1_455 ? OW1 La S3 83.31(10) . 1_455 ? O24 La S3 70.05(8) . 1_455 ? O32 La S3 27.18(9) . 1_455 ? O33 La S3 27.40(9) . 1_455 ? O21 La S3 106.03(8) . 1_455 ? O22 La S3 90.59(8) . 1_455 ? O23 La S3 124.15(7) . 1_455 ? S2 La S3 98.35(4) 4_565 1_455 ? O13 La S2 82.44(10) . . ? O31 La S2 99.53(9) . . ? OW1 La S2 158.56(11) . . ? O24 La S2 27.13(8) . . ? O32 La S2 94.56(10) . . ? O33 La S2 97.55(10) . . ? O21 La S2 76.72(9) . . ? O22 La S2 130.29(9) . . ? O23 La S2 27.00(7) . . ? S2 La S2 103.452(9) 4_565 . ? S3 La S2 97.17(3) 1_455 . ? O11 S1 O12 111.1(3) . . ? O11 S1 O14 110.8(3) . . ? O12 S1 O14 108.5(2) . . ? O11 S1 O13 108.7(2) . . ? O12 S1 O13 108.5(2) . . ? O14 S1 O13 109.2(3) . . ? O22 S2 O21 107.0(2) 4_566 4_566 ? O22 S2 O23 111.6(2) 4_566 . ? O21 S2 O23 111.4(2) 4_566 . ? O22 S2 O24 110.5(2) 4_566 . ? O21 S2 O24 110.8(2) 4_566 . ? O23 S2 O24 105.7(2) . . ? O22 S2 La 53.54(16) 4_566 4_566 ? O21 S2 La 53.49(16) 4_566 4_566 ? O23 S2 La 130.46(16) . 4_566 ? O24 S2 La 123.83(15) . 4_566 ? O22 S2 La 127.22(17) 4_566 . ? O21 S2 La 125.80(17) 4_566 . ? O23 S2 La 53.43(15) . . ? O24 S2 La 52.28(14) . . ? La S2 La 176.04(4) 4_566 . ? O34 S3 O31 111.1(2) . . ? O34 S3 O32 110.9(3) . 1_655 ? O31 S3 O32 109.3(2) . 1_655 ? O34 S3 O33 111.0(3) . 1_655 ? O31 S3 O33 108.8(2) . 1_655 ? O32 S3 O33 105.4(2) 1_655 1_655 ? O34 S3 La 125.32(16) . 1_655 ? O31 S3 La 123.53(16) . 1_655 ? O32 S3 La 52.64(14) 1_655 1_655 ? O33 S3 La 52.79(14) 1_655 1_655 ? S1 O13 La 143.9(3) . . ? S2 O21 La 99.42(19) 4_565 . ? S2 O22 La 99.5(2) 4_565 . ? S2 O23 La 99.57(17) . . ? S2 O24 La 100.59(16) . . ? S3 O31 La 140.3(2) . . ? S3 O32 La 100.18(19) 1_455 . ? S3 O33 La 99.80(19) 1_455 . ? La OW1 H11 125(5) . . ? La OW1 H12 109(5) . . ? H11 OW1 H12 118(6) . . ? C1 N1 HN1A 110(4) . . ? C1 N1 HN1B 102(5) . . ? HN1A N1 HN1B 109(6) . . ? C1 N1 HN1C 112(5) . . ? HN1A N1 HN1C 105(6) . . ? HN1B N1 HN1C 119(6) . . ? N1 C1 C2 111.0(5) . . ? N1 C1 HC1A 109(5) . . ? C2 C1 HC1A 120(5) . . ? N1 C1 HC1B 104(5) . . ? C2 C1 HC1B 115(5) . . ? HC1A C1 HC1B 96(6) . . ? N2 C2 C1 111.1(6) . . ? N2 C2 HC2A 103(4) . . ? C1 C2 HC2A 115(3) . . ? N2 C2 HC2B 111(4) . . ? C1 C2 HC2B 111(4) . . ? HC2A C2 HC2B 105(6) . . ? C2 N2 HN2A 110(4) . . ? C2 N2 HN2B 110(4) . . ? HN2A N2 HN2B 115(6) . . ? C2 N2 HN2C 109(4) . . ? HN2A N2 HN2C 107(5) . . ? HN2B N2 HN2C 106(6) . . ? C3 N3 HN3A 105(4) . . ? C3 N3 HN3B 111(4) . . ? HN3A N3 HN3B 117(5) . . ? C3 N3 HN3C 107(4) . . ? HN3A N3 HN3C 106(6) . . ? HN3B N3 HN3C 111(6) . . ? N3 C3 C3 110.1(6) . 3_566 ? N3 C3 HC3A 105(4) . . ? C3 C3 HC3A 115(4) 3_566 . ? N3 C3 HC3B 104(4) . . ? C3 C3 HC3B 111(4) 3_566 . ? HC3A C3 HC3B 111(6) . . ? H21 OW2 H22 109(9) . . ? H31 OW3 H32 105(8) . . ? 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 OW1 H11 OW3 0.95(2) 2.30(4) 3.167(10) 153(6) 1_554 OW1 H12 O14 0.95(2) 1.75(3) 2.681(6) 165(7) . OW2 H21 O12 0.96(2) 1.84(3) 2.785(7) 170(10) 2_656 OW2 H22 O11 0.95(2) 1.84(4) 2.759(7) 162(9) 4_566 OW3 H31 OW2 0.95(2) 1.93(4) 2.856(8) 162(9) 2_646 OW3 H32 O22 0.95(2) 2.11(6) 2.896(7) 140(7) 1_556 N1 HN1A O12 0.98(2) 1.88(2) 2.846(7) 173(5) 2_656 N1 HN1B OW3 0.98(2) 1.92(3) 2.884(9) 166(7) 2_556 N1 HN1C O33 0.98(2) 2.12(2) 3.095(7) 172(7) 2_556 N2 HN2A O32 0.97(2) 2.13(4) 3.000(7) 148(5) 2 N2 HN2B O24 0.98(2) 2.14(5) 2.966(6) 140(6) 3_566 N2 HN2C O21 0.98(2) 1.99(2) 2.971(6) 177(6) 3_666 N3 HN3A O14 0.97(2) 1.87(2) 2.840(6) 178(7) 2_655 N3 HN3B O34 0.96(2) 2.31(5) 2.977(7) 126(5) 4_466 N3 HN3C OW2 0.97(2) 1.85(4) 2.755(8) 155(6) 3_566 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.620 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.203 data_job _database_code_CSD 183663 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'lanthanum piperazine sulfate dihydrate' _chemical_melting_point ? _chemical_formula_moiety 'La2 (H2 O)2 (C4 H12 N2) (S1 O4)4' _chemical_formula_sum 'C4 H16 La2 N2 O18 S4' _chemical_formula_weight 786.25 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 'P 1 21/c 1' 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 16.7936(2) _cell_length_b 9.58580(10) _cell_length_c 22.5827(3) _cell_angle_alpha 90.000(5) _cell_angle_beta 104.2164(4) _cell_angle_gamma 90.000(5) _cell_volume 3524.03(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12149 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 32.032 _exptl_crystal_description 'Plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.255 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.0375 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 5.359 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.40164 _exptl_absorpt_correction_T_max 0.81193 _exptl_absorpt_process_details 'N.W. Alcock (1970). Cryst. Computing, p271)' _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_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53463 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 32.04 _reflns_number_total 12271 _reflns_number_gt 8634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0547P)^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 SHELXL _refine_ls_extinction_coef 0.00021(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12271 _refine_ls_number_parameters 572 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.067 _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 0.574340(16) 0.27607(3) 0.181449(12) 0.01379(7) Uani 1 1 d . . . La2 La 0.738707(17) 0.77010(3) 0.047694(13) 0.01492(7) Uani 1 1 d . . . La3 La 1.031282(17) 0.73901(3) 0.083823(13) 0.01497(7) Uani 1 1 d . . . La4 La 0.828767(18) 0.20478(3) 0.129468(13) 0.01584(7) Uani 1 1 d . . . S1 S 0.86993(7) 0.47847(11) 0.01512(5) 0.0149(2) Uani 1 1 d . . . S2 S 0.65781(7) 1.03346(11) 0.10686(5) 0.0147(2) Uani 1 1 d . . . S3 S 0.87609(8) 0.99663(12) -0.00147(6) 0.0203(3) Uani 1 1 d . . . S4 S 0.79962(8) 0.29525(12) 0.28044(6) 0.0187(2) Uani 1 1 d . . . S5 S 0.51097(8) 0.03579(11) 0.25907(5) 0.0168(2) Uani 1 1 d . . . S6 S 0.67868(8) 0.51341(11) 0.11587(6) 0.0169(2) Uani 1 1 d . . . S7 S 0.41236(7) 0.25083(11) 0.07203(5) 0.0158(2) Uani 1 1 d . . . S8 S 0.91001(7) 0.83357(11) 0.17018(6) 0.0161(2) Uani 1 1 d . . . O11 O 0.8344(3) 0.3798(5) 0.0494(2) 0.0596(15) Uani 1 1 d . . . O12 O 0.8147(3) 0.5982(4) 0.00157(19) 0.0428(12) Uani 1 1 d . . . O13 O 0.9506(2) 0.5214(4) 0.05003(19) 0.0335(10) Uani 1 1 d . . . O14 O 0.8747(2) 0.4153(4) -0.04324(17) 0.0264(8) Uani 1 1 d . . . O21 O 0.6997(2) 1.1051(3) 0.16393(15) 0.0188(7) Uani 1 1 d . . . O22 O 0.6592(2) 0.8818(3) 0.11597(17) 0.0218(7) Uani 1 1 d . . . O23 O 0.7077(2) 0.0624(4) 0.06174(16) 0.0237(8) Uani 1 1 d . . . O24 O 0.5752(2) 0.0892(3) 0.08691(17) 0.0234(8) Uani 1 1 d . . . O31 O 0.7970(2) 0.9235(4) -0.01667(17) 0.0256(8) Uani 1 1 d . . . O32 O 0.8898(3) 1.0646(4) -0.05472(18) 0.0365(10) Uani 1 1 d . . . O33A O 0.9356(5) 0.9220(8) 0.0381(4) 0.0339(14) Uani 0.50 1 d P . . O33B O 0.9390(5) 0.8719(8) 0.0031(4) 0.0339(14) Uani 0.50 1 d P . . O34A O 0.8944(5) 1.0644(7) 0.0556(4) 0.0279(13) Uani 0.50 1 d P . . O34B O 0.8583(5) 1.1284(7) 0.0324(4) 0.0279(13) Uani 0.50 1 d P . . O41 O 0.8290(2) 0.2452(4) 0.34375(18) 0.0286(9) Uani 1 1 d . . . O42 O 0.8366(2) 0.2050(3) 0.24077(16) 0.0199(7) Uani 1 1 d . . . O43 O 0.8258(3) 0.4394(4) 0.2747(2) 0.0377(10) Uani 1 1 d . . . O44 O 0.7102(2) 0.2855(4) 0.26274(18) 0.0307(9) Uani 1 1 d . . . O51 O 0.5485(2) -0.0377(4) 0.31585(16) 0.0258(8) Uani 1 1 d . . . O52 O 0.5588(2) 0.0189(3) 0.21305(16) 0.0214(7) Uani 1 1 d . . . O53 O 0.5716(2) 0.4770(3) 0.26290(17) 0.0233(8) Uani 1 1 d . . . O54 O 0.5091(2) 0.1893(3) 0.26952(16) 0.0229(8) Uani 1 1 d . . . O61 O 0.7030(2) 0.3665(4) 0.1148(2) 0.0385(11) Uani 1 1 d . . . O62 O 0.6188(2) 0.5182(4) 0.15279(17) 0.0301(9) Uani 1 1 d . . . O63 O 0.6437(2) 0.5643(3) 0.05375(16) 0.0222(8) Uani 1 1 d . . . O64 O 0.7493(2) 0.6040(3) 0.14145(17) 0.0249(8) Uani 1 1 d . . . O71 O 0.3973(2) 0.1552(3) 0.01932(16) 0.0217(7) Uani 1 1 d . . . O72 O 0.4834(2) 0.3412(3) 0.07512(15) 0.0182(7) Uani 1 1 d . . . O73 O 0.4286(2) 0.1722(3) 0.12997(16) 0.0199(7) Uani 1 1 d . . . O74 O 0.3356(2) 0.3330(3) 0.06386(16) 0.0213(7) Uani 1 1 d . . . O81 O 0.8505(3) 0.9486(4) 0.1554(2) 0.0453(12) Uani 1 1 d . . . O82 O 0.9048(3) 0.7680(4) 0.2262(2) 0.0392(11) Uani 1 1 d . . . O83 O 0.8885(2) 0.7337(4) 0.11813(19) 0.0297(9) Uani 1 1 d . . . O84 O 0.9942(2) 0.8810(3) 0.17192(17) 0.0228(8) Uani 1 1 d . . . C11 C 0.5538(4) 0.3355(6) -0.0474(3) 0.0374(15) Uani 1 1 d . . . H11A H 0.5235 0.3980 -0.0787 0.056 Uiso 1 1 calc R . . H11B H 0.5392 0.3583 -0.0095 0.056 Uiso 1 1 calc R . . N12 N 0.6408(4) 0.3593(7) -0.0396(4) 0.074(2) Uani 1 1 d D . . H12A H 0.6701 0.3222 0.0008 0.110 Uiso 1 1 calc RD . . H12B H 0.6504 0.4613 -0.0390 0.110 Uiso 1 1 calc RD . . C13 C 0.6768(4) 0.2982(6) -0.0856(4) 0.0436(17) Uani 1 1 d . . . H13A H 0.7361 0.3002 -0.0706 0.065 Uiso 1 1 calc R . . H13B H 0.6627 0.3561 -0.1219 0.065 Uiso 1 1 calc R . . C14 C 0.6517(4) 0.1548(6) -0.1029(3) 0.0365(14) Uani 1 1 d . . . H14A H 0.6796 0.0918 -0.0709 0.055 Uiso 1 1 calc R . . H14B H 0.6681 0.1308 -0.1400 0.055 Uiso 1 1 calc R . . N15 N 0.5626(4) 0.1361(6) -0.1132(3) 0.0534(16) Uani 1 1 d D . . H15A H 0.5351 0.1823 -0.1521 0.080 Uiso 1 1 calc RD . . H15B H 0.5499 0.0352 -0.1178 0.080 Uiso 1 1 calc RD . . C16 C 0.5284(4) 0.1917(6) -0.0644(3) 0.0393(15) Uani 1 1 d . . . H16A H 0.5455 0.1326 -0.0286 0.059 Uiso 1 1 calc R . . H16B H 0.4690 0.1881 -0.0774 0.059 Uiso 1 1 calc R . . C21 C 0.8138(5) 0.7684(6) 0.3657(3) 0.0480(19) Uani 1 1 d . . . H21A H 0.8338 0.7614 0.4097 0.072 Uiso 1 1 calc R . . H21B H 0.8607 0.7637 0.3479 0.072 Uiso 1 1 calc R . . C22 C 0.7588(4) 0.6500(5) 0.3433(3) 0.0313(13) Uani 1 1 d . . . H22A H 0.7157 0.6476 0.3651 0.047 Uiso 1 1 calc R . . H22B H 0.7897 0.5638 0.3520 0.047 Uiso 1 1 calc R . . N23 N 0.7208(4) 0.6589(5) 0.2764(3) 0.0435(14) Uani 1 1 d D . . H23A H 0.7635 0.6413 0.2539 0.065 Uiso 1 1 calc RD . . H23B H 0.6785 0.5852 0.2649 0.065 Uiso 1 1 calc RD . . C24 C 0.6832(5) 0.7935(6) 0.2583(3) 0.0480(18) Uani 1 1 d . . . H24A H 0.6337 0.8014 0.2730 0.072 Uiso 1 1 calc R . . H24B H 0.6671 0.7982 0.2141 0.072 Uiso 1 1 calc R . . C25 C 0.7391(4) 0.9165(6) 0.2824(3) 0.0422(16) Uani 1 1 d . . . H25A H 0.7842 0.9190 0.2625 0.063 Uiso 1 1 calc R . . H25B H 0.7086 1.0029 0.2733 0.063 Uiso 1 1 calc R . . N26 N 0.7725(4) 0.9023(5) 0.3503(3) 0.0506(16) Uani 1 1 d D . . H26A H 0.8118 0.9789 0.3653 0.076 Uiso 1 1 calc RD . . H26B H 0.7269 0.9103 0.3708 0.076 Uiso 1 1 calc RD . . OW31 O 1.0510(3) 0.5531(4) 0.16954(18) 0.0317(9) Uani 1 1 d D . . H31A H 1.004(2) 0.498(6) 0.172(2) 0.047 Uiso 1 1 d D . . H31B H 1.082(3) 0.576(6) 0.2097(11) 0.047 Uiso 1 1 d D . . OW32 O 0.9795(7) 0.7291(8) -0.0361(4) 0.109(3) Uani 1 1 d D . . H32A H 0.978(8) 0.649(6) -0.062(4) 0.163 Uiso 1 1 d D . . H32B H 0.980(9) 0.812(5) -0.061(4) 0.163 Uiso 1 1 d D . . OW41 O 0.8984(2) 0.4382(3) 0.17969(17) 0.0242(8) Uani 1 1 d D . . H41A H 0.892(3) 0.441(5) 0.2207(10) 0.036 Uiso 1 1 d D . . H41B H 0.862(3) 0.508(4) 0.1579(19) 0.036 Uiso 1 1 d D . . OW42 O 0.9829(2) 0.1714(4) 0.1720(2) 0.0324(9) Uani 1 1 d D . . H42A H 1.016(3) 0.218(5) 0.207(2) 0.049 Uiso 1 1 d D . . H42B H 1.001(3) 0.077(2) 0.172(3) 0.049 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 0.01413(15) 0.01284(13) 0.01408(15) -0.00009(9) 0.00283(11) -0.00049(8) La2 0.01555(15) 0.01313(13) 0.01708(15) 0.00186(9) 0.00592(11) 0.00034(9) La3 0.01418(15) 0.01605(13) 0.01517(15) 0.00027(9) 0.00452(11) 0.00208(9) La4 0.01874(15) 0.01423(13) 0.01505(15) -0.00114(9) 0.00512(11) -0.00256(9) S1 0.0163(6) 0.0135(5) 0.0156(6) -0.0006(4) 0.0049(4) 0.0009(4) S2 0.0151(6) 0.0142(5) 0.0156(6) -0.0019(4) 0.0054(5) 0.0004(4) S3 0.0214(7) 0.0220(6) 0.0176(6) 0.0047(4) 0.0052(5) -0.0055(4) S4 0.0163(6) 0.0241(6) 0.0146(6) -0.0030(4) 0.0016(5) 0.0061(4) S5 0.0219(6) 0.0136(5) 0.0162(6) 0.0027(4) 0.0075(5) -0.0010(4) S6 0.0187(6) 0.0122(5) 0.0196(6) 0.0026(4) 0.0046(5) -0.0027(4) S7 0.0140(6) 0.0185(5) 0.0136(6) 0.0001(4) 0.0013(5) -0.0007(4) S8 0.0162(6) 0.0164(5) 0.0160(6) 0.0006(4) 0.0046(5) 0.0029(4) O11 0.074(4) 0.066(3) 0.040(3) 0.023(2) 0.016(3) -0.032(3) O12 0.050(3) 0.044(2) 0.029(2) -0.0095(18) -0.002(2) 0.031(2) O13 0.021(2) 0.045(2) 0.033(2) -0.0197(18) 0.0042(17) -0.0045(17) O14 0.021(2) 0.034(2) 0.026(2) -0.0164(15) 0.0082(16) -0.0004(15) O21 0.0217(19) 0.0199(16) 0.0161(18) -0.0045(13) 0.0071(14) -0.0031(13) O22 0.0236(19) 0.0151(16) 0.028(2) -0.0019(13) 0.0094(16) 0.0023(13) O23 0.024(2) 0.0304(19) 0.0196(19) -0.0058(14) 0.0102(16) -0.0040(14) O24 0.0192(19) 0.0229(18) 0.028(2) 0.0005(14) 0.0046(16) 0.0042(13) O31 0.022(2) 0.0278(19) 0.029(2) -0.0016(15) 0.0111(17) -0.0107(14) O32 0.036(2) 0.053(3) 0.019(2) 0.0120(18) 0.0033(18) -0.0188(19) O33A 0.036(3) 0.032(3) 0.034(4) 0.013(3) 0.008(3) 0.017(3) O33B 0.036(3) 0.032(3) 0.034(4) 0.013(3) 0.008(3) 0.017(3) O34A 0.043(4) 0.018(3) 0.026(3) -0.005(2) 0.015(3) 0.001(2) O34B 0.043(4) 0.018(3) 0.026(3) -0.005(2) 0.015(3) 0.001(2) O41 0.021(2) 0.049(2) 0.015(2) -0.0030(16) 0.0023(16) 0.0111(16) O42 0.0200(19) 0.0236(17) 0.0156(18) -0.0020(13) 0.0036(15) 0.0051(13) O43 0.044(3) 0.021(2) 0.052(3) -0.0078(17) 0.018(2) 0.0022(16) O44 0.016(2) 0.054(3) 0.021(2) -0.0091(17) 0.0021(16) 0.0054(16) O51 0.032(2) 0.0261(19) 0.019(2) 0.0062(14) 0.0066(17) 0.0024(15) O52 0.027(2) 0.0188(17) 0.0207(19) 0.0034(13) 0.0107(16) 0.0001(13) O53 0.025(2) 0.0191(17) 0.027(2) 0.0005(14) 0.0091(16) 0.0065(13) O54 0.031(2) 0.0173(17) 0.022(2) -0.0001(13) 0.0094(16) -0.0011(14) O61 0.033(2) 0.0165(19) 0.060(3) 0.0057(17) -0.001(2) 0.0000(15) O62 0.034(2) 0.034(2) 0.027(2) -0.0011(16) 0.0156(18) -0.0129(16) O63 0.027(2) 0.0213(17) 0.0171(19) 0.0038(13) 0.0027(15) -0.0054(13) O64 0.022(2) 0.0214(18) 0.029(2) 0.0065(14) 0.0009(16) -0.0076(14) O71 0.0188(19) 0.0221(17) 0.021(2) -0.0039(13) -0.0010(15) 0.0005(13) O72 0.0183(18) 0.0163(16) 0.0189(18) 0.0008(12) 0.0025(14) -0.0019(12) O73 0.0192(19) 0.0211(17) 0.0191(19) 0.0026(13) 0.0038(14) -0.0022(13) O74 0.0173(19) 0.0264(18) 0.0189(19) -0.0010(14) 0.0020(15) 0.0043(13) O81 0.026(2) 0.026(2) 0.093(4) 0.023(2) 0.030(2) 0.0151(16) O82 0.038(3) 0.054(3) 0.023(2) 0.0105(18) 0.005(2) -0.002(2) O83 0.016(2) 0.048(2) 0.027(2) -0.0195(17) 0.0083(17) -0.0096(16) O84 0.0173(19) 0.0214(17) 0.029(2) -0.0094(14) 0.0052(15) -0.0035(13) C11 0.030(3) 0.035(3) 0.052(4) -0.014(3) 0.017(3) 0.003(2) N12 0.064(5) 0.069(4) 0.098(6) -0.055(4) 0.040(4) -0.031(4) C13 0.025(3) 0.045(4) 0.067(5) -0.015(3) 0.022(3) -0.007(3) C14 0.040(4) 0.035(3) 0.037(4) -0.013(3) 0.014(3) 0.007(2) N15 0.055(4) 0.035(3) 0.071(5) -0.022(3) 0.017(3) -0.015(3) C16 0.036(4) 0.044(4) 0.042(4) -0.005(3) 0.016(3) -0.011(3) C21 0.061(5) 0.044(4) 0.027(4) 0.006(3) -0.012(3) -0.001(3) C22 0.046(4) 0.024(3) 0.023(3) 0.001(2) 0.006(3) 0.012(2) N23 0.051(4) 0.038(3) 0.035(3) -0.004(2) -0.002(3) 0.005(2) C24 0.057(5) 0.040(4) 0.042(4) 0.003(3) 0.003(4) 0.016(3) C25 0.045(4) 0.031(3) 0.049(4) 0.019(3) 0.007(3) 0.002(3) N26 0.074(4) 0.037(3) 0.041(4) -0.004(2) 0.012(3) -0.017(3) OW31 0.031(2) 0.038(2) 0.023(2) 0.0050(16) 0.0006(18) -0.0123(17) OW32 0.112(7) 0.107(6) 0.103(7) -0.011(5) 0.019(6) -0.009(5) OW41 0.026(2) 0.0216(18) 0.025(2) -0.0029(14) 0.0055(16) -0.0026(14) OW42 0.027(2) 0.0228(19) 0.042(3) -0.0076(16) -0.0022(19) 0.0031(15) _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 O44 2.555(4) . ? La1 O62 2.569(3) . ? La1 O72 2.586(3) . ? La1 O52 2.597(3) . ? La1 O54 2.631(4) . ? La1 O73 2.634(3) . ? La1 O53 2.672(3) . ? La1 O51 2.740(4) 2_655 ? La1 O21 2.772(3) 1_545 ? La1 O24 2.790(4) . ? La1 S7 3.2036(12) . ? La1 S5 3.2291(11) . ? La2 O31 2.436(3) . ? La2 O12 2.466(4) . ? La2 O22 2.513(3) . ? La2 O71 2.515(3) 3_665 ? La2 O63 2.561(3) . ? La2 O64 2.620(3) . ? La2 O83 2.649(4) . ? La2 O74 2.709(3) 3_665 ? La2 O23 2.881(3) 1_565 ? La2 S6 3.1943(11) . ? La2 S7 3.2275(12) 3_665 ? La2 S2 3.3008(11) . ? La3 O33A 2.431(7) . ? La3 O33B 2.441(8) . ? La3 O32 2.482(4) 3_775 ? La3 O14 2.497(3) 3_765 ? La3 O13 2.502(4) . ? La3 O41 2.510(4) 2_755 ? La3 OW31 2.592(4) . ? La3 O84 2.609(3) . ? La3 OW32 2.634(9) . ? La3 O83 2.695(4) . ? La3 S8 3.2747(12) . ? La4 O34B 2.475(7) 1_545 ? La4 O42 2.485(4) . ? La4 O11 2.486(4) . ? La4 O81 2.530(4) 1_545 ? La4 OW42 2.550(4) . ? La4 O61 2.574(4) . ? La4 O34A 2.591(7) 1_545 ? La4 O23 2.609(3) . ? La4 OW41 2.648(3) . ? La4 O21 2.654(3) 1_545 ? La4 S2 3.2373(12) 1_545 ? S1 O11 1.441(4) . ? S1 O13 1.450(4) . ? S1 O12 1.460(4) . ? S1 O14 1.470(4) . ? S2 O24 1.451(4) 1_565 ? S2 O22 1.468(3) . ? S2 O21 1.477(3) . ? S2 O23 1.496(4) 1_565 ? S2 La4 3.2373(12) 1_565 ? S2 La1 3.3721(11) 1_565 ? S3 O33A 1.367(8) . ? S3 O34A 1.407(8) . ? S3 O32 1.435(4) . ? S3 O31 1.465(4) . ? S3 O34B 1.543(7) . ? S3 O33B 1.582(8) . ? S4 O44 1.459(4) . ? S4 O43 1.465(4) . ? S4 O41 1.474(4) . ? S4 O42 1.487(3) . ? S5 O51 1.463(4) . ? S5 O53 1.466(4) 2_645 ? S5 O52 1.470(4) . ? S5 O54 1.492(3) . ? S5 La1 3.3166(11) 2_645 ? S6 O62 1.456(4) . ? S6 O63 1.465(4) . ? S6 O61 1.468(4) . ? S6 O64 1.469(4) . ? S7 O72 1.462(3) . ? S7 O71 1.474(3) . ? S7 O73 1.476(4) . ? S7 O74 1.483(3) . ? S7 La2 3.2275(12) 3_665 ? S8 O82 1.433(4) . ? S8 O81 1.471(4) . ? S8 O84 1.477(4) . ? S8 O83 1.490(4) . ? O14 La3 2.497(3) 3_765 ? O21 La4 2.654(3) 1_565 ? O21 La1 2.772(3) 1_565 ? O23 S2 1.496(4) 1_545 ? O23 La2 2.881(3) 1_545 ? O24 S2 1.451(4) 1_545 ? O32 La3 2.482(4) 3_775 ? O33A O33B 0.937(11) . ? O33A O34A 1.623(11) . ? O34A O34B 0.929(10) . ? O34A La4 2.591(7) 1_565 ? O34B La4 2.475(7) 1_565 ? O41 La3 2.510(4) 2_745 ? O51 La1 2.740(4) 2_645 ? O53 S5 1.466(4) 2_655 ? O71 La2 2.515(3) 3_665 ? O74 La2 2.709(3) 3_665 ? O81 La4 2.530(4) 1_565 ? C11 N12 1.446(8) . ? C11 C16 1.466(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N12 C13 1.448(9) . ? N12 H12A 0.9900 . ? N12 H12B 0.9900 . ? C13 C14 1.463(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N15 1.467(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? N15 C16 1.463(8) . ? N15 H15A 0.9900 . ? N15 H15B 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C21 N26 1.460(8) . ? C21 C22 1.472(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N23 1.491(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N23 C24 1.451(8) . ? N23 H23A 0.9900 . ? N23 H23B 0.9900 . ? C24 C25 1.522(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N26 1.504(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N26 H26A 0.9900 . ? N26 H26B 0.9900 . ? OW31 H31A 0.958(12) . ? OW31 H31B 0.951(12) . ? OW32 H32A 0.969(12) . ? OW32 H32B 0.972(12) . ? OW41 H41A 0.961(12) . ? OW41 H41B 0.963(12) . ? OW42 H42A 0.961(12) . ? OW42 H42B 0.953(12) . ? 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 O44 La1 O62 83.41(13) . . ? O44 La1 O72 151.43(12) . . ? O62 La1 O72 71.94(11) . . ? O44 La1 O52 88.20(12) . . ? O62 La1 O52 169.01(12) . . ? O72 La1 O52 114.08(10) . . ? O44 La1 O54 86.13(13) . . ? O62 La1 O54 132.62(11) . . ? O72 La1 O54 121.17(11) . . ? O52 La1 O54 53.37(10) . . ? O44 La1 O73 154.13(12) . . ? O62 La1 O73 121.77(11) . . ? O72 La1 O73 53.73(10) . . ? O52 La1 O73 67.50(11) . . ? O54 La1 O73 72.51(11) . . ? O44 La1 O53 69.08(11) . . ? O62 La1 O53 65.00(11) . . ? O72 La1 O53 111.04(10) . . ? O52 La1 O53 118.38(10) . . ? O54 La1 O53 68.09(10) . . ? O73 La1 O53 113.91(11) . . ? O44 La1 O51 120.36(11) . 2_655 ? O62 La1 O51 71.60(12) . 2_655 ? O72 La1 O51 65.60(10) . 2_655 ? O52 La1 O51 119.02(11) . 2_655 ? O54 La1 O51 74.54(11) . 2_655 ? O73 La1 O51 68.46(10) . 2_655 ? O53 La1 O51 51.30(11) . 2_655 ? O44 La1 O21 63.12(11) . 1_545 ? O62 La1 O21 102.71(11) . 1_545 ? O72 La1 O21 107.85(10) . 1_545 ? O52 La1 O21 67.00(10) . 1_545 ? O54 La1 O21 113.14(10) . 1_545 ? O73 La1 O21 111.69(10) . 1_545 ? O53 La1 O21 131.80(10) . 1_545 ? O51 La1 O21 172.19(10) 2_655 1_545 ? O44 La1 O24 113.64(11) . . ? O62 La1 O24 109.31(11) . . ? O72 La1 O24 63.74(10) . . ? O52 La1 O24 67.70(11) . . ? O54 La1 O24 117.19(10) . . ? O73 La1 O24 66.32(10) . . ? O53 La1 O24 173.77(10) . . ? O51 La1 O24 125.51(10) 2_655 . ? O21 La1 O24 50.52(10) 1_545 . ? O44 La1 S7 175.05(9) . . ? O62 La1 S7 96.79(9) . . ? O72 La1 S7 26.62(7) . . ? O52 La1 S7 90.95(8) . . ? O54 La1 S7 97.28(8) . . ? O73 La1 S7 27.12(7) . . ? O53 La1 S7 115.52(8) . . ? O51 La1 S7 64.21(8) 2_655 . ? O21 La1 S7 112.09(7) 1_545 . ? O24 La1 S7 61.59(7) . . ? O44 La1 S5 89.46(10) . . ? O62 La1 S5 159.41(9) . . ? O72 La1 S5 118.56(7) . . ? O52 La1 S5 26.50(8) . . ? O54 La1 S5 27.11(7) . . ? O73 La1 S5 64.88(8) . . ? O53 La1 S5 94.41(8) . . ? O51 La1 S5 95.87(8) 2_655 . ? O21 La1 S5 91.08(7) 1_545 . ? O24 La1 S5 91.25(7) . . ? S7 La1 S5 91.96(3) . . ? O31 La2 O12 79.96(15) . . ? O31 La2 O22 117.43(11) . . ? O12 La2 O22 162.13(13) . . ? O31 La2 O71 84.73(12) . 3_665 ? O12 La2 O71 115.09(12) . 3_665 ? O22 La2 O71 72.97(11) . 3_665 ? O31 La2 O63 147.53(11) . . ? O12 La2 O63 84.37(14) . . ? O22 La2 O63 82.18(11) . . ? O71 La2 O63 76.45(11) 3_665 . ? O31 La2 O64 153.08(12) . . ? O12 La2 O64 89.76(13) . . ? O22 La2 O64 72.78(11) . . ? O71 La2 O64 122.05(11) 3_665 . ? O63 La2 O64 53.73(11) . . ? O31 La2 O83 88.62(13) . . ? O12 La2 O83 69.62(13) . . ? O22 La2 O83 104.89(12) . . ? O71 La2 O83 170.91(11) 3_665 . ? O63 La2 O83 112.25(12) . . ? O64 La2 O83 64.45(12) . . ? O31 La2 O74 80.00(11) . 3_665 ? O12 La2 O74 62.07(12) . 3_665 ? O22 La2 O74 122.23(11) . 3_665 ? O71 La2 O74 53.21(10) 3_665 3_665 ? O63 La2 O74 67.53(10) . 3_665 ? O64 La2 O74 117.00(10) . 3_665 ? O83 La2 O74 131.54(11) . 3_665 ? O31 La2 O23 65.70(11) . 1_565 ? O12 La2 O23 145.31(14) . 1_565 ? O22 La2 O23 51.74(10) . 1_565 ? O71 La2 O23 68.14(10) 3_665 1_565 ? O63 La2 O23 127.69(10) . 1_565 ? O64 La2 O23 118.70(11) . 1_565 ? O83 La2 O23 103.44(11) . 1_565 ? O74 La2 O23 113.76(10) 3_665 1_565 ? O31 La2 S6 166.75(9) . . ? O12 La2 S6 86.93(12) . . ? O22 La2 S6 75.79(8) . . ? O71 La2 S6 99.30(8) 3_665 . ? O63 La2 S6 26.70(8) . . ? O64 La2 S6 27.03(8) . . ? O83 La2 S6 88.56(9) . . ? O74 La2 S6 92.25(8) 3_665 . ? O23 La2 S6 127.52(7) 1_565 . ? O31 La2 S7 83.47(9) . 3_665 ? O12 La2 S7 89.24(10) . 3_665 ? O22 La2 S7 96.53(9) . 3_665 ? O71 La2 S7 26.17(8) 3_665 3_665 ? O63 La2 S7 67.99(8) . 3_665 ? O64 La2 S7 121.50(8) . 3_665 ? O83 La2 S7 158.46(8) . 3_665 ? O74 La2 S7 27.18(7) 3_665 3_665 ? O23 La2 S7 91.53(7) 1_565 3_665 ? S6 La2 S7 94.57(3) . 3_665 ? O31 La2 S2 92.61(9) . . ? O12 La2 S2 171.52(12) . . ? O22 La2 S2 24.83(8) . . ? O71 La2 S2 67.82(8) 3_665 . ? O63 La2 S2 104.11(8) . . ? O64 La2 S2 95.20(8) . . ? O83 La2 S2 106.40(8) . . ? O74 La2 S2 120.94(7) 3_665 . ? O23 La2 S2 26.92(7) 1_565 . ? S6 La2 S2 100.61(3) . . ? S7 La2 S2 93.99(3) 3_665 . ? O33A La3 O33B 22.2(2) . . ? O33A La3 O32 71.4(2) . 3_775 ? O33B La3 O32 71.9(2) . 3_775 ? O33A La3 O14 133.1(2) . 3_765 ? O33B La3 O14 112.2(2) . 3_765 ? O32 La3 O14 85.72(14) 3_775 3_765 ? O33A La3 O13 102.7(2) . . ? O33B La3 O13 90.6(2) . . ? O32 La3 O13 146.70(14) 3_775 . ? O14 La3 O13 74.80(12) 3_765 . ? O33A La3 O41 132.4(2) . 2_755 ? O33B La3 O41 142.6(2) . 2_755 ? O32 La3 O41 71.34(12) 3_775 2_755 ? O14 La3 O41 71.27(13) 3_765 2_755 ? O13 La3 O41 124.61(13) . 2_755 ? O33A La3 OW31 139.8(2) . . ? O33B La3 OW31 149.1(2) . . ? O32 La3 OW31 137.79(13) 3_775 . ? O14 La3 OW31 83.70(13) 3_765 . ? O13 La3 OW31 67.35(13) . . ? O41 La3 OW31 66.55(12) 2_755 . ? O33A La3 O84 72.0(2) . . ? O33B La3 O84 94.0(2) . . ? O32 La3 O84 92.81(13) 3_775 . ? O14 La3 O84 151.63(12) 3_765 . ? O13 La3 O84 117.07(12) . . ? O41 La3 O84 81.40(12) 2_755 . ? OW31 La3 O84 78.46(12) . . ? O33A La3 OW32 64.7(3) . . ? O33B La3 OW32 42.5(3) . . ? O32 La3 OW32 79.5(2) 3_775 . ? O14 La3 OW32 71.4(2) 3_765 . ? O13 La3 OW32 68.9(2) . . ? O41 La3 OW32 133.7(2) 2_755 . ? OW31 La3 OW32 133.8(2) . . ? O84 La3 OW32 136.2(2) . . ? O33A La3 O83 66.0(2) . . ? O33B La3 O83 77.2(2) . . ? O32 La3 O83 131.37(13) 3_775 . ? O14 La3 O83 141.44(11) 3_765 . ? O13 La3 O83 67.60(12) . . ? O41 La3 O83 124.64(13) 2_755 . ? OW31 La3 O83 74.46(13) . . ? O84 La3 O83 52.76(11) . . ? OW32 La3 O83 101.7(2) . . ? O33A La3 S8 67.1(2) . . ? O33B La3 S8 85.8(2) . . ? O32 La3 S8 113.47(11) 3_775 . ? O14 La3 S8 157.61(9) 3_765 . ? O13 La3 S8 92.48(9) . . ? O41 La3 S8 102.94(10) 2_755 . ? OW31 La3 S8 74.32(10) . . ? O84 La3 S8 26.06(8) . . ? OW32 La3 S8 121.7(2) . . ? O83 La3 S8 26.71(8) . . ? O34B La4 O42 157.6(2) 1_545 . ? O34B La4 O11 60.2(2) 1_545 . ? O42 La4 O11 137.17(15) . . ? O34B La4 O81 82.5(2) 1_545 1_545 ? O42 La4 O81 78.35(14) . 1_545 ? O11 La4 O81 142.60(18) . 1_545 ? O34B La4 OW42 83.7(2) 1_545 . ? O42 La4 OW42 79.77(13) . . ? O11 La4 OW42 98.17(16) . . ? O81 La4 OW42 73.50(13) 1_545 . ? O34B La4 O61 113.6(2) 1_545 . ? O42 La4 O61 88.15(13) . . ? O11 La4 O61 71.12(17) . . ? O81 La4 O61 132.94(12) 1_545 . ? OW42 La4 O61 148.04(12) . . ? O34B La4 O34A 21.0(2) 1_545 1_545 ? O42 La4 O34A 136.62(19) . 1_545 ? O11 La4 O34A 77.5(2) . 1_545 ? O81 La4 O34A 65.5(2) 1_545 1_545 ? OW42 La4 O34A 68.0(2) . 1_545 ? O61 La4 O34A 134.0(2) . 1_545 ? O34B La4 O23 67.8(2) 1_545 . ? O42 La4 O23 115.70(11) . . ? O11 La4 O23 95.17(14) . . ? O81 La4 O23 71.04(13) 1_545 . ? OW42 La4 O23 136.71(11) . . ? O61 La4 O23 75.13(12) . . ? O34A La4 O23 75.2(2) 1_545 . ? O34B La4 OW41 117.77(19) 1_545 . ? O42 La4 OW41 69.99(11) . . ? O11 La4 OW41 69.47(15) . . ? O81 La4 OW41 134.26(14) 1_545 . ? OW42 La4 OW41 69.14(11) . . ? O61 La4 OW41 78.94(12) . . ? O34A La4 OW41 120.14(19) 1_545 . ? O23 La4 OW41 153.10(11) . . ? O34B La4 O21 120.6(2) 1_545 1_545 ? O42 La4 O21 63.12(11) . 1_545 ? O11 La4 O21 129.49(15) . 1_545 ? O81 La4 O21 70.40(11) 1_545 1_545 ? OW42 La4 O21 132.14(12) . 1_545 ? O61 La4 O21 63.35(11) . 1_545 ? O34A La4 O21 120.59(18) 1_545 1_545 ? O23 La4 O21 53.76(10) . 1_545 ? OW41 La4 O21 119.02(10) . 1_545 ? O34B La4 S2 94.20(19) 1_545 1_545 ? O42 La4 S2 89.12(9) . 1_545 ? O11 La4 S2 114.74(12) . 1_545 ? O81 La4 S2 67.41(10) 1_545 1_545 ? OW42 La4 S2 140.77(9) . 1_545 ? O61 La4 S2 67.52(8) . 1_545 ? O34A La4 S2 97.80(18) 1_545 1_545 ? O23 La4 S2 27.01(8) . 1_545 ? OW41 La4 S2 141.04(8) . 1_545 ? O21 La4 S2 26.78(7) 1_545 1_545 ? O11 S1 O13 110.4(3) . . ? O11 S1 O12 107.7(3) . . ? O13 S1 O12 110.6(2) . . ? O11 S1 O14 109.4(3) . . ? O13 S1 O14 110.8(2) . . ? O12 S1 O14 107.9(2) . . ? O24 S2 O22 112.9(2) 1_565 . ? O24 S2 O21 108.3(2) 1_565 . ? O22 S2 O21 110.5(2) . . ? O24 S2 O23 111.9(2) 1_565 1_565 ? O22 S2 O23 106.7(2) . 1_565 ? O21 S2 O23 106.4(2) . 1_565 ? O24 S2 La4 127.25(15) 1_565 1_565 ? O22 S2 La4 119.81(15) . 1_565 ? O21 S2 La4 54.04(13) . 1_565 ? O23 S2 La4 52.39(14) 1_565 1_565 ? O24 S2 La2 127.80(15) 1_565 . ? O22 S2 La2 45.98(14) . . ? O21 S2 La2 123.62(14) . . ? O23 S2 La2 60.71(13) 1_565 . ? La4 S2 La2 90.84(3) 1_565 . ? O24 S2 La1 54.43(15) 1_565 1_565 ? O22 S2 La1 127.41(15) . 1_565 ? O21 S2 La1 53.90(13) . 1_565 ? O23 S2 La1 125.71(14) 1_565 1_565 ? La4 S2 La1 91.87(3) 1_565 1_565 ? La2 S2 La1 173.02(4) . 1_565 ? O33A S3 O34A 71.6(5) . . ? O33A S3 O32 122.9(4) . . ? O34A S3 O32 120.9(4) . . ? O33A S3 O31 112.2(4) . . ? O34A S3 O31 114.6(4) . . ? O32 S3 O31 110.1(2) . . ? O33A S3 O34B 107.7(5) . . ? O34A S3 O34B 36.3(4) . . ? O32 S3 O34B 97.7(3) . . ? O31 S3 O34B 103.5(3) . . ? O33A S3 O33B 36.1(4) . . ? O34A S3 O33B 107.2(5) . . ? O32 S3 O33B 99.0(4) . . ? O31 S3 O33B 101.9(4) . . ? O34B S3 O33B 142.5(5) . . ? O44 S4 O43 110.3(2) . . ? O44 S4 O41 108.8(2) . . ? O43 S4 O41 110.9(3) . . ? O44 S4 O42 110.6(2) . . ? O43 S4 O42 108.5(2) . . ? O41 S4 O42 107.8(2) . . ? O51 S5 O53 106.3(2) . 2_645 ? O51 S5 O52 111.9(2) . . ? O53 S5 O52 110.7(2) 2_645 . ? O51 S5 O54 111.0(2) . . ? O53 S5 O54 112.2(2) 2_645 . ? O52 S5 O54 104.9(2) . . ? O51 S5 La1 133.68(16) . . ? O53 S5 La1 120.06(15) 2_645 . ? O52 S5 La1 52.02(13) . . ? O54 S5 La1 53.49(14) . . ? O51 S5 La1 54.53(15) . 2_645 ? O53 S5 La1 51.82(14) 2_645 2_645 ? O52 S5 La1 124.68(13) . 2_645 ? O54 S5 La1 130.40(15) . 2_645 ? La1 S5 La1 171.12(4) . 2_645 ? O62 S6 O63 111.6(2) . . ? O62 S6 O61 105.9(2) . . ? O63 S6 O61 110.6(2) . . ? O62 S6 O64 111.1(2) . . ? O63 S6 O64 105.9(2) . . ? O61 S6 O64 111.9(2) . . ? O62 S6 La2 126.57(15) . . ? O63 S6 La2 51.78(13) . . ? O61 S6 La2 127.50(19) . . ? O64 S6 La2 54.14(14) . . ? O72 S7 O71 112.5(2) . . ? O72 S7 O73 106.8(2) . . ? O71 S7 O73 110.9(2) . . ? O72 S7 O74 111.39(19) . . ? O71 S7 O74 105.0(2) . . ? O73 S7 O74 110.3(2) . . ? O72 S7 La1 52.43(14) . . ? O71 S7 La1 127.91(15) . . ? O73 S7 La1 54.40(14) . . ? O74 S7 La1 127.10(14) . . ? O72 S7 La2 122.75(14) . 3_665 ? O71 S7 La2 48.81(14) . 3_665 ? O73 S7 La2 130.30(14) . 3_665 ? O74 S7 La2 56.53(14) . 3_665 ? La1 S7 La2 174.10(4) . 3_665 ? O82 S8 O81 110.1(3) . . ? O82 S8 O84 112.1(3) . . ? O81 S8 O84 111.6(2) . . ? O82 S8 O83 111.0(2) . . ? O81 S8 O83 106.4(3) . . ? O84 S8 O83 105.3(2) . . ? O82 S8 La3 125.8(2) . . ? O81 S8 La3 124.03(19) . . ? O84 S8 La3 50.91(14) . . ? O83 S8 La3 54.40(15) . . ? S1 O11 La4 158.2(3) . . ? S1 O12 La2 143.6(3) . . ? S1 O13 La3 140.0(3) . . ? S1 O14 La3 138.7(2) . 3_765 ? S2 O21 La4 99.19(16) . 1_565 ? S2 O21 La1 100.60(17) . 1_565 ? La4 O21 La1 122.18(12) 1_565 1_565 ? S2 O22 La2 109.19(19) . . ? S2 O23 La4 100.60(17) 1_545 . ? S2 O23 La2 92.36(15) 1_545 1_545 ? La4 O23 La2 115.94(13) . 1_545 ? S2 O24 La1 100.55(18) 1_545 . ? S3 O31 La2 128.5(2) . . ? S3 O32 La3 140.5(2) . 3_775 ? O33B O33A S3 84.5(8) . . ? O33B O33A O34A 138.9(10) . . ? S3 O33A O34A 55.4(4) . . ? O33B O33A La3 79.5(7) . . ? S3 O33A La3 162.9(6) . . ? O34A O33A La3 141.3(6) . . ? O33A O33B S3 59.4(7) . . ? O33A O33B La3 78.3(7) . . ? S3 O33B La3 137.3(5) . . ? O34B O34A S3 79.8(8) . . ? O34B O34A O33A 132.6(9) . . ? S3 O34A O33A 53.1(4) . . ? O34B O34A La4 72.4(7) . 1_565 ? S3 O34A La4 142.9(5) . 1_565 ? O33A O34A La4 150.3(5) . 1_565 ? O34A O34B S3 63.9(6) . . ? O34A O34B La4 86.6(7) . 1_565 ? S3 O34B La4 141.8(4) . 1_565 ? S4 O41 La3 132.6(2) . 2_745 ? S4 O42 La4 133.15(19) . . ? S4 O44 La1 151.2(3) . . ? S5 O51 La1 99.69(19) . 2_645 ? S5 O52 La1 101.48(16) . . ? S5 O53 La1 102.63(18) 2_655 . ? S5 O54 La1 99.40(17) . . ? S6 O61 La4 143.0(2) . . ? S6 O62 La1 113.6(2) . . ? S6 O63 La2 101.51(17) . . ? S6 O64 La2 98.83(18) . . ? S7 O71 La2 105.02(17) . 3_665 ? S7 O72 La1 100.95(16) . . ? S7 O73 La1 98.48(16) . . ? S7 O74 La2 96.29(16) . 3_665 ? S8 O81 La4 146.3(2) . 1_565 ? S8 O83 La2 113.5(2) . . ? S8 O83 La3 98.89(18) . . ? La2 O83 La3 127.29(16) . . ? S8 O84 La3 103.03(17) . . ? N12 C11 C16 113.6(5) . . ? N12 C11 H11A 108.9 . . ? C16 C11 H11A 108.9 . . ? N12 C11 H11B 108.9 . . ? C16 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 N12 C13 115.9(6) . . ? C11 N12 H12A 108.3 . . ? C13 N12 H12A 108.3 . . ? C11 N12 H12B 108.3 . . ? C13 N12 H12B 108.3 . . ? H12A N12 H12B 107.4 . . ? N12 C13 C14 115.4(6) . . ? N12 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? N12 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C13 C14 N15 111.9(5) . . ? C13 C14 H14A 109.2 . . ? N15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? N15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 N15 C14 114.2(5) . . ? C16 N15 H15A 108.7 . . ? C14 N15 H15A 108.7 . . ? C16 N15 H15B 108.7 . . ? C14 N15 H15B 108.7 . . ? H15A N15 H15B 107.6 . . ? N15 C16 C11 113.4(5) . . ? N15 C16 H16A 108.9 . . ? C11 C16 H16A 108.9 . . ? N15 C16 H16B 108.9 . . ? C11 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N26 C21 C22 112.0(6) . . ? N26 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N26 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 N23 112.3(5) . . ? C21 C22 H22A 109.1 . . ? N23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? N23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C24 N23 C22 112.6(5) . . ? C24 N23 H23A 109.1 . . ? C22 N23 H23A 109.1 . . ? C24 N23 H23B 109.1 . . ? C22 N23 H23B 109.1 . . ? H23A N23 H23B 107.8 . . ? N23 C24 C25 113.6(6) . . ? N23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? N23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N26 C25 C24 109.7(5) . . ? N26 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? N26 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C21 N26 C25 110.9(5) . . ? C21 N26 H26A 109.4 . . ? C25 N26 H26A 109.4 . . ? C21 N26 H26B 109.4 . . ? C25 N26 H26B 109.4 . . ? H26A N26 H26B 108.0 . . ? La3 OW31 H31A 118(3) . . ? La3 OW31 H31B 120(3) . . ? H31A OW31 H31B 109(3) . . ? La3 OW32 H32A 128(6) . . ? La3 OW32 H32B 121(6) . . ? H32A OW32 H32B 107(3) . . ? La4 OW41 H41A 107(3) . . ? La4 OW41 H41B 102(3) . . ? H41A OW41 H41B 105(2) . . ? La4 OW42 H42A 126(4) . . ? La4 OW42 H42B 114(3) . . ? H42A OW42 H42B 109(3) . . ? 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 N12 H12A O61 0.99 2.53 3.386(9) 144.2 . N12 H12B O74 0.99 2.08 3.043(8) 164.0 3_665 N12 H12B O63 0.99 2.34 2.873(7) 112.7 . N15 H15A O54 0.99 2.11 3.075(8) 163.6 4_565 N15 H15B O73 0.99 2.05 2.988(6) 157.0 3_655 N15 H15B O52 0.99 2.51 3.031(7) 112.6 3_655 N23 H23A O43 0.99 2.20 2.752(6) 114.1 . N23 H23A O64 0.99 2.52 3.243(7) 129.9 . N23 H23B O53 0.99 2.06 3.005(7) 158.1 . N23 H23B O62 0.99 2.57 3.193(7) 121.3 . N26 H26A O14 0.99 2.31 3.123(7) 138.8 4_576 N26 H26B O74 0.99 2.14 3.037(7) 149.5 2_655 OW31 H31A OW41 0.958(12) 1.92(2) 2.850(5) 164(6) . OW31 H31B O42 0.951(12) 1.98(3) 2.812(5) 145(5) 2_755 OW32 H32A O13 0.969(12) 2.00(9) 2.725(10) 130(10) 3_765 OW32 H32B O34A 0.972(12) 2.40(13) 3.010(12) 120(11) 3_775 OW41 H41A O43 0.961(12) 1.84(3) 2.716(6) 151(5) . OW41 H41B O64 0.963(12) 2.05(3) 2.912(5) 148(4) . OW42 H42A O82 0.961(12) 1.81(2) 2.752(6) 166(5) 2_745 OW42 H42B O84 0.953(12) 1.88(3) 2.791(5) 159(6) 1_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.881 _refine_diff_density_min -2.048 _refine_diff_density_rms 0.283