Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_laalmo1 _database_code_CSD 184859 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Shivaiah, V.' 'Reddy, P. V. N.' 'Cronin, L.' 'Das, S. K.' _publ_contact_author_name 'S. K. Das' _publ_contact_author_address ; School of Chemistry University of Hyderabad Hyderbad 500 0456 India ; _publ_contact_author_email skdsc@uohyd.ernet.in _publ_section_title ; A novel polyoxometalate chain formed from heteropolyanion building blocks and lanthanum cation linkers: [La(H2O)7Al(OH)6Mo6O18]n . 4nH2O ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H28 Al La Mo6 O35' _chemical_formula_weight 1329.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_c_a_21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 11.844(2) _cell_length_b 11.010(2) _cell_length_c 22.643(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2952.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 32.618 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD Diffractometer' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5272 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 70.60 _reflns_number_total 5272 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0465P)^2^+1.5341P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 5272 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 O1 O 0.8506(4) 0.1427(5) 0.7931(2) 0.0206(11) Uani 1 1 d . . . O2 O 0.7509(4) 0.3511(4) 0.7962(2) 0.0188(11) Uani 1 1 d . . . O3 O 0.9310(3) 0.3420(4) 0.8578(3) 0.0181(9) Uani 1 1 d . . . O4 O 0.7509(4) 0.3434(4) 0.9195(2) 0.0202(11) Uani 1 1 d . . . O5 O 0.8480(4) 0.1348(5) 0.9168(2) 0.0203(11) Uani 1 1 d . . . O6 O 0.6686(3) 0.1445(4) 0.8538(2) 0.0171(9) Uani 1 1 d . . . O7 O 0.7605(4) -0.0609(4) 0.8512(2) 0.0218(10) Uani 1 1 d . . . O8 O 0.5667(5) -0.0464(5) 0.7812(3) 0.0292(13) Uani 1 1 d . . . O9 O 0.7733(6) 0.9118(6) 0.7309(3) 0.0330(14) Uani 1 1 d . . . O10 O 0.6791(5) 0.1431(5) 0.7295(2) 0.0239(12) Uani 1 1 d . . . O11 O 0.8763(5) 0.1616(5) 0.6626(3) 0.0330(13) Uani 1 1 d . . . O12 O 0.7274(5) 0.3513(5) 0.6694(2) 0.0271(12) Uani 1 1 d . . . O13 O 0.9281(5) 0.3504(5) 0.7359(2) 0.0244(12) Uani 1 1 d . . . O14 O 0.8310(5) 0.5813(5) 0.7390(3) 0.0283(13) Uani 1 1 d . . . O15 O 1.0364(5) 0.5404(6) 0.7908(3) 0.0304(13) Uani 1 1 d . . . O24 O 0.5630(5) -0.0489(6) 0.9197(3) 0.0322(14) Uani 1 1 d . . . O16 O 0.8422(4) 0.5487(4) 0.8605(3) 0.0219(10) Uani 1 1 d . . . O17 O 1.0374(5) 0.5340(6) 0.9297(3) 0.0372(15) Uani 1 1 d . . . O18 O 0.8278(6) 0.5631(5) 0.9822(3) 0.0328(14) Uani 1 1 d . . . O23 O 0.7680(6) -0.0988(6) 0.9686(3) 0.0349(15) Uani 1 1 d . . . O19 O 0.9297(5) 0.3331(5) 0.9810(2) 0.0244(12) Uani 1 1 d . . . O20 O 0.7279(6) 0.3286(6) 1.0463(3) 0.0353(14) Uani 1 1 d . . . O21 O 0.8687(6) 0.1346(6) 1.0476(3) 0.0373(15) Uani 1 1 d . . . O22 O 0.6735(5) 0.1334(5) 0.9787(2) 0.0223(11) Uani 1 1 d . . . O25 O 1.0019(5) 0.6237(6) 0.6294(3) 0.0420(15) Uani 1 1 d . . . O26 O 0.7546(7) 0.5609(5) 0.6024(3) 0.0364(13) Uani 1 1 d . . . O27 O 0.8681(6) 0.7437(5) 0.5404(3) 0.0362(15) Uani 1 1 d . . . O28 O 0.6912(7) 0.8946(8) 0.6033(3) 0.063(2) Uani 1 1 d . . . O29 O 0.9489(7) 0.9315(6) 0.6253(3) 0.0537(19) Uani 1 1 d . . . O30 O 0.9731(6) 0.7811(6) 0.7311(3) 0.0378(14) Uani 1 1 d . . . O31 O 0.6354(6) 0.7057(8) 0.6900(5) 0.071(3) Uani 1 1 d . . . O32 O 0.6497(5) 0.7027(6) 0.8420(4) 0.054(2) Uani 1 1 d . . . O33 O 0.9489(4) 0.7891(5) 0.8558(4) 0.0413(14) Uani 1 1 d . . . O34 O 0.4939(8) 0.6037(7) 0.5883(4) 0.063(2) Uani 1 1 d . . . O35 O 0.5366(7) 0.8164(10) 0.5241(4) 0.078(3) Uani 1 1 d . . . Al1 Al 0.79993(17) 0.24370(16) 0.85682(12) 0.0171(4) Uani 1 1 d . . . Mo1 Mo 0.80494(5) 0.25062(5) 0.71135(3) 0.02013(15) Uani 1 1 d . . . Mo2 Mo 0.69811(5) 0.00312(5) 0.92656(3) 0.02045(16) Uani 1 1 d . . . Mo3 Mo 0.80275(5) 0.23374(6) 1.00313(3) 0.02171(15) Uani 1 1 d . . . Mo4 Mo 0.70325(5) 0.00564(5) 0.78005(3) 0.01964(15) Uani 1 1 d . . . Mo5 Mo 0.90233(5) 0.47578(6) 0.93396(3) 0.02142(15) Uani 1 1 d . . . Mo6 Mo 0.90051(5) 0.48595(5) 0.78765(3) 0.01979(15) Uani 1 1 d . . . La1 La 0.82878(4) 0.74862(4) 0.65583(3) 0.02124(11) 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 O1 0.016(3) 0.026(3) 0.020(3) 0.000(2) 0.005(2) 0.002(2) O2 0.019(3) 0.019(2) 0.019(3) 0.004(2) -0.001(2) 0.000(2) O3 0.016(2) 0.018(2) 0.020(2) 0.004(3) 0.001(2) -0.0004(16) O4 0.018(2) 0.024(3) 0.019(3) 0.001(2) 0.002(2) 0.001(2) O5 0.015(3) 0.022(3) 0.024(3) 0.002(2) -0.002(2) 0.001(2) O6 0.014(2) 0.019(2) 0.018(2) 0.002(2) 0.001(2) -0.0008(15) O7 0.023(2) 0.021(2) 0.022(2) 0.001(2) -0.001(2) 0.0013(18) O8 0.019(3) 0.032(3) 0.036(3) 0.003(3) 0.001(3) -0.004(2) O9 0.039(4) 0.033(3) 0.027(3) -0.007(3) -0.003(3) 0.005(3) O10 0.021(3) 0.029(3) 0.022(3) 0.000(2) -0.001(2) -0.007(2) O11 0.037(3) 0.033(3) 0.029(3) -0.006(3) 0.009(3) -0.001(3) O12 0.031(3) 0.030(3) 0.020(3) 0.008(2) -0.003(2) -0.005(2) O13 0.020(3) 0.027(3) 0.026(3) -0.002(2) 0.003(2) -0.004(2) O14 0.031(3) 0.025(3) 0.028(3) 0.002(3) -0.001(2) 0.001(2) O15 0.018(3) 0.039(3) 0.034(3) 0.007(3) -0.005(3) -0.006(2) O24 0.032(3) 0.033(3) 0.032(3) -0.003(3) 0.008(3) -0.009(3) O16 0.026(2) 0.017(2) 0.024(2) 0.000(2) 0.002(3) 0.0062(18) O17 0.028(3) 0.039(3) 0.044(4) 0.010(3) -0.008(3) -0.018(3) O18 0.043(4) 0.028(3) 0.028(3) -0.003(3) 0.002(3) 0.003(3) O23 0.041(4) 0.034(3) 0.030(3) 0.014(3) 0.002(3) -0.002(3) O19 0.022(3) 0.024(3) 0.027(3) 0.004(2) -0.004(2) -0.004(2) O20 0.038(4) 0.038(3) 0.030(3) -0.001(3) 0.005(3) -0.001(3) O21 0.039(4) 0.033(3) 0.040(4) 0.006(3) -0.007(3) -0.007(3) O22 0.019(3) 0.028(3) 0.020(2) -0.004(2) 0.004(2) -0.003(2) O25 0.027(3) 0.047(4) 0.052(4) -0.011(3) -0.005(3) 0.007(3) O26 0.049(3) 0.029(3) 0.031(3) 0.001(3) -0.002(3) -0.007(3) O27 0.032(4) 0.053(4) 0.023(3) 0.003(3) 0.006(3) -0.004(3) O28 0.067(5) 0.073(6) 0.048(4) 0.007(4) 0.001(4) 0.033(4) O29 0.065(5) 0.032(3) 0.064(4) -0.009(3) 0.036(4) -0.013(3) O30 0.037(3) 0.042(3) 0.035(3) 0.000(3) -0.010(3) -0.008(3) O31 0.037(4) 0.059(5) 0.116(8) 0.006(5) 0.025(5) -0.002(4) O32 0.025(3) 0.028(3) 0.110(8) 0.001(4) -0.001(4) 0.002(2) O33 0.024(3) 0.031(3) 0.069(4) -0.003(4) 0.002(4) 0.001(2) O34 0.049(5) 0.064(5) 0.075(6) 0.017(4) -0.005(4) -0.008(4) O35 0.044(5) 0.109(8) 0.081(6) 0.039(6) -0.012(4) -0.015(5) Al1 0.0178(9) 0.0172(10) 0.0161(10) 0.0006(9) -0.0013(9) -0.0009(6) Mo1 0.0210(3) 0.0221(3) 0.0173(3) 0.0001(2) 0.0011(2) -0.0008(3) Mo2 0.0195(3) 0.0219(3) 0.0199(3) 0.0025(2) 0.0004(3) -0.0036(2) Mo3 0.0235(3) 0.0242(3) 0.0174(3) 0.0002(3) -0.0015(2) -0.0023(2) Mo4 0.0190(3) 0.0192(3) 0.0208(3) -0.0024(2) -0.0005(3) -0.0010(2) Mo5 0.0234(3) 0.0209(3) 0.0200(3) -0.0013(3) -0.0013(2) -0.0028(2) Mo6 0.0190(3) 0.0194(3) 0.0209(3) 0.0020(2) 0.0007(2) -0.0021(2) La1 0.02147(19) 0.0211(2) 0.0211(2) -0.00084(16) 0.00112(19) -0.00025(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 O1 Al1 1.918(6) . ? O1 Mo1 2.266(5) . ? O1 Mo4 2.326(5) . ? O2 Al1 1.903(5) . ? O2 Mo1 2.307(5) . ? O2 Mo6 2.320(5) . ? O3 Al1 1.893(5) . ? O3 Mo6 2.273(5) . ? O3 Mo5 2.294(5) . ? O4 Al1 1.886(5) . ? O4 Mo3 2.328(5) . ? O4 Mo5 2.335(5) . ? O5 Al1 1.898(6) . ? O5 Mo3 2.302(5) . ? O5 Mo2 2.303(5) . ? O6 Al1 1.902(5) . ? O6 Mo2 2.293(5) . ? O6 Mo4 2.302(5) . ? O7 Mo4 1.896(5) . ? O7 Mo2 1.988(5) . ? O8 Mo4 1.716(6) . ? O9 Mo4 1.730(6) 1_565 ? O9 La1 2.560(6) . ? O10 Mo4 1.919(6) . ? O10 Mo1 1.947(6) . ? O11 Mo1 1.701(6) . ? O12 Mo1 1.725(6) . ? O13 Mo1 1.909(6) . ? O13 Mo6 1.925(6) . ? O14 Mo6 1.731(6) . ? O14 La1 2.634(6) . ? O15 Mo6 1.719(6) . ? O24 Mo2 1.707(6) . ? O16 Mo6 1.917(5) . ? O16 Mo5 1.980(6) . ? O17 Mo5 1.726(6) . ? O18 Mo5 1.701(6) . ? O23 Mo2 1.688(6) . ? O19 Mo5 1.925(5) . ? O19 Mo3 1.926(5) . ? O20 Mo3 1.682(6) . ? O21 Mo3 1.678(7) . ? O22 Mo2 1.881(5) . ? O22 Mo3 1.967(6) . ? O25 La1 2.541(6) . ? O26 La1 2.551(6) . ? O27 La1 2.655(6) . ? O28 La1 2.580(7) . ? O29 La1 2.561(6) . ? O30 La1 2.441(6) . ? O31 La1 2.463(7) . ? Mo4 O9 1.730(6) 1_545 ? 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 Al1 O1 Mo1 103.6(2) . . ? Al1 O1 Mo4 103.7(2) . . ? Mo1 O1 Mo4 93.28(19) . . ? Al1 O2 Mo1 102.6(2) . . ? Al1 O2 Mo6 103.0(2) . . ? Mo1 O2 Mo6 91.46(18) . . ? Al1 O3 Mo6 105.1(2) . . ? Al1 O3 Mo5 104.7(2) . . ? Mo6 O3 Mo5 93.09(16) . . ? Al1 O4 Mo3 103.2(2) . . ? Al1 O4 Mo5 103.4(2) . . ? Mo3 O4 Mo5 90.40(18) . . ? Al1 O5 Mo3 103.8(2) . . ? Al1 O5 Mo2 103.6(2) . . ? Mo3 O5 Mo2 92.09(18) . . ? Al1 O6 Mo2 103.9(2) . . ? Al1 O6 Mo4 105.1(2) . . ? Mo2 O6 Mo4 92.47(16) . . ? Mo4 O7 Mo2 117.4(2) . . ? Mo4 O9 La1 165.8(4) 1_565 . ? Mo4 O10 Mo1 119.4(3) . . ? Mo1 O13 Mo6 119.6(3) . . ? Mo6 O14 La1 152.1(3) . . ? Mo6 O16 Mo5 116.5(2) . . ? Mo5 O19 Mo3 118.4(3) . . ? Mo2 O22 Mo3 118.9(3) . . ? O4 Al1 O3 84.9(2) . . ? O4 Al1 O5 85.5(3) . . ? O3 Al1 O5 96.1(2) . . ? O4 Al1 O6 96.2(2) . . ? O3 Al1 O6 178.6(3) . . ? O5 Al1 O6 84.7(2) . . ? O4 Al1 O2 95.0(2) . . ? O3 Al1 O2 84.5(2) . . ? O5 Al1 O2 179.3(3) . . ? O6 Al1 O2 94.7(2) . . ? O4 Al1 O1 179.7(3) . . ? O3 Al1 O1 94.8(2) . . ? O5 Al1 O1 94.4(2) . . ? O6 Al1 O1 84.0(2) . . ? O2 Al1 O1 85.0(3) . . ? O11 Mo1 O12 106.1(3) . . ? O11 Mo1 O13 98.1(3) . . ? O12 Mo1 O13 101.4(3) . . ? O11 Mo1 O10 99.6(3) . . ? O12 Mo1 O10 95.7(3) . . ? O13 Mo1 O10 150.9(2) . . ? O11 Mo1 O1 96.3(3) . . ? O12 Mo1 O1 156.2(2) . . ? O13 Mo1 O1 83.2(2) . . ? O10 Mo1 O1 72.0(2) . . ? O11 Mo1 O2 162.6(3) . . ? O12 Mo1 O2 90.2(2) . . ? O13 Mo1 O2 72.2(2) . . ? O10 Mo1 O2 84.5(2) . . ? O1 Mo1 O2 68.76(19) . . ? O23 Mo2 O24 106.8(3) . . ? O23 Mo2 O22 103.2(3) . . ? O24 Mo2 O22 99.6(3) . . ? O23 Mo2 O7 93.8(3) . . ? O24 Mo2 O7 98.7(2) . . ? O22 Mo2 O7 150.1(2) . . ? O23 Mo2 O6 158.6(2) . . ? O24 Mo2 O6 91.1(2) . . ? O22 Mo2 O6 84.8(2) . . ? O7 Mo2 O6 71.42(19) . . ? O23 Mo2 O5 95.4(3) . . ? O24 Mo2 O5 157.7(3) . . ? O22 Mo2 O5 72.5(2) . . ? O7 Mo2 O5 81.62(19) . . ? O6 Mo2 O5 67.73(16) . . ? O21 Mo3 O20 107.5(3) . . ? O21 Mo3 O19 99.3(3) . . ? O20 Mo3 O19 102.1(3) . . ? O21 Mo3 O22 99.5(3) . . ? O20 Mo3 O22 95.8(3) . . ? O19 Mo3 O22 148.6(2) . . ? O21 Mo3 O5 95.3(3) . . ? O20 Mo3 O5 155.5(3) . . ? O19 Mo3 O5 82.3(2) . . ? O22 Mo3 O5 71.2(2) . . ? O21 Mo3 O4 161.4(3) . . ? O20 Mo3 O4 90.6(3) . . ? O19 Mo3 O4 72.5(2) . . ? O22 Mo3 O4 81.8(2) . . ? O5 Mo3 O4 67.40(19) . . ? O8 Mo4 O9 105.2(3) . 1_545 ? O8 Mo4 O7 101.2(2) . . ? O9 Mo4 O7 98.3(3) 1_545 . ? O8 Mo4 O10 97.6(3) . . ? O9 Mo4 O10 99.1(3) 1_545 . ? O7 Mo4 O10 149.9(2) . . ? O8 Mo4 O6 92.4(2) . . ? O9 Mo4 O6 161.6(3) 1_545 . ? O7 Mo4 O6 72.74(19) . . ? O10 Mo4 O6 83.3(2) . . ? O8 Mo4 O1 157.2(2) . . ? O9 Mo4 O1 96.3(3) 1_545 . ? O7 Mo4 O1 82.78(19) . . ? O10 Mo4 O1 71.1(2) . . ? O6 Mo4 O1 67.10(16) . . ? O18 Mo5 O17 107.9(3) . . ? O18 Mo5 O19 101.1(3) . . ? O17 Mo5 O19 100.3(3) . . ? O18 Mo5 O16 97.1(3) . . ? O17 Mo5 O16 97.8(3) . . ? O19 Mo5 O16 148.9(2) . . ? O18 Mo5 O3 157.3(3) . . ? O17 Mo5 O3 93.4(3) . . ? O19 Mo5 O3 82.4(2) . . ? O16 Mo5 O3 71.45(19) . . ? O18 Mo5 O4 92.5(3) . . ? O17 Mo5 O4 159.4(3) . . ? O19 Mo5 O4 72.4(2) . . ? O16 Mo5 O4 81.89(19) . . ? O3 Mo5 O4 66.88(16) . . ? O15 Mo6 O14 105.1(3) . . ? O15 Mo6 O16 100.2(3) . . ? O14 Mo6 O16 99.1(3) . . ? O15 Mo6 O13 97.8(3) . . ? O14 Mo6 O13 99.4(3) . . ? O16 Mo6 O13 149.8(2) . . ? O15 Mo6 O3 93.8(2) . . ? O14 Mo6 O3 160.7(2) . . ? O16 Mo6 O3 73.00(19) . . ? O13 Mo6 O3 81.8(2) . . ? O15 Mo6 O2 159.2(2) . . ? O14 Mo6 O2 94.5(2) . . ? O16 Mo6 O2 83.32(19) . . ? O13 Mo6 O2 71.6(2) . . ? O3 Mo6 O2 67.48(16) . . ? O30 La1 O31 117.4(3) . . ? O30 La1 O25 71.3(2) . . ? O31 La1 O25 136.1(3) . . ? O30 La1 O26 133.7(2) . . ? O31 La1 O26 70.9(3) . . ? O25 La1 O26 74.2(2) . . ? O30 La1 O9 67.2(2) . . ? O31 La1 O9 71.8(3) . . ? O25 La1 O9 138.1(2) . . ? O26 La1 O9 142.7(2) . . ? O30 La1 O29 71.6(2) . . ? O31 La1 O29 138.8(3) . . ? O25 La1 O29 85.1(2) . . ? O26 La1 O29 134.5(2) . . ? O9 La1 O29 76.7(2) . . ? O30 La1 O28 132.3(3) . . ? O31 La1 O28 71.1(3) . . ? O25 La1 O28 137.6(2) . . ? O26 La1 O28 93.9(3) . . ? O9 La1 O28 73.0(2) . . ? O29 La1 O28 74.7(3) . . ? O30 La1 O14 66.2(2) . . ? O31 La1 O14 69.6(3) . . ? O25 La1 O14 77.4(2) . . ? O26 La1 O14 77.03(19) . . ? O9 La1 O14 91.1(2) . . ? O29 La1 O14 137.5(2) . . ? O28 La1 O14 140.5(2) . . ? O30 La1 O27 124.6(2) . . ? O31 La1 O27 117.9(3) . . ? O25 La1 O27 67.4(2) . . ? O26 La1 O27 65.0(2) . . ? O9 La1 O27 135.49(19) . . ? O29 La1 O27 69.7(2) . . ? O28 La1 O27 70.7(2) . . ? O14 La1 O27 133.44(18) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 70.60 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.587 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.172