# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_LaVO(IO3)5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I5 La O16 V' _chemical_formula_sum 'I5 La O16 V' _chemical_formula_weight 1080.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.562(3) _cell_length_b 18.102(6) _cell_length_c 10.444(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.501(5) _cell_angle_gamma 90.00 _cell_volume 1428.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3676 _cell_measurement_theta_min 2.2501 _cell_measurement_theta_max 27.4758 _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 14.499 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6565 _exptl_absorpt_process_details crystalclear _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 10642 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3263 _reflns_number_gt 2879 _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^)+(0.0378P)^2^+4.7857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3263 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 0.24825(6) 0.73377(3) 0.26018(5) 0.01099(12) Uani 1 1 d . . . V1 V 0.77209(18) 0.49874(7) 0.26818(14) 0.0115(3) Uani 1 1 d . . . I1 I 0.60526(7) 0.62465(3) 0.06313(5) 0.01141(13) Uani 1 1 d . . . I2 I 0.57708(7) 0.87066(3) 0.44825(5) 0.01159(13) Uani 1 1 d . . . I3 I 0.77985(7) 0.66289(3) 0.43416(5) 0.01258(13) Uani 1 1 d . . . I4 I 0.71059(7) 0.32645(3) 0.39764(5) 0.01209(13) Uani 1 1 d . . . I5 I 0.28887(7) 0.50508(3) 0.25915(5) 0.01227(13) Uani 1 1 d . . . O1 O 0.8028(7) 0.5881(3) 0.1507(6) 0.0154(13) Uani 1 1 d . . . O2 O 0.5390(8) 0.6863(3) 0.1872(6) 0.0194(13) Uani 1 1 d . . . O3 O 0.7241(8) 0.6943(3) -0.0259(6) 0.0190(13) Uani 1 1 d . . . O4 O 0.7483(8) 0.9300(3) 0.3893(6) 0.0193(14) Uani 1 1 d . . . O5 O 0.7258(8) 0.8036(3) 0.5237(6) 0.0206(14) Uani 1 1 d . . . O6 O 0.5242(8) 0.8178(3) 0.3065(6) 0.0162(13) Uani 1 1 d . . . O7 O 0.7321(9) 0.5646(3) 0.4141(7) 0.0220(14) Uani 1 1 d . . . O8 O 1.0161(8) 0.6667(3) 0.4120(6) 0.0199(14) Uani 1 1 d . . . O9 O 0.7794(8) 0.6612(3) 0.6069(6) 0.0185(13) Uani 1 1 d . . . O10 O 0.5576(8) 0.2786(4) 0.2906(6) 0.0209(14) Uani 1 1 d . . . O11 O 0.6473(8) 0.4214(3) 0.3654(6) 0.0209(14) Uani 1 1 d . . . O12 O 0.5962(8) 0.3237(3) 0.5475(6) 0.0162(13) Uani 1 1 d . . . O13 O 0.2202(9) 0.4485(4) 0.1259(7) 0.0268(15) Uani 1 1 d . . . O14 O 0.2014(8) 0.5928(3) 0.2105(7) 0.0215(14) Uani 1 1 d . . . O15 O 0.5116(8) 0.5223(3) 0.2000(6) 0.0187(13) Uani 1 1 d . . . O16 O 0.9755(8) 0.4814(4) 0.3061(7) 0.0224(15) 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 La1 0.0125(2) 0.0102(2) 0.0101(3) 0.00043(17) -0.00137(17) 0.00128(16) V1 0.0105(6) 0.0103(7) 0.0135(8) 0.0010(5) -0.0005(5) 0.0000(5) I1 0.0124(2) 0.0100(2) 0.0118(3) 0.00007(19) -0.0003(2) 0.00004(17) I2 0.0133(2) 0.0108(3) 0.0106(3) -0.00020(19) -0.0009(2) 0.00019(18) I3 0.0135(2) 0.0122(3) 0.0118(3) -0.0016(2) -0.0020(2) 0.00045(18) I4 0.0127(2) 0.0127(3) 0.0108(3) 0.0007(2) -0.0007(2) -0.00177(18) I5 0.0128(2) 0.0110(3) 0.0131(3) 0.0000(2) 0.0005(2) -0.00119(18) O1 0.009(3) 0.016(3) 0.020(3) 0.005(2) -0.002(2) 0.006(2) O2 0.018(3) 0.017(3) 0.023(4) -0.003(3) -0.001(3) 0.006(2) O3 0.027(3) 0.009(3) 0.021(4) 0.010(2) 0.002(3) -0.001(2) O4 0.014(3) 0.021(3) 0.023(4) 0.011(3) -0.002(3) -0.008(2) O5 0.024(3) 0.021(3) 0.017(3) 0.001(3) -0.003(3) 0.009(3) O6 0.020(3) 0.022(3) 0.006(3) -0.001(2) -0.002(2) -0.005(2) O7 0.028(3) 0.014(3) 0.025(4) -0.002(3) 0.004(3) 0.000(3) O8 0.013(3) 0.024(3) 0.023(4) 0.001(3) 0.000(3) -0.001(2) O9 0.025(3) 0.020(3) 0.010(3) -0.001(2) 0.000(3) -0.001(3) O10 0.018(3) 0.025(3) 0.019(4) -0.004(3) -0.001(3) -0.007(3) O11 0.026(3) 0.011(3) 0.026(4) 0.008(3) 0.006(3) 0.001(2) O12 0.015(3) 0.022(3) 0.012(3) 0.003(3) 0.008(2) 0.004(2) O13 0.028(4) 0.026(4) 0.027(4) -0.009(3) 0.006(3) -0.008(3) O14 0.019(3) 0.018(3) 0.027(4) -0.001(3) -0.002(3) 0.003(2) O15 0.017(3) 0.020(3) 0.020(4) 0.009(3) 0.002(3) 0.000(2) O16 0.017(3) 0.022(3) 0.027(4) 0.001(3) -0.005(3) 0.000(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 O10 2.486(6) 2 ? La1 O9 2.504(6) 4_575 ? La1 O12 2.509(6) 3_666 ? La1 O2 2.510(6) . ? La1 O5 2.559(6) 4_575 ? La1 O3 2.599(6) 4_576 ? La1 O6 2.610(6) . ? La1 O14 2.625(6) . ? La1 O8 2.705(6) 1_455 ? V1 O16 1.603(6) . ? V1 O7 1.969(7) . ? V1 O11 1.991(6) . ? V1 O1 2.050(6) . ? V1 O4 2.063(6) 2_645 ? V1 O15 2.108(6) . ? I1 O2 1.798(6) . ? I1 O3 1.826(6) . ? I1 O1 1.840(5) . ? I1 O15 2.464(6) . ? I2 O6 1.794(6) . ? I2 O4 1.811(6) . ? I2 O5 1.812(6) . ? I3 O9 1.804(6) . ? I3 O8 1.812(6) . ? I3 O7 1.825(6) . ? I4 O10 1.796(6) . ? I4 O11 1.812(6) . ? I4 O12 1.822(6) . ? I5 O14 1.786(6) . ? I5 O13 1.787(7) . ? I5 O15 1.846(6) . ? I5 O16 2.478(6) 1_455 ? O3 La1 2.599(6) 4_675 ? O4 V1 2.063(6) 2_655 ? O5 La1 2.559(6) 4_676 ? O8 La1 2.705(6) 1_655 ? O9 La1 2.504(6) 4_676 ? O10 La1 2.486(6) 2_545 ? O12 La1 2.509(6) 3_666 ? O16 I5 2.478(6) 1_655 ? 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 O10 La1 O9 74.2(2) 2 4_575 ? O10 La1 O12 134.9(2) 2 3_666 ? O9 La1 O12 140.6(2) 4_575 3_666 ? O10 La1 O2 150.0(2) 2 . ? O9 La1 O2 87.6(2) 4_575 . ? O12 La1 O2 73.4(2) 3_666 . ? O10 La1 O5 81.9(2) 2 4_575 ? O9 La1 O5 65.6(2) 4_575 4_575 ? O12 La1 O5 132.2(2) 3_666 4_575 ? O2 La1 O5 68.8(2) . 4_575 ? O10 La1 O3 85.4(2) 2 4_576 ? O9 La1 O3 100.5(2) 4_575 4_576 ? O12 La1 O3 64.4(2) 3_666 4_576 ? O2 La1 O3 121.9(2) . 4_576 ? O5 La1 O3 163.3(2) 4_575 4_576 ? O10 La1 O6 125.3(2) 2 . ? O9 La1 O6 65.13(19) 4_575 . ? O12 La1 O6 75.53(19) 3_666 . ? O2 La1 O6 63.4(2) . . ? O5 La1 O6 110.58(19) 4_575 . ? O3 La1 O6 68.56(19) 4_576 . ? O10 La1 O14 99.2(2) 2 . ? O9 La1 O14 128.9(2) 4_575 . ? O12 La1 O14 79.0(2) 3_666 . ? O2 La1 O14 73.7(2) . . ? O5 La1 O14 63.2(2) 4_575 . ? O3 La1 O14 130.0(2) 4_576 . ? O6 La1 O14 134.66(19) . . ? O10 La1 O8 69.5(2) 2 1_455 ? O9 La1 O8 142.9(2) 4_575 1_455 ? O12 La1 O8 68.77(18) 3_666 1_455 ? O2 La1 O8 128.60(19) . 1_455 ? O5 La1 O8 115.46(19) 4_575 1_455 ? O3 La1 O8 69.5(2) 4_576 1_455 ? O6 La1 O8 133.40(19) . 1_455 ? O14 La1 O8 66.0(2) . 1_455 ? O16 V1 O7 96.1(3) . . ? O16 V1 O11 102.0(3) . . ? O7 V1 O11 86.5(3) . . ? O16 V1 O1 99.8(3) . . ? O7 V1 O1 90.6(3) . . ? O11 V1 O1 158.2(2) . . ? O16 V1 O4 96.7(3) . 2_645 ? O7 V1 O4 166.9(3) . 2_645 ? O11 V1 O4 87.8(3) . 2_645 ? O1 V1 O4 90.3(3) . 2_645 ? O16 V1 O15 174.5(3) . . ? O7 V1 O15 88.1(3) . . ? O11 V1 O15 81.8(3) . . ? O1 V1 O15 76.5(2) . . ? O4 V1 O15 79.4(2) 2_645 . ? O2 I1 O3 95.6(3) . . ? O2 I1 O1 96.4(3) . . ? O3 I1 O1 95.4(3) . . ? O2 I1 O15 87.3(3) . . ? O3 I1 O15 167.2(2) . . ? O1 I1 O15 71.9(2) . . ? O6 I2 O4 100.0(3) . . ? O6 I2 O5 96.5(3) . . ? O4 I2 O5 96.1(3) . . ? O9 I3 O8 100.0(3) . . ? O9 I3 O7 95.1(3) . . ? O8 I3 O7 102.3(3) . . ? O10 I4 O11 100.6(3) . . ? O10 I4 O12 101.8(3) . . ? O11 I4 O12 93.1(3) . . ? O14 I5 O13 101.4(3) . . ? O14 I5 O15 95.0(3) . . ? O13 I5 O15 94.3(3) . . ? O14 I5 O16 82.2(3) . 1_455 ? O13 I5 O16 78.9(3) . 1_455 ? O15 I5 O16 171.9(2) . 1_455 ? I1 O1 V1 118.1(3) . . ? I1 O2 La1 135.0(3) . . ? I1 O3 La1 146.9(3) . 4_675 ? I2 O4 V1 126.8(3) . 2_655 ? I2 O5 La1 127.6(3) . 4_676 ? I2 O6 La1 127.7(3) . . ? I3 O7 V1 130.0(4) . . ? I3 O8 La1 139.5(3) . 1_655 ? I3 O9 La1 129.1(3) . 4_676 ? I4 O10 La1 149.1(4) . 2_545 ? I4 O11 V1 129.4(4) . . ? I4 O12 La1 118.4(3) . 3_666 ? I5 O14 La1 139.7(3) . . ? I5 O15 V1 134.9(3) . . ? I5 O15 I1 127.6(3) . . ? V1 O15 I1 93.4(2) . . ? V1 O16 I5 146.4(4) . 1_655 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.508 _refine_diff_density_min -2.236 _refine_diff_density_rms 0.397 #===end data_LaV2O6(IO3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I La O9 V2' _chemical_formula_sum 'I La O9 V2 ' _chemical_formula_weight 511.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'I' 'I' -0.4742 1.8119 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 '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 b c m' _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 7.077(2) _cell_length_b 14.620(5) _cell_length_c 7.305(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 755.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2137 _cell_measurement_theta_min 3.1167 _cell_measurement_theta_max 27.4603 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 12.079 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 0.299 _exptl_absorpt_correction_T_min 0.131 _exptl_absorpt_process_details 'CrystalClear' _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 'Mercury70' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 5459 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 939 _reflns_number_gt 905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 939 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La -0.84946(4) -0.048294(18) 0.2500 0.00578(13) Uani 1 2 d S . . V1 V -0.53129(11) -0.2500 0.0000 0.0056(2) Uani 1 2 d S . . V2 V -1.18239(11) -0.27141(5) 0.2500 0.0055(2) Uani 1 2 d S . . I1 I -1.29821(5) 0.05704(2) 0.2500 0.00665(14) Uani 1 2 d S . . O1 O -1.1759(3) -0.00762(17) 0.0724(4) 0.0091(5) Uani 1 1 d . . . O2 O -1.5220(5) 0.0019(3) 0.2500 0.0193(9) Uani 1 2 d S . . O3 O -0.6648(4) -0.15940(18) 0.0435(4) 0.0131(6) Uani 1 1 d . . . O4 O -0.4673(5) -0.2799(2) 0.2500 0.0091(7) Uani 1 2 d S . . O5 O -0.2599(5) -0.2500 0.0000 0.0127(8) Uani 1 2 d S . . O6 O -1.0124(5) -0.1958(2) 0.2500 0.0155(9) Uani 1 2 d S . . O7 O -0.9154(5) 0.1261(2) 0.2500 0.0110(8) Uani 1 2 d S . . 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 0.00959(19) 0.00698(19) 0.0008(2) 0.000 0.000 0.00065(9) V1 0.0092(4) 0.0066(4) 0.0009(4) -0.0003(3) 0.000 0.000 V2 0.0080(4) 0.0075(4) 0.0009(4) 0.000 0.000 0.0010(3) I1 0.0091(2) 0.0100(2) 0.0009(2) 0.000 0.000 0.00159(10) O1 0.0137(12) 0.0117(12) 0.0017(12) -0.0014(10) 0.0007(10) 0.0031(9) O2 0.0108(17) 0.029(2) 0.019(2) 0.000 0.000 -0.0065(15) O3 0.0193(14) 0.0163(13) 0.0036(14) -0.0006(11) 0.0024(11) 0.0060(10) O4 0.0114(16) 0.0141(16) 0.0018(18) 0.000 0.000 0.0006(14) O5 0.0118(17) 0.024(2) 0.003(2) 0.0028(15) 0.000 0.000 O6 0.020(2) 0.0146(19) 0.012(2) 0.000 0.000 -0.0067(16) O7 0.0168(18) 0.0090(16) 0.007(2) 0.000 0.000 -0.0033(14) _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 O2 2.431(4) 1_655 ? La1 O6 2.445(3) . ? La1 O1 2.500(3) 2_355 ? La1 O1 2.500(3) 5_355 ? La1 O3 2.573(3) . ? La1 O3 2.573(3) 6_556 ? La1 O7 2.592(4) . ? La1 O1 2.715(2) . ? La1 O1 2.715(2) 6_556 ? La1 I1 3.5294(10) . ? V1 O3 1.658(3) 3_545 ? V1 O3 1.658(3) . ? V1 O5 1.921(4) . ? V1 O4 1.9318(12) . ? V1 O4 1.9318(12) 3_545 ? V1 V2 3.0871(11) 1_655 ? V1 V2 3.0871(11) 3_645 ? V2 O6 1.634(3) . ? V2 O7 1.651(4) 7_355 ? V2 O5 1.9323(11) 1_455 ? V2 O5 1.9323(11) 6_456 ? V2 O4 2.020(4) 1_455 ? V2 V1 3.0871(11) 1_455 ? V2 V1 3.0871(11) 6_456 ? I1 O2 1.777(4) . ? I1 O1 1.824(3) . ? I1 O1 1.824(3) 6_556 ? O1 La1 2.500(3) 5_355 ? O2 La1 2.431(4) 1_455 ? O4 V1 1.9318(12) 6_556 ? O4 V2 2.020(4) 1_655 ? O5 V2 1.9323(11) 1_655 ? O5 V2 1.9323(11) 3_645 ? O7 V2 1.651(4) 7_365 ? 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 O2 La1 O6 135.70(13) 1_655 . ? O2 La1 O1 80.38(6) 1_655 2_355 ? O6 La1 O1 108.80(6) . 2_355 ? O2 La1 O1 80.38(6) 1_655 5_355 ? O6 La1 O1 108.80(6) . 5_355 ? O1 La1 O1 140.88(12) 2_355 5_355 ? O2 La1 O3 72.93(10) 1_655 . ? O6 La1 O3 71.50(9) . . ? O1 La1 O3 136.25(8) 2_355 . ? O1 La1 O3 67.52(8) 5_355 . ? O2 La1 O3 72.93(10) 1_655 6_556 ? O6 La1 O3 71.50(9) . 6_556 ? O1 La1 O3 67.52(8) 2_355 6_556 ? O1 La1 O3 136.25(8) 5_355 6_556 ? O3 La1 O3 71.77(12) . 6_556 ? O2 La1 O7 82.81(13) 1_655 . ? O6 La1 O7 141.49(11) . . ? O1 La1 O7 72.02(6) 2_355 . ? O1 La1 O7 72.02(6) 5_355 . ? O3 La1 O7 135.43(7) . . ? O3 La1 O7 135.43(7) 6_556 . ? O2 La1 O1 138.16(9) 1_655 . ? O6 La1 O1 78.00(9) . . ? O1 La1 O1 116.07(6) 2_355 . ? O1 La1 O1 62.57(9) 5_355 . ? O3 La1 O1 106.87(8) . . ? O3 La1 O1 148.24(8) 6_556 . ? O7 La1 O1 68.37(9) . . ? O2 La1 O1 138.16(9) 1_655 6_556 ? O6 La1 O1 78.00(9) . 6_556 ? O1 La1 O1 62.57(9) 2_355 6_556 ? O1 La1 O1 116.07(6) 5_355 6_556 ? O3 La1 O1 148.24(8) . 6_556 ? O3 La1 O1 106.87(8) 6_556 6_556 ? O7 La1 O1 68.37(9) . 6_556 ? O1 La1 O1 57.07(11) . 6_556 ? O2 La1 I1 136.56(10) 1_655 . ? O6 La1 I1 87.74(9) . . ? O1 La1 I1 85.52(5) 2_355 . ? O1 La1 I1 85.52(5) 5_355 . ? O3 La1 I1 137.08(6) . . ? O3 La1 I1 137.08(6) 6_556 . ? O7 La1 I1 53.75(8) . . ? O1 La1 I1 30.56(6) . . ? O1 La1 I1 30.56(6) 6_556 . ? O3 V1 O3 110.49(19) 3_545 . ? O3 V1 O5 124.75(10) 3_545 . ? O3 V1 O5 124.75(10) . . ? O3 V1 O4 97.71(14) 3_545 . ? O3 V1 O4 97.66(14) . . ? O5 V1 O4 76.43(10) . . ? O3 V1 O4 97.66(14) 3_545 3_545 ? O3 V1 O4 97.71(14) . 3_545 ? O5 V1 O4 76.43(10) . 3_545 ? O4 V1 O4 152.9(2) . 3_545 ? O3 V1 V2 119.24(9) 3_545 1_655 ? O3 V1 V2 115.05(10) . 1_655 ? O5 V1 V2 36.884(17) . 1_655 ? O4 V1 V2 39.66(10) . 1_655 ? O4 V1 V2 113.24(11) 3_545 1_655 ? O3 V1 V2 115.05(10) 3_545 3_645 ? O3 V1 V2 119.24(9) . 3_645 ? O5 V1 V2 36.884(17) . 3_645 ? O4 V1 V2 113.24(11) . 3_645 ? O4 V1 V2 39.66(10) 3_545 3_645 ? V2 V1 V2 73.77(3) 1_655 3_645 ? O6 V2 O7 107.78(19) . 7_355 ? O6 V2 O5 95.70(9) . 1_455 ? O7 V2 O5 105.43(5) 7_355 1_455 ? O6 V2 O5 95.70(9) . 6_456 ? O7 V2 O5 105.43(5) 7_355 6_456 ? O5 V2 O5 141.86(17) 1_455 6_456 ? O6 V2 O4 140.95(17) . 1_455 ? O7 V2 O4 111.26(17) 7_355 1_455 ? O5 V2 O4 74.14(10) 1_455 1_455 ? O5 V2 O4 74.14(10) 6_456 1_455 ? O6 V2 V1 121.36(10) . 1_455 ? O7 V2 V1 115.31(10) 7_355 1_455 ? O5 V2 V1 36.63(10) 1_455 1_455 ? O5 V2 V1 108.40(10) 6_456 1_455 ? O4 V2 V1 37.62(3) 1_455 1_455 ? O6 V2 V1 121.36(10) . 6_456 ? O7 V2 V1 115.31(10) 7_355 6_456 ? O5 V2 V1 108.40(10) 1_455 6_456 ? O5 V2 V1 36.63(10) 6_456 6_456 ? O4 V2 V1 37.62(3) 1_455 6_456 ? V1 V2 V1 72.54(3) 1_455 6_456 ? O2 I1 O1 100.83(12) . . ? O2 I1 O1 100.83(12) . 6_556 ? O1 I1 O1 90.67(16) . 6_556 ? O2 I1 La1 127.15(14) . . ? O1 I1 La1 49.20(8) . . ? O1 I1 La1 49.20(8) 6_556 . ? I1 O1 La1 122.33(12) . 5_355 ? I1 O1 La1 100.23(11) . . ? La1 O1 La1 117.43(9) 5_355 . ? I1 O2 La1 170.6(2) . 1_455 ? V1 O3 La1 154.99(15) . . ? V1 O4 V1 141.94(19) 6_556 . ? V1 O4 V2 102.72(11) 6_556 1_655 ? V1 O4 V2 102.72(11) . 1_655 ? V1 O5 V2 106.49(10) . 1_655 ? V1 O5 V2 106.49(10) . 3_645 ? V2 O5 V2 147.0(2) 1_655 3_645 ? V2 O6 La1 160.7(2) . . ? V2 O7 La1 144.8(2) 7_365 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.401 _refine_diff_density_min -1.777 _refine_diff_density_rms 0.279 #===end data_LaVO2(IO3)4.H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I4 La O14 V, H2 O' _chemical_formula_sum 'H2 I4 La O15 V' _chemical_formula_weight 939.47 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' 'I' 'I' -0.4742 1.8119 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 '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 21' _symmetry_space_group_name_Hall 'P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.0737(5) _cell_length_b 14.2499(6) _cell_length_c 7.1663(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.659(4) _cell_angle_gamma 90.00 _cell_volume 645.57(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1991 _cell_measurement_theta_min 3.1807 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Orange' _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 13.634 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4077 _exptl_absorpt_process_details 'CrystalClear' _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 'Mercury70' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4919 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2803 _reflns_number_gt 2740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0192P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0283(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 2803 _refine_ls_number_parameters 191 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 -0.92188(6) 0.25763(3) -0.57271(6) 0.00649(10) Uani 1 1 d . . . I1 I -0.83481(7) 0.38626(3) -1.04049(7) 0.00722(11) Uani 1 1 d . . . I2 I -1.24669(7) 0.50635(3) -0.68354(7) 0.00720(11) Uani 1 1 d . . . I3 I -1.53215(7) 0.16167(3) -0.76300(7) 0.00650(11) Uani 1 1 d . . . I4 I -1.25791(7) 0.20407(3) -1.13958(7) 0.00697(11) Uani 1 1 d . . . V1 V -0.41916(19) 0.42914(9) -1.20469(19) 0.0068(3) Uani 1 1 d . . . O1 O -0.7618(8) 0.3237(4) -0.8000(8) 0.0120(12) Uani 1 1 d . . . O2 O -0.9043(8) 0.2859(4) -1.2110(8) 0.0133(12) Uani 1 1 d . . . O3 O -0.5657(8) 0.4113(4) -0.9958(9) 0.0128(12) Uani 1 1 d . . . O4 O -1.0565(9) 0.4148(4) -0.5704(9) 0.0160(13) Uani 1 1 d . . . O5 O -1.2294(8) 0.5109(4) -0.9322(8) 0.0129(11) Uani 1 1 d . . . O6 O -0.9273(8) 0.1026(4) -0.4326(8) 0.0135(12) Uani 1 1 d . . . O7 O -1.2971(9) 0.2308(4) -0.6456(9) 0.0140(12) Uani 1 1 d . . . O8 O -1.4060(8) 0.0443(4) -0.7063(8) 0.0100(11) Uani 1 1 d . . . O9 O -0.6057(8) 0.1634(4) -0.5513(8) 0.0100(10) Uani 1 1 d . . . O10 O -1.4854(8) 0.1630(5) -1.1113(9) 0.0166(12) Uani 1 1 d . . . O11 O -1.2295(8) 0.3249(4) -1.0277(9) 0.0127(12) Uani 1 1 d . . . O12 O -1.0468(8) 0.1585(4) -0.9027(8) 0.0130(11) Uani 1 1 d . . . O13 O -0.5967(8) 0.3582(4) -0.3736(9) 0.0131(12) Uani 1 1 d . . . O14 O -0.2677(8) 0.4605(4) -1.3110(9) 0.0143(12) Uani 1 1 d . . . O1W O -1.2174(9) 0.0353(4) -1.2465(9) 0.0165(12) Uani 1 1 d . . . H1 H -1.1713 0.0501 -1.3335 0.020 Uiso 1 1 d R . . H2 H -1.1803 -0.0206 -1.2045 0.020 Uiso 1 1 d 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 La1 0.00614(19) 0.0055(2) 0.0093(2) -0.00107(16) 0.00472(16) -0.00107(15) I1 0.0052(2) 0.0072(2) 0.0084(2) 0.00034(18) 0.00226(17) 0.00005(17) I2 0.0060(2) 0.0064(2) 0.0089(2) -0.00079(18) 0.00305(17) 0.00013(18) I3 0.00436(19) 0.0071(2) 0.0080(2) -0.00057(17) 0.00272(17) -0.00015(17) I4 0.0058(2) 0.0074(2) 0.0071(2) -0.00086(19) 0.00226(17) -0.00161(18) V1 0.0056(6) 0.0062(6) 0.0082(6) -0.0011(5) 0.0028(5) -0.0003(5) O1 0.010(2) 0.018(3) 0.010(3) 0.000(2) 0.007(2) -0.006(2) O2 0.013(2) 0.015(3) 0.012(3) -0.006(2) 0.005(2) -0.005(2) O3 0.008(2) 0.015(3) 0.019(3) -0.002(2) 0.009(2) -0.006(2) O4 0.020(3) 0.011(3) 0.017(3) 0.006(2) 0.008(2) 0.006(2) O5 0.009(2) 0.018(3) 0.012(3) -0.001(2) 0.005(2) -0.005(2) O6 0.011(2) 0.012(3) 0.019(3) 0.003(3) 0.008(2) 0.001(2) O7 0.012(3) 0.008(3) 0.022(3) -0.005(2) 0.007(2) -0.005(2) O8 0.009(2) 0.006(3) 0.014(3) 0.002(2) 0.004(2) 0.000(2) O9 0.012(2) 0.011(3) 0.013(3) 0.001(2) 0.010(2) 0.001(2) O10 0.014(3) 0.025(3) 0.016(3) -0.005(3) 0.011(2) -0.009(3) O11 0.010(2) 0.010(3) 0.019(3) -0.003(2) 0.006(2) 0.002(2) O12 0.015(2) 0.014(3) 0.007(2) 0.000(2) 0.002(2) 0.003(2) O13 0.011(3) 0.010(3) 0.015(3) -0.005(2) 0.003(2) -0.005(2) O14 0.009(2) 0.018(3) 0.018(3) -0.002(2) 0.009(2) 0.000(2) O1W 0.017(3) 0.013(3) 0.023(3) 0.000(3) 0.012(2) -0.001(2) _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 O6 2.434(6) . ? La1 O4 2.437(6) . ? La1 O7 2.494(5) . ? La1 O13 2.537(5) . ? La1 O1 2.545(5) . ? La1 O12 2.548(6) . ? La1 O9 2.554(5) . ? La1 O2 2.571(5) 1_556 ? La1 I4 3.7510(7) . ? I1 O1 1.798(5) . ? I1 O2 1.801(6) . ? I1 O3 1.818(5) . ? I2 O6 1.780(5) 2_354 ? I2 O4 1.786(6) . ? I2 O5 1.841(5) . ? I3 O7 1.786(5) . ? I3 O9 1.811(5) 1_455 ? I3 O8 1.852(6) . ? I4 O12 1.805(5) . ? I4 O10 1.807(5) . ? I4 O11 1.872(6) . ? I4 O1W 2.579(6) . ? V1 O14 1.631(6) . ? V1 O13 1.644(5) 1_554 ? V1 O8 1.981(6) 2_353 ? V1 O11 2.022(6) 1_655 ? V1 O5 2.150(5) 1_655 ? V1 O3 2.185(6) . ? O2 La1 2.571(5) 1_554 ? O5 V1 2.150(5) 1_455 ? O6 I2 1.780(5) 2_344 ? O8 V1 1.981(6) 2_343 ? O9 I3 1.811(5) 1_655 ? O11 V1 2.022(6) 1_455 ? O13 V1 1.644(5) 1_556 ? O1W H1 0.8501 . ? O1W H2 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 La1 O4 138.8(2) . . ? O6 La1 O7 74.64(18) . . ? O4 La1 O7 76.11(19) . . ? O6 La1 O13 117.32(18) . . ? O4 La1 O13 74.65(19) . . ? O7 La1 O13 144.65(18) . . ? O6 La1 O1 133.90(18) . . ? O4 La1 O1 87.24(19) . . ? O7 La1 O1 131.28(18) . . ? O13 La1 O1 66.40(18) . . ? O6 La1 O12 79.44(19) . . ? O4 La1 O12 122.82(18) . . ? O7 La1 O12 80.06(17) . . ? O13 La1 O12 133.18(18) . . ? O1 La1 O12 71.29(18) . . ? O6 La1 O9 70.95(17) . . ? O4 La1 O9 144.79(19) . . ? O7 La1 O9 138.89(18) . . ? O13 La1 O9 73.40(17) . . ? O1 La1 O9 66.64(18) . . ? O12 La1 O9 72.19(16) . . ? O6 La1 O2 74.26(18) . 1_556 ? O4 La1 O2 72.03(19) . 1_556 ? O7 La1 O2 78.50(17) . 1_556 ? O13 La1 O2 73.92(18) . 1_556 ? O1 La1 O2 138.90(18) . 1_556 ? O12 La1 O2 149.59(19) . 1_556 ? O9 La1 O2 112.15(17) . 1_556 ? O6 La1 I4 98.18(13) . . ? O4 La1 I4 97.75(13) . . ? O7 La1 I4 69.16(13) . . ? O13 La1 I4 134.28(13) . . ? O1 La1 I4 68.26(12) . . ? O12 La1 I4 25.14(13) . . ? O9 La1 I4 94.04(12) . . ? O2 La1 I4 147.61(12) 1_556 . ? O1 I1 O2 97.4(3) . . ? O1 I1 O3 95.8(2) . . ? O2 I1 O3 102.8(3) . . ? O6 I2 O4 97.4(2) 2_354 . ? O6 I2 O5 95.3(2) 2_354 . ? O4 I2 O5 95.8(3) . . ? O7 I3 O9 98.9(2) . 1_455 ? O7 I3 O8 98.0(2) . . ? O9 I3 O8 96.9(2) 1_455 . ? O12 I4 O10 100.4(3) . . ? O12 I4 O11 92.5(3) . . ? O10 I4 O11 100.4(3) . . ? O12 I4 O1W 77.8(2) . . ? O10 I4 O1W 87.4(2) . . ? O11 I4 O1W 168.6(2) . . ? O12 I4 La1 36.85(19) . . ? O10 I4 La1 96.20(18) . . ? O11 I4 La1 56.97(17) . . ? O1W I4 La1 114.24(13) . . ? O14 V1 O13 105.6(3) . 1_554 ? O14 V1 O8 93.9(3) . 2_353 ? O13 V1 O8 96.5(3) 1_554 2_353 ? O14 V1 O11 96.0(3) . 1_655 ? O13 V1 O11 94.7(3) 1_554 1_655 ? O8 V1 O11 162.5(2) 2_353 1_655 ? O14 V1 O5 90.1(3) . 1_655 ? O13 V1 O5 164.2(3) 1_554 1_655 ? O8 V1 O5 83.6(2) 2_353 1_655 ? O11 V1 O5 82.0(2) 1_655 1_655 ? O14 V1 O3 164.8(3) . . ? O13 V1 O3 89.6(3) 1_554 . ? O8 V1 O3 84.1(2) 2_353 . ? O11 V1 O3 82.5(2) 1_655 . ? O5 V1 O3 74.7(2) 1_655 . ? I1 O1 La1 141.1(3) . . ? I1 O2 La1 133.1(3) . 1_554 ? I1 O3 V1 133.1(3) . . ? I2 O4 La1 152.3(3) . . ? I2 O5 V1 125.1(3) . 1_455 ? I2 O6 La1 139.2(3) 2_344 . ? I3 O7 La1 149.5(3) . . ? I3 O8 V1 120.5(3) . 2_343 ? I3 O9 La1 122.0(2) 1_655 . ? I4 O11 V1 119.6(3) . 1_455 ? I4 O12 La1 118.0(3) . . ? V1 O13 La1 164.2(3) 1_556 . ? I4 O1W H1 96.7 . . ? I4 O1W H2 145.7 . . ? H1 O1W H2 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 O1W H2 O1 0.85 2.26 3.045(8) 153.6 2_343 O1W H1 O6 0.85 2.27 3.060(8) 155.3 1_554 O1W H1 O8 0.85 2.43 2.951(8) 120.0 1_554 O1W H2 I1 0.85 2.17 2.863(6) 139.1 2_343 O1W H1 I2 0.85 2.97 3.560(6) 128.3 2_343 O1W H1 I3 0.85 3.39 3.809(6) 113.8 1_554 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.887 _refine_diff_density_min -1.524 _refine_diff_density_rms 0.225