# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 912014' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H30 Ce2 Mn N O49 V13' _chemical_formula_weight 1885.70 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 26.671(4) _cell_length_b 26.671(4) _cell_length_c 30.260(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21525(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9447 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7192 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.690 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 77027 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9447 _reflns_number_gt 8294 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.003 -0.007 -0.003 13676.7 273.6 _platon_squeeze_details ; ; _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^)+(0.0500P)^2^+400.0000P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 9447 _refine_ls_number_parameters 301 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.026 _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 Ce1 Ce 0.152810(19) 0.428040(19) -0.218080(19) 0.02975(14) Uani 1 1 d . . . Mn Mn 0.2500 0.57195(7) -0.1250 0.0241(4) Uani 1 2 d S . . V3 V 0.34996(6) 0.51529(6) -0.13465(5) 0.0274(3) Uani 1 1 d . . . V4 V 0.2500 0.45338(8) -0.1250 0.0254(5) Uani 1 2 d S . . V5 V 0.26908(6) 0.51519(6) -0.21156(6) 0.0290(4) Uani 1 1 d . . . V6 V 0.34336(7) 0.63716(6) -0.13194(6) 0.0365(4) Uani 1 1 d . . . V7 V 0.16681(5) 0.57290(6) -0.20350(5) 0.0280(3) Uani 1 1 d . . . V8 V 0.36537(6) 0.58024(7) -0.21923(7) 0.0408(4) Uani 1 1 d . . . V9 V 0.26429(6) 0.63681(6) -0.20720(6) 0.0365(4) Uani 1 1 d . . . O19 O 0.3002(2) 0.4750(2) -0.1660(2) 0.0281(14) Uani 1 1 d . . . O18 O 0.2161(2) 0.5220(2) -0.1565(2) 0.0235(13) Uani 1 1 d . . . O17 O 0.1430(2) 0.5205(2) -0.2243(2) 0.0324(15) Uani 1 1 d . . . O16 O 0.1326(2) 0.5745(2) -0.1478(2) 0.0284(14) Uani 1 1 d . . . O15 O 0.3213(2) 0.5258(3) -0.2420(2) 0.0386(17) Uani 1 1 d . . . O14 O 0.2134(2) 0.6197(2) -0.1604(2) 0.0296(15) Uani 1 1 d . . . O13 O 0.3875(2) 0.5263(3) -0.1797(2) 0.0371(16) Uani 1 1 d . . . O12 O 0.3007(2) 0.5727(2) -0.1669(2) 0.0281(13) Uani 1 1 d . . . O11 O 0.2323(2) 0.5742(2) -0.2294(2) 0.0305(14) Uani 1 1 d . . . O10 O 0.1385(2) 0.6175(2) -0.2301(2) 0.0363(17) Uani 1 1 d . . . O9 O 0.2373(2) 0.4715(2) -0.2366(2) 0.0354(16) Uani 1 1 d . . . O8 O 0.2342(3) 0.6790(3) -0.2331(3) 0.048(2) Uani 1 1 d . . . O7 O 0.3764(2) 0.4717(2) -0.1057(2) 0.0334(16) Uani 1 1 d . . . O6 O 0.3723(3) 0.6785(3) -0.1038(3) 0.049(2) Uani 1 1 d . . . O5 O 0.3861(3) 0.6243(3) -0.1766(3) 0.0430(18) Uani 1 1 d . . . O4 O 0.3003(3) 0.6723(2) -0.1666(3) 0.0415(19) Uani 1 1 d . . . O3 O 0.2163(2) 0.4169(2) -0.1568(2) 0.0328(15) Uani 1 1 d . . . O2 O 0.3187(3) 0.6243(3) -0.2412(3) 0.0430(18) Uani 1 1 d . . . O4W O 0.0613(3) 0.4397(3) -0.2262(3) 0.0456(19) Uani 1 1 d . . . O3W O 0.1239(3) 0.3600(3) -0.1692(3) 0.057(2) Uani 1 1 d . . . O1 O 0.4091(3) 0.5802(3) -0.2549(3) 0.057(2) Uani 1 1 d . . . O2W O 0.1541(4) 0.4539(3) -0.2976(3) 0.054(2) Uani 1 1 d . . . OW1 O 0.5411(5) 0.7017(5) -0.0754(4) 0.096(4) Uiso 1 1 d . . . O1W O 0.2160(3) 0.3625(3) -0.2407(3) 0.057(2) Uiso 1 1 d . . . C3 C 0.0000 0.5000 -0.0588(5) 0.075(6) Uiso 1 2 d SD . . C2 C 0.0000 0.5000 -0.1380(5) 0.084(7) Uiso 1 2 d SD . . C1 C 0.0000(15) 0.4470(4) -0.1215(7) 0.088(10) Uiso 0.50 1 d PD . . N1 N 0.0157(9) 0.5282(5) -0.0985(5) 0.19(2) Uiso 0.50 1 d PD . . C4 C -0.0032(9) 0.5762(7) -0.1173(7) 0.047(5) Uiso 0.50 1 d PD . . C5 C 0.0131(9) 0.4480(4) -0.0736(5) 0.056 Uiso 0.50 1 d PD . . O20 O 0.0000 0.5000 -0.1803(5) 0.064(3) Uiso 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 Ce1 0.0302(3) 0.0267(3) 0.0323(3) -0.0061(2) -0.0101(2) 0.0005(2) Mn 0.0234(9) 0.0226(9) 0.0263(11) 0.000 -0.0083(7) 0.000 V3 0.0228(7) 0.0293(8) 0.0302(9) 0.0031(6) -0.0058(7) 0.0009(7) V4 0.0262(11) 0.0230(10) 0.0268(13) 0.000 -0.0081(9) 0.000 V5 0.0285(8) 0.0329(8) 0.0256(9) -0.0004(7) -0.0055(7) 0.0003(6) V6 0.0367(9) 0.0301(8) 0.0426(11) 0.0096(7) -0.0150(8) -0.0090(7) V7 0.0286(8) 0.0258(7) 0.0297(9) 0.0010(7) -0.0111(6) 0.0007(7) V8 0.0325(8) 0.0516(11) 0.0382(11) 0.0135(9) -0.0009(8) -0.0051(8) V9 0.0354(9) 0.0331(9) 0.0410(11) 0.0124(8) -0.0118(8) -0.0045(7) O19 0.026(3) 0.026(3) 0.032(4) -0.002(3) -0.007(3) 0.002(3) O18 0.025(3) 0.025(3) 0.021(3) 0.003(3) -0.009(2) 0.000(2) O17 0.033(3) 0.034(3) 0.030(4) -0.005(3) -0.014(3) 0.000(3) O16 0.021(3) 0.028(3) 0.036(4) 0.001(3) -0.007(3) -0.002(3) O15 0.032(4) 0.053(4) 0.031(4) 0.001(3) 0.001(3) 0.002(3) O14 0.025(3) 0.024(3) 0.040(4) 0.004(3) -0.011(3) 0.001(3) O13 0.027(3) 0.046(4) 0.037(4) 0.001(3) -0.001(3) 0.000(3) O12 0.023(3) 0.030(3) 0.031(4) 0.008(3) -0.004(2) -0.003(3) O11 0.027(3) 0.035(3) 0.030(4) 0.005(3) -0.012(3) -0.003(3) O10 0.033(4) 0.032(3) 0.044(5) 0.006(3) -0.016(3) -0.003(3) O9 0.034(4) 0.037(4) 0.035(4) -0.006(3) -0.008(3) 0.004(3) O8 0.046(4) 0.041(4) 0.058(6) 0.018(4) -0.017(4) -0.006(3) O7 0.037(4) 0.025(3) 0.039(4) 0.004(3) -0.004(3) 0.000(3) O6 0.049(4) 0.039(4) 0.059(6) 0.007(4) -0.029(4) -0.012(3) O5 0.033(4) 0.054(5) 0.042(5) 0.019(4) -0.008(3) -0.007(3) O4 0.036(4) 0.031(4) 0.058(5) 0.010(3) -0.018(3) -0.011(3) O3 0.035(3) 0.028(3) 0.035(4) -0.006(3) -0.007(3) 0.001(3) O2 0.040(4) 0.048(4) 0.041(5) 0.013(3) -0.009(3) -0.004(3) O4W 0.036(4) 0.049(4) 0.052(5) -0.016(4) -0.008(3) 0.001(3) O3W 0.069(6) 0.042(5) 0.059(6) 0.011(4) -0.015(4) -0.011(4) O1 0.043(4) 0.076(6) 0.052(5) 0.015(5) 0.006(4) -0.003(4) O2W 0.080(6) 0.043(4) 0.039(5) -0.008(3) -0.011(4) -0.003(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 Ce1 O3W 2.466(8) . ? Ce1 O4W 2.473(7) . ? Ce1 O17 2.488(6) . ? Ce1 O2W 2.504(8) . ? Ce1 O1W 2.522(9) . ? Ce1 O3 2.530(7) . ? Ce1 O10 2.549(6) 11_454 ? Ce1 O9 2.595(7) . ? Ce1 O7 2.635(7) 5_554 ? Mn O12 1.854(6) 5_554 ? Mn O12 1.854(6) . ? Mn O18 1.871(6) . ? Mn O18 1.871(6) 5_554 ? Mn O14 1.930(6) 5_554 ? Mn O14 1.930(6) . ? Mn V6 3.045(2) 5_554 ? Mn V6 3.045(2) . ? Mn V9 3.054(2) 5_554 ? Mn V9 3.054(2) . ? Mn V5 3.068(2) . ? Mn V5 3.068(2) 5_554 ? V3 O7 1.617(6) . ? V3 O13 1.717(7) . ? V3 O16 1.917(6) 5_554 ? V3 O19 1.952(6) . ? V3 O18 2.165(6) 5_554 ? V3 O12 2.242(6) . ? V3 V7 3.111(2) 5_554 ? V3 V8 3.118(2) . ? V4 O3 1.636(6) . ? V4 O3 1.636(6) 5_554 ? V4 O19 1.914(7) 5_554 ? V4 O19 1.914(7) . ? V4 O18 2.251(6) 5_554 ? V4 O18 2.251(6) . ? V5 O9 1.628(7) . ? V5 O15 1.693(7) . ? V5 O19 1.934(6) . ? V5 O11 1.933(7) . ? V5 O18 2.192(6) . ? V5 O12 2.211(7) . ? V5 V8 3.108(2) . ? V6 O6 1.593(7) . ? V6 O5 1.799(8) . ? V6 O4 1.815(7) . ? V6 O16 2.004(6) 5_554 ? V6 O14 2.038(7) 5_554 ? V6 O12 2.318(7) . ? V6 V9 3.104(2) . ? V6 V8 3.103(3) . ? V6 V7 3.114(2) 5_554 ? V7 O10 1.623(6) . ? V7 O17 1.659(6) . ? V7 O11 1.915(6) . ? V7 O16 1.917(7) . ? V7 O14 2.192(6) . ? V7 O18 2.367(6) . ? V7 V3 3.111(2) 5_554 ? V7 V9 3.111(2) . ? V7 V6 3.114(2) 5_554 ? V8 O1 1.589(8) . ? V8 O2 1.835(7) . ? V8 O5 1.831(8) . ? V8 O13 1.961(7) . ? V8 O15 1.991(7) . ? V8 O12 2.350(6) . ? V8 V9 3.111(3) . ? V9 O8 1.590(7) . ? V9 O2 1.810(8) . ? V9 O4 1.824(7) . ? V9 O11 1.991(7) . ? V9 O14 2.012(7) . ? V9 O12 2.313(6) . ? O18 V3 2.165(6) 5_554 ? O16 V3 1.917(6) 5_554 ? O16 V6 2.004(6) 5_554 ? O14 V6 2.038(7) 5_554 ? O10 Ce1 2.549(6) 12_554 ? O7 Ce1 2.635(7) 5_554 ? C3 N1 1.478(10) 2_565 ? C3 N1 1.478(10) . ? C3 C5 1.499(9) 2_565 ? C3 C5 1.499(9) . ? C2 O20 1.279(18) . ? C2 N1 1.473(10) . ? C2 N1 1.473(10) 2_565 ? C2 C1 1.499(10) 2_565 ? C2 C1 1.499(10) . ? C1 C4 0.64(2) 2_565 ? C1 N1 1.05(3) 2_565 ? C1 C5 1.490(10) . ? N1 C1 1.05(3) 2_565 ? N1 C5 1.25(2) 2_565 ? N1 C4 1.489(10) . ? N1 N1 1.72(3) 2_565 ? C4 C1 0.64(2) 2_565 ? C4 C5 1.50(2) 2_565 ? C5 N1 1.25(2) 2_565 ? C5 C4 1.50(2) 2_565 ? 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 O3W Ce1 O4W 81.0(3) . . ? O3W Ce1 O17 137.9(3) . . ? O4W Ce1 O17 76.3(2) . . ? O3W Ce1 O2W 141.6(3) . . ? O4W Ce1 O2W 83.4(3) . . ? O17 Ce1 O2W 69.9(2) . . ? O3W Ce1 O1W 82.0(3) . . ? O4W Ce1 O1W 136.0(3) . . ? O17 Ce1 O1W 137.5(2) . . ? O2W Ce1 O1W 85.4(3) . . ? O3W Ce1 O3 71.5(2) . . ? O4W Ce1 O3 138.4(2) . . ? O17 Ce1 O3 104.0(2) . . ? O2W Ce1 O3 136.7(3) . . ? O1W Ce1 O3 70.8(2) . . ? O3W Ce1 O10 75.0(3) . 11_454 ? O4W Ce1 O10 70.2(2) . 11_454 ? O17 Ce1 O10 127.2(2) . 11_454 ? O2W Ce1 O10 66.7(2) . 11_454 ? O1W Ce1 O10 66.2(2) . 11_454 ? O3 Ce1 O10 128.1(2) . 11_454 ? O3W Ce1 O9 136.9(2) . . ? O4W Ce1 O9 141.2(2) . . ? O17 Ce1 O9 68.4(2) . . ? O2W Ce1 O9 70.0(3) . . ? O1W Ce1 O9 70.8(2) . . ? O3 Ce1 O9 68.2(2) . . ? O10 Ce1 O9 119.9(2) 11_454 . ? O3W Ce1 O7 74.0(3) . 5_554 ? O4W Ce1 O7 74.7(2) . 5_554 ? O17 Ce1 O7 66.1(2) . 5_554 ? O2W Ce1 O7 134.2(2) . 5_554 ? O1W Ce1 O7 137.2(3) . 5_554 ? O3 Ce1 O7 68.2(2) . 5_554 ? O10 Ce1 O7 136.1(2) 11_454 5_554 ? O9 Ce1 O7 104.0(2) . 5_554 ? O12 Mn O12 178.8(4) 5_554 . ? O12 Mn O18 90.2(3) 5_554 . ? O12 Mn O18 90.7(3) . . ? O12 Mn O18 90.7(3) 5_554 5_554 ? O12 Mn O18 90.2(3) . 5_554 ? O18 Mn O18 89.1(4) . 5_554 ? O12 Mn O14 88.9(3) 5_554 5_554 ? O12 Mn O14 90.3(3) . 5_554 ? O18 Mn O14 175.8(3) . 5_554 ? O18 Mn O14 86.8(2) 5_554 5_554 ? O12 Mn O14 90.3(3) 5_554 . ? O12 Mn O14 88.9(3) . . ? O18 Mn O14 86.8(2) . . ? O18 Mn O14 175.8(3) 5_554 . ? O14 Mn O14 97.4(4) 5_554 . ? O12 Mn V6 49.5(2) 5_554 5_554 ? O12 Mn V6 129.6(2) . 5_554 ? O18 Mn V6 92.71(18) . 5_554 ? O18 Mn V6 140.08(19) 5_554 5_554 ? O14 Mn V6 89.88(19) 5_554 5_554 ? O14 Mn V6 41.2(2) . 5_554 ? O12 Mn V6 129.6(2) 5_554 . ? O12 Mn V6 49.5(2) . . ? O18 Mn V6 140.08(19) . . ? O18 Mn V6 92.71(18) 5_554 . ? O14 Mn V6 41.2(2) 5_554 . ? O14 Mn V6 89.88(19) . . ? V6 Mn V6 110.32(9) 5_554 . ? O12 Mn V9 49.11(19) 5_554 5_554 ? O12 Mn V9 130.0(2) . 5_554 ? O18 Mn V9 139.28(19) . 5_554 ? O18 Mn V9 92.83(18) 5_554 5_554 ? O14 Mn V9 40.2(2) 5_554 5_554 ? O14 Mn V9 90.9(2) . 5_554 ? V6 Mn V9 61.19(5) 5_554 5_554 ? V6 Mn V9 80.48(6) . 5_554 ? O12 Mn V9 130.0(2) 5_554 . ? O12 Mn V9 49.11(19) . . ? O18 Mn V9 92.83(18) . . ? O18 Mn V9 139.28(19) 5_554 . ? O14 Mn V9 90.9(2) 5_554 . ? O14 Mn V9 40.2(2) . . ? V6 Mn V9 80.48(6) 5_554 . ? V6 Mn V9 61.19(5) . . ? V9 Mn V9 110.99(9) 5_554 . ? O12 Mn V5 135.3(2) 5_554 . ? O12 Mn V5 45.6(2) . . ? O18 Mn V5 45.08(19) . . ? O18 Mn V5 90.16(19) 5_554 . ? O14 Mn V5 135.8(2) 5_554 . ? O14 Mn V5 86.3(2) . . ? V6 Mn V5 118.45(4) 5_554 . ? V6 Mn V5 95.01(5) . . ? V9 Mn V5 174.70(7) 5_554 . ? V9 Mn V5 64.11(5) . . ? O12 Mn V5 45.6(2) 5_554 5_554 ? O12 Mn V5 135.3(2) . 5_554 ? O18 Mn V5 90.16(19) . 5_554 ? O18 Mn V5 45.08(19) 5_554 5_554 ? O14 Mn V5 86.3(2) 5_554 5_554 ? O14 Mn V5 135.8(2) . 5_554 ? V6 Mn V5 95.01(5) 5_554 5_554 ? V6 Mn V5 118.45(4) . 5_554 ? V9 Mn V5 64.11(5) 5_554 5_554 ? V9 Mn V5 174.70(7) . 5_554 ? V5 Mn V5 120.87(8) . 5_554 ? O7 V3 O13 107.5(3) . . ? O7 V3 O16 102.0(3) . 5_554 ? O13 V3 O16 97.1(3) . 5_554 ? O7 V3 O19 99.4(3) . . ? O13 V3 O19 96.0(3) . . ? O16 V3 O19 150.1(3) 5_554 . ? O7 V3 O18 95.8(3) . 5_554 ? O13 V3 O18 156.5(3) . 5_554 ? O16 V3 O18 80.5(2) 5_554 5_554 ? O19 V3 O18 76.8(2) . 5_554 ? O7 V3 O12 169.2(3) . . ? O13 V3 O12 83.1(3) . . ? O16 V3 O12 78.6(2) 5_554 . ? O19 V3 O12 76.4(2) . . ? O18 V3 O12 73.5(2) 5_554 . ? O7 V3 Mn 132.7(3) . . ? O13 V3 Mn 119.8(2) . . ? O16 V3 Mn 75.96(17) 5_554 . ? O19 V3 Mn 74.19(18) . . ? O18 V3 Mn 36.86(15) 5_554 . ? O12 V3 Mn 36.70(16) . . ? O7 V3 V7 87.3(3) . 5_554 ? O13 V3 V7 132.8(2) . 5_554 ? O16 V3 V7 35.78(19) 5_554 5_554 ? O19 V3 V7 126.2(2) . 5_554 ? O18 V3 V7 49.42(15) 5_554 5_554 ? O12 V3 V7 87.23(17) . 5_554 ? Mn V3 V7 63.36(4) . 5_554 ? O7 V3 V8 141.9(3) . . ? O13 V3 V8 34.5(2) . . ? O16 V3 V8 86.0(2) 5_554 . ? O19 V3 V8 89.8(2) . . ? O18 V3 V8 122.23(16) 5_554 . ? O12 V3 V8 48.72(16) . . ? Mn V3 V8 85.37(5) . . ? V7 V3 V8 116.64(7) 5_554 . ? O3 V4 O3 107.1(5) . 5_554 ? O3 V4 O19 100.1(3) . 5_554 ? O3 V4 O19 100.5(3) 5_554 5_554 ? O3 V4 O19 100.5(3) . . ? O3 V4 O19 100.1(3) 5_554 . ? O19 V4 O19 144.9(4) 5_554 . ? O3 V4 O18 162.1(3) . 5_554 ? O3 V4 O18 90.8(3) 5_554 5_554 ? O19 V4 O18 76.2(2) 5_554 5_554 ? O19 V4 O18 75.4(2) . 5_554 ? O3 V4 O18 90.8(3) . . ? O3 V4 O18 162.1(3) 5_554 . ? O19 V4 O18 75.4(2) 5_554 . ? O19 V4 O18 76.2(2) . . ? O18 V4 O18 71.3(3) 5_554 . ? O3 V4 Mn 126.5(2) . . ? O3 V4 Mn 126.5(2) 5_554 . ? O19 V4 Mn 72.44(19) 5_554 . ? O19 V4 Mn 72.44(19) . . ? O18 V4 Mn 35.66(15) 5_554 . ? O18 V4 Mn 35.66(15) . . ? O9 V5 O15 107.2(4) . . ? O9 V5 O19 99.1(3) . . ? O15 V5 O19 97.3(3) . . ? O9 V5 O11 100.9(3) . . ? O15 V5 O11 97.4(3) . . ? O19 V5 O11 150.3(3) . . ? O9 V5 O18 94.4(3) . . ? O15 V5 O18 158.4(3) . . ? O19 V5 O18 77.3(2) . . ? O11 V5 O18 79.6(2) . . ? O9 V5 O12 168.3(3) . . ? O15 V5 O12 84.4(3) . . ? O19 V5 O12 77.6(2) . . ? O11 V5 O12 78.4(2) . . ? O18 V5 O12 74.0(2) . . ? O9 V5 Mn 131.6(3) . . ? O15 V5 Mn 121.2(3) . . ? O19 V5 Mn 74.7(2) . . ? O11 V5 Mn 75.68(19) . . ? O18 V5 Mn 37.17(15) . . ? O12 V5 Mn 36.79(16) . . ? O9 V5 V8 142.7(3) . . ? O15 V5 V8 35.6(3) . . ? O19 V5 V8 90.42(19) . . ? O11 V5 V8 86.77(19) . . ? O18 V5 V8 122.89(17) . . ? O12 V5 V8 48.96(16) . . ? Mn V5 V8 85.72(6) . . ? O6 V6 O5 103.1(4) . . ? O6 V6 O4 104.9(3) . . ? O5 V6 O4 93.8(3) . . ? O6 V6 O16 100.5(3) . 5_554 ? O5 V6 O16 88.6(3) . 5_554 ? O4 V6 O16 153.1(3) . 5_554 ? O6 V6 O14 100.4(4) . 5_554 ? O5 V6 O14 154.0(3) . 5_554 ? O4 V6 O14 90.6(3) . 5_554 ? O16 V6 O14 76.4(2) 5_554 5_554 ? O6 V6 O12 174.7(3) . . ? O5 V6 O12 80.0(3) . . ? O4 V6 O12 78.9(3) . . ? O16 V6 O12 75.2(2) 5_554 . ? O14 V6 O12 75.7(2) 5_554 . ? O6 V6 Mn 139.0(3) . . ? O5 V6 Mn 117.4(2) . . ? O4 V6 Mn 79.4(2) . . ? O16 V6 Mn 75.79(17) 5_554 . ? O14 V6 Mn 38.62(17) 5_554 . ? O12 V6 Mn 37.44(15) . . ? O6 V6 V9 136.3(3) . . ? O5 V6 V9 83.0(2) . . ? O4 V6 V9 31.5(2) . . ? O16 V6 V9 123.00(19) 5_554 . ? O14 V6 V9 87.49(18) 5_554 . ? O12 V6 V9 47.84(16) . . ? Mn V6 V9 59.55(5) . . ? O6 V6 V8 134.6(3) . . ? O5 V6 V8 31.6(2) . . ? O4 V6 V8 83.1(3) . . ? O16 V6 V8 85.0(2) 5_554 . ? O14 V6 V8 124.38(18) 5_554 . ? O12 V6 V8 48.79(16) . . ? Mn V6 V8 86.21(5) . . ? V9 V6 V8 60.16(6) . . ? O6 V6 V7 88.8(3) . 5_554 ? O5 V6 V7 125.0(2) . 5_554 ? O4 V6 V7 135.1(3) . 5_554 ? O16 V6 V7 36.47(18) 5_554 5_554 ? O14 V6 V7 44.55(18) 5_554 5_554 ? O12 V6 V7 85.88(16) . 5_554 ? Mn V6 V7 63.71(4) . 5_554 ? V9 V6 V7 123.26(7) . 5_554 ? V8 V6 V7 117.00(7) . 5_554 ? O10 V7 O17 104.6(3) . . ? O10 V7 O11 102.0(3) . . ? O17 V7 O11 102.1(3) . . ? O10 V7 O16 101.4(3) . . ? O17 V7 O16 99.8(3) . . ? O11 V7 O16 142.6(3) . . ? O10 V7 O14 98.1(3) . . ? O17 V7 O14 157.4(3) . . ? O11 V7 O14 73.5(3) . . ? O16 V7 O14 74.6(3) . . ? O10 V7 O18 167.8(3) . . ? O17 V7 O18 87.6(3) . . ? O11 V7 O18 75.5(2) . . ? O16 V7 O18 75.5(2) . . ? O14 V7 O18 69.8(2) . . ? O10 V7 V3 136.1(3) . 5_554 ? O17 V7 V3 81.6(2) . 5_554 ? O11 V7 V3 119.45(19) . 5_554 ? O16 V7 V3 35.79(19) . 5_554 ? O14 V7 V3 81.57(18) . 5_554 ? O18 V7 V3 44.00(15) . 5_554 ? O10 V7 V9 88.2(2) . . ? O17 V7 V9 140.2(2) . . ? O11 V7 V9 38.1(2) . . ? O16 V7 V9 114.68(19) . . ? O14 V7 V9 40.09(18) . . ? O18 V7 V9 82.62(15) . . ? V3 V7 V9 114.94(6) 5_554 . ? O10 V7 V6 88.1(3) . 5_554 ? O17 V7 V6 138.2(3) . 5_554 ? O11 V7 V6 114.2(2) . 5_554 ? O16 V7 V6 38.41(19) . 5_554 ? O14 V7 V6 40.72(18) . 5_554 ? O18 V7 V6 82.24(16) . 5_554 ? V3 V7 V6 63.09(5) 5_554 5_554 ? V9 V7 V6 78.53(6) . 5_554 ? O1 V8 O2 104.6(4) . . ? O1 V8 O5 105.0(4) . . ? O2 V8 O5 92.8(3) . . ? O1 V8 O13 101.1(4) . . ? O2 V8 O13 153.4(3) . . ? O5 V8 O13 87.1(3) . . ? O1 V8 O15 101.4(4) . . ? O2 V8 O15 86.7(3) . . ? O5 V8 O15 152.8(3) . . ? O13 V8 O15 81.6(3) . . ? O1 V8 O12 175.0(4) . . ? O2 V8 O12 78.5(3) . . ? O5 V8 O12 78.5(3) . . ? O13 V8 O12 75.4(3) . . ? O15 V8 O12 74.7(3) . . ? O1 V8 V6 135.9(3) . . ? O2 V8 V6 82.3(3) . . ? O5 V8 V6 31.0(2) . . ? O13 V8 V6 84.1(2) . . ? O15 V8 V6 122.6(2) . . ? O12 V8 V6 47.90(16) . . ? O1 V8 V5 131.0(4) . . ? O2 V8 V5 79.9(2) . . ? O5 V8 V5 123.7(2) . . ? O13 V8 V5 78.1(2) . . ? O15 V8 V5 29.6(2) . . ? O12 V8 V5 45.19(16) . . ? V6 V8 V5 93.05(7) . . ? O1 V8 V9 135.7(3) . . ? O2 V8 V9 31.2(2) . . ? O5 V8 V9 82.4(2) . . ? O13 V8 V9 123.0(2) . . ? O15 V8 V9 83.3(2) . . ? O12 V8 V9 47.65(16) . . ? V6 V8 V9 59.94(6) . . ? V5 V8 V9 62.99(5) . . ? O1 V8 V3 130.8(3) . . ? O2 V8 V3 124.3(3) . . ? O5 V8 V3 79.5(2) . . ? O13 V8 V3 29.7(2) . . ? O15 V8 V3 78.5(2) . . ? O12 V8 V3 45.80(15) . . ? V6 V8 V3 63.14(6) . . ? V5 V8 V3 61.29(5) . . ? V9 V8 V3 93.40(6) . . ? O8 V9 O2 104.8(4) . . ? O8 V9 O4 103.4(4) . . ? O2 V9 O4 93.2(4) . . ? O8 V9 O11 102.1(3) . . ? O2 V9 O11 89.8(3) . . ? O4 V9 O11 152.6(3) . . ? O8 V9 O14 99.6(4) . . ? O2 V9 O14 153.9(3) . . ? O4 V9 O14 89.9(3) . . ? O11 V9 O14 76.1(3) . . ? O8 V9 O12 174.5(3) . . ? O2 V9 O12 80.0(3) . . ? O4 V9 O12 78.9(3) . . ? O11 V9 O12 74.8(2) . . ? O14 V9 O12 75.2(2) . . ? O8 V9 Mn 137.7(3) . . ? O2 V9 Mn 117.3(2) . . ? O4 V9 Mn 79.1(2) . . ? O11 V9 Mn 75.35(19) . . ? O14 V9 Mn 38.28(17) . . ? O12 V9 Mn 37.29(15) . . ? O8 V9 V6 134.7(3) . . ? O2 V9 V6 82.7(2) . . ? O4 V9 V6 31.4(2) . . ? O11 V9 V6 122.80(18) . . ? O14 V9 V6 86.73(18) . . ? O12 V9 V6 47.98(16) . . ? Mn V9 V6 59.26(5) . . ? O8 V9 V7 89.1(3) . . ? O2 V9 V7 126.1(3) . . ? O4 V9 V7 134.4(3) . . ? O11 V9 V7 36.38(19) . . ? O14 V9 V7 44.54(18) . . ? O12 V9 V7 85.79(15) . . ? Mn V9 V7 63.64(5) . . ? V6 V9 V7 122.90(7) . . ? O8 V9 V8 136.3(3) . . ? O2 V9 V8 31.7(2) . . ? O4 V9 V8 82.8(2) . . ? O11 V9 V8 85.72(19) . . ? O14 V9 V8 123.84(18) . . ? O12 V9 V8 48.67(15) . . ? Mn V9 V8 85.92(6) . . ? V6 V9 V8 59.90(6) . . ? V7 V9 V8 117.57(7) . . ? V4 O19 V5 109.2(3) . . ? V4 O19 V3 109.1(3) . . ? V5 O19 V3 109.5(3) . . ? Mn O18 V3 99.2(3) . 5_554 ? Mn O18 V5 97.7(3) . . ? V3 O18 V5 162.7(3) 5_554 . ? Mn O18 V4 99.8(2) . . ? V3 O18 V4 91.0(2) 5_554 . ? V5 O18 V4 89.8(2) . . ? Mn O18 V7 99.5(2) . . ? V3 O18 V7 86.6(2) 5_554 . ? V5 O18 V7 87.0(2) . . ? V4 O18 V7 160.7(3) . . ? V7 O17 Ce1 140.0(3) . . ? V3 O16 V7 108.4(3) 5_554 . ? V3 O16 V6 112.3(3) 5_554 5_554 ? V7 O16 V6 105.1(3) . 5_554 ? V5 O15 V8 114.8(4) . . ? Mn O14 V9 101.5(3) . . ? Mn O14 V6 100.2(3) . 5_554 ? V9 O14 V6 153.1(3) . 5_554 ? Mn O14 V7 103.9(3) . . ? V9 O14 V7 95.4(3) . . ? V6 O14 V7 94.7(2) 5_554 . ? V3 O13 V8 115.7(4) . . ? Mn O12 V5 97.6(3) . . ? Mn O12 V3 97.0(3) . . ? V5 O12 V3 90.9(2) . . ? Mn O12 V9 93.6(3) . . ? V5 O12 V9 91.8(2) . . ? V3 O12 V9 168.6(3) . . ? Mn O12 V6 93.1(3) . . ? V5 O12 V6 168.8(3) . . ? V3 O12 V6 91.1(2) . . ? V9 O12 V6 84.2(2) . . ? Mn O12 V8 175.7(4) . . ? V5 O12 V8 85.9(2) . . ? V3 O12 V8 85.5(2) . . ? V9 O12 V8 83.7(2) . . ? V6 O12 V8 83.3(2) . . ? V7 O11 V5 109.4(3) . . ? V7 O11 V9 105.5(3) . . ? V5 O11 V9 111.8(3) . . ? V7 O10 Ce1 154.1(4) . 12_554 ? V5 O9 Ce1 132.2(4) . . ? V3 O7 Ce1 130.4(4) . 5_554 ? V6 O5 V8 117.4(4) . . ? V6 O4 V9 117.1(4) . . ? V4 O3 Ce1 136.8(3) . . ? V9 O2 V8 117.1(4) . . ? N1 C3 N1 71.3(10) 2_565 . ? N1 C3 C5 99.4(9) 2_565 2_565 ? N1 C3 C5 49.6(10) . 2_565 ? N1 C3 C5 49.6(10) 2_565 . ? N1 C3 C5 99.4(9) . . ? C5 C3 C5 145.3(10) 2_565 . ? O20 C2 N1 144.2(5) . . ? O20 C2 N1 144.2(5) . 2_565 ? N1 C2 N1 71.6(10) . 2_565 ? O20 C2 C1 109.5(7) . 2_565 ? N1 C2 C1 41.2(13) . 2_565 ? N1 C2 C1 102.2(9) 2_565 2_565 ? O20 C2 C1 109.5(7) . . ? N1 C2 C1 102.2(9) . . ? N1 C2 C1 41.2(13) 2_565 . ? C1 C2 C1 140.9(15) 2_565 . ? C4 C1 N1 123(4) 2_565 2_565 ? C4 C1 C5 78(2) 2_565 . ? N1 C1 C5 55.8(14) 2_565 . ? C4 C1 C2 169(6) 2_565 . ? N1 C1 C2 68.1(10) 2_565 . ? C5 C1 C2 107.9(9) . . ? C1 N1 C5 80.4(19) 2_565 2_565 ? C1 N1 C2 70.8(10) 2_565 . ? C5 N1 C2 125(2) 2_565 . ? C1 N1 C3 138(3) 2_565 . ? C5 N1 C3 66.0(8) 2_565 . ? C2 N1 C3 108.5(10) . . ? C1 N1 C4 21.2(14) 2_565 . ? C5 N1 C4 65.6(11) 2_565 . ? C2 N1 C4 91.9(14) . . ? C3 N1 C4 130.7(14) . . ? C1 N1 N1 111(2) 2_565 2_565 ? C5 N1 N1 98.3(19) 2_565 2_565 ? C2 N1 N1 54.2(5) . 2_565 ? C3 N1 N1 54.3(5) . 2_565 ? C4 N1 N1 126(2) . 2_565 ? C1 C4 N1 36(3) 2_565 . ? C1 C4 C5 77.1(18) 2_565 2_565 ? N1 C4 C5 49.5(9) . 2_565 ? N1 C5 C1 43.8(14) 2_565 . ? N1 C5 C3 64.3(7) 2_565 . ? C1 C5 C3 104.5(10) . . ? N1 C5 C4 64.9(10) 2_565 2_565 ? C1 C5 C4 24.7(10) . 2_565 ? C3 C5 C4 128.5(13) . 2_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.425 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.146 data_2 _database_code_depnum_ccdc_archive 'CCDC 912015' #TrackingRef 'compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H30 La2 Mn N O49 V13' _chemical_formula_weight 1883.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 26.725(4) _cell_length_b 26.725(4) _cell_length_c 30.487(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21775(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9572 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7176 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_T_max 0.699 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 79213 _diffrn_reflns_av_R_equivalents 0.1167 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9572 _reflns_number_gt 7874 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.472 -0.017 0.081 13875.0 274.9 _platon_squeeze_details ; ; _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^)+(0.0400P)^2^+500.0000P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.01(3) _refine_ls_number_reflns 9572 _refine_ls_number_parameters 306 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 1.65274(2) 0.42729(2) -0.53191(2) 0.03056(15) Uani 1 1 d . . . Mn1 Mn 1.7500 0.57145(9) -0.6250 0.0250(5) Uani 1 2 d S . . V3 V 1.84982(7) 0.51498(7) -0.61564(6) 0.0285(4) Uani 1 1 d . . . V4 V 1.76926(7) 0.51488(7) -0.53909(6) 0.0298(4) Uani 1 1 d . . . V5 V 1.84364(8) 0.63648(7) -0.61847(7) 0.0379(5) Uani 1 1 d . . . V6 V 1.7500 0.45296(9) -0.6250 0.0269(6) Uani 1 2 d S . . V7 V 1.66705(6) 0.57260(7) -0.54661(6) 0.0289(4) Uani 1 1 d . . . V8 V 1.86549(7) 0.57968(9) -0.53148(7) 0.0425(5) Uani 1 1 d . . . V9 V 1.76432(8) 0.63611(7) -0.54309(7) 0.0378(5) Uani 1 1 d . . . O19 O 1.8001(3) 0.4748(3) -0.5844(2) 0.0305(17) Uani 1 1 d . . . O18 O 1.7166(2) 0.5215(2) -0.5939(2) 0.0234(15) Uani 1 1 d . . . O17 O 1.6433(3) 0.5204(3) -0.5262(2) 0.0353(18) Uani 1 1 d . . . O16 O 1.6328(2) 0.5742(3) -0.6020(2) 0.0300(16) Uani 1 1 d . . . O15 O 1.8214(3) 0.5253(3) -0.5092(2) 0.039(2) Uani 1 1 d . . . O14 O 1.7136(3) 0.6195(3) -0.5896(2) 0.0299(17) Uani 1 1 d . . . O13 O 1.8009(3) 0.5721(3) -0.5833(2) 0.0307(16) Uani 1 1 d . . . O12 O 1.6397(3) 0.6176(3) -0.5204(3) 0.0370(19) Uani 1 1 d . . . O11 O 1.8875(3) 0.5260(3) -0.5713(2) 0.0373(19) Uani 1 1 d . . . O10 O 1.7327(3) 0.5740(3) -0.5212(2) 0.0336(17) Uani 1 1 d . . . O9 O 1.7380(3) 0.4716(3) -0.5140(2) 0.0367(19) Uani 1 1 d . . . O8 O 1.8002(3) 0.6721(3) -0.5839(3) 0.040(2) Uani 1 1 d . . . O7 O 1.7344(3) 0.6784(3) -0.5174(3) 0.049(2) Uani 1 1 d . . . O6 O 1.7168(3) 0.4171(3) -0.5932(2) 0.0326(18) Uani 1 1 d . . . O5 O 1.8759(3) 0.4711(3) -0.6447(3) 0.0359(19) Uani 1 1 d . . . O4 O 1.8719(3) 0.6778(3) -0.6470(3) 0.050(2) Uani 1 1 d . . . O3 O 1.8187(3) 0.6241(3) -0.5101(3) 0.044(2) Uani 1 1 d . . . O2 O 1.8856(3) 0.6236(3) -0.5737(3) 0.045(2) Uani 1 1 d . . . O4W O 1.6234(4) 0.3587(3) -0.5807(3) 0.059(3) Uani 1 1 d . . . O3W O 1.5604(3) 0.4388(3) -0.5240(3) 0.047(2) Uani 1 1 d . . . O1 O 1.9090(3) 0.5796(4) -0.4963(3) 0.060(3) Uani 1 1 d . . . O2W O 1.7162(3) 0.3610(3) -0.5088(4) 0.068(3) Uani 1 1 d . . . O1W O 1.6547(4) 0.4536(3) -0.4520(3) 0.056(2) Uani 1 1 d . . . OW1 O 1.5000 0.5000 -0.4309(5) 0.064(4) Uiso 1 2 d S . . OW2 O 1.7038(5) 0.5416(5) -0.4259(4) 0.101(4) Uiso 1 1 d . . . C3 C 1.5000 0.5000 -0.3089(7) 0.085(8) Uiso 1 2 d SD . . C1 C 1.5000 0.5000 -0.3875(8) 0.081(7) Uiso 1 2 d SD . . C5 C 1.5329(6) 0.497(2) -0.3485(6) 0.14(2) Uiso 0.50 1 d PD . . C2 C 1.4480(5) 0.4875(15) -0.3237(7) 0.096(12) Uiso 0.50 1 d PD . . N1 N 1.4457(4) 0.5000(15) -0.3716(6) 0.115 Uiso 0.50 1 d PD . . C4 C 1.4010(10) 0.4976(18) -0.4016(9) 0.115 Uiso 0.50 1 d PD . . 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 0.0301(3) 0.0261(3) 0.0355(3) 0.0061(3) 0.0111(3) 0.0006(3) Mn1 0.0215(11) 0.0227(11) 0.0309(11) 0.000 0.0091(9) 0.000 V3 0.0226(9) 0.0297(10) 0.0331(10) -0.0029(8) 0.0057(8) 0.0016(8) V4 0.0278(10) 0.0318(10) 0.0299(10) 0.0004(8) 0.0056(8) 0.0013(8) V5 0.0362(11) 0.0306(10) 0.0470(12) -0.0096(9) 0.0157(10) -0.0070(9) V6 0.0256(14) 0.0235(13) 0.0315(14) 0.000 0.0087(11) 0.000 V7 0.0290(10) 0.0259(9) 0.0319(9) -0.0001(8) 0.0115(7) 0.0016(8) V8 0.0323(10) 0.0527(13) 0.0424(11) -0.0138(11) 0.0009(9) -0.0056(10) V9 0.0362(11) 0.0334(11) 0.0437(12) -0.0131(9) 0.0146(9) -0.0047(9) O19 0.027(4) 0.033(4) 0.032(4) 0.003(3) 0.007(3) -0.002(3) O18 0.025(4) 0.021(4) 0.024(3) -0.001(3) 0.009(3) -0.001(3) O17 0.035(4) 0.034(4) 0.036(4) 0.004(3) 0.010(4) -0.004(3) O16 0.023(4) 0.028(4) 0.039(4) 0.000(3) 0.006(3) 0.000(3) O15 0.031(5) 0.052(5) 0.033(4) -0.004(4) 0.001(3) 0.004(4) O14 0.026(4) 0.026(4) 0.037(4) 0.002(3) 0.010(3) -0.003(3) O13 0.025(4) 0.035(4) 0.032(4) -0.006(4) 0.008(3) -0.001(4) O12 0.032(4) 0.026(4) 0.052(5) -0.007(3) 0.010(4) 0.000(3) O11 0.030(4) 0.047(5) 0.035(4) -0.002(4) 0.004(3) 0.004(4) O10 0.033(4) 0.038(4) 0.030(4) -0.007(4) 0.011(3) -0.004(4) O9 0.043(5) 0.033(4) 0.035(4) 0.005(3) 0.011(4) 0.003(4) O8 0.037(5) 0.032(5) 0.052(5) -0.007(4) 0.011(4) -0.004(4) O7 0.045(5) 0.042(5) 0.059(6) -0.019(4) 0.010(4) -0.006(4) O6 0.031(4) 0.025(4) 0.042(4) 0.002(3) 0.007(3) -0.004(3) O5 0.038(5) 0.027(4) 0.043(4) -0.007(3) 0.008(4) 0.002(3) O4 0.046(5) 0.041(5) 0.062(6) -0.010(4) 0.029(4) -0.014(4) O3 0.043(5) 0.047(5) 0.041(5) -0.016(4) 0.012(4) -0.007(4) O2 0.038(5) 0.053(6) 0.045(5) -0.018(4) 0.007(4) -0.009(4) O4W 0.075(7) 0.047(6) 0.054(6) -0.007(5) 0.018(5) -0.014(5) O3W 0.037(5) 0.048(5) 0.055(5) 0.021(4) 0.006(4) 0.006(4) O1 0.047(6) 0.077(7) 0.056(5) -0.013(5) -0.006(4) -0.001(5) O2W 0.042(6) 0.051(6) 0.110(8) 0.045(6) 0.028(5) 0.014(5) O1W 0.089(7) 0.045(5) 0.034(4) 0.004(4) 0.014(5) 0.003(5) _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 O4W 2.488(9) . ? La1 O3W 2.498(8) . ? La1 O17 2.507(8) . ? La1 O1W 2.537(8) . ? La1 O6 2.549(7) . ? La1 O2W 2.553(9) . ? La1 O12 2.574(7) 3_674 ? La1 O9 2.624(8) . ? La1 O5 2.637(8) 5_853 ? Mn1 O13 1.863(7) . ? Mn1 O13 1.863(7) 5_853 ? Mn1 O18 1.866(7) 5_853 ? Mn1 O18 1.866(7) . ? Mn1 O14 1.939(7) . ? Mn1 O14 1.939(7) 5_853 ? Mn1 V5 3.053(2) . ? Mn1 V5 3.053(2) 5_853 ? Mn1 V9 3.061(2) . ? Mn1 V9 3.061(2) 5_853 ? Mn1 V4 3.068(2) 5_853 ? Mn1 V4 3.068(2) . ? V3 O5 1.628(7) . ? V3 O11 1.712(8) . ? V3 O16 1.922(8) 5_853 ? V3 O19 1.956(7) . ? V3 O18 2.168(7) 5_853 ? V3 O13 2.238(7) . ? V3 V7 3.120(3) 5_853 ? V4 O9 1.621(8) . ? V4 O15 1.686(8) . ? V4 O19 1.931(7) . ? V4 O10 1.937(8) . ? V4 O18 2.192(7) . ? V4 O13 2.206(8) . ? V4 V8 3.109(3) . ? V5 O4 1.596(8) . ? V5 O2 1.799(9) . ? V5 O8 1.834(8) . ? V5 O16 1.992(8) 5_853 ? V5 O14 2.043(8) 5_853 ? V5 O13 2.328(8) . ? V5 V8 3.111(3) . ? V5 V7 3.114(3) 5_853 ? V6 O6 1.626(7) . ? V6 O6 1.626(7) 5_853 ? V6 O19 1.916(7) . ? V6 O19 1.916(7) 5_853 ? V6 O18 2.247(7) . ? V6 O18 2.247(7) 5_853 ? V7 O12 1.619(7) . ? V7 O17 1.654(7) . ? V7 O10 1.917(7) . ? V7 O16 1.922(7) . ? V7 O14 2.199(7) . ? V7 O18 2.387(7) . ? V7 V9 3.106(3) . ? V7 V5 3.114(3) 5_853 ? V7 V3 3.120(3) 5_853 ? V8 O1 1.580(9) . ? V8 O2 1.822(9) . ? V8 O3 1.844(8) . ? V8 O11 1.968(8) . ? V8 O15 1.991(9) . ? V8 O13 2.348(7) . ? V8 V9 3.116(3) . ? V9 O7 1.590(8) . ? V9 O3 1.796(9) . ? V9 O8 1.843(8) . ? V9 O10 1.977(8) . ? V9 O14 2.013(8) . ? V9 O13 2.321(8) . ? O18 V3 2.168(7) 5_853 ? O16 V3 1.922(8) 5_853 ? O16 V5 1.992(8) 5_853 ? O14 V5 2.043(8) 5_853 ? O12 La1 2.574(7) 4_744 ? O5 La1 2.637(8) 5_853 ? OW1 C1 1.32(2) . ? C3 C5 1.495(10) . ? C3 C5 1.495(10) 2_865 ? C3 C2 1.499(9) . ? C3 C2 1.499(9) 2_865 ? C1 C5 1.482(10) 2_865 ? C1 C5 1.482(10) . ? C1 N1 1.531(10) 2_865 ? C1 N1 1.531(10) . ? C5 N1 0.912(17) 2_865 ? C5 C2 1.01(4) 2_865 ? C5 C5 1.77(4) 2_865 ? C2 C5 1.01(4) 2_865 ? C2 N1 1.498(9) . ? N1 C5 0.912(17) 2_865 ? N1 C4 1.507(9) . ? 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 O4W La1 O3W 80.7(3) . . ? O4W La1 O17 137.9(3) . . ? O3W La1 O17 76.8(2) . . ? O4W La1 O1W 141.8(3) . . ? O3W La1 O1W 83.9(3) . . ? O17 La1 O1W 70.1(3) . . ? O4W La1 O6 72.2(3) . . ? O3W La1 O6 138.4(3) . . ? O17 La1 O6 103.0(2) . . ? O1W La1 O6 136.1(3) . . ? O4W La1 O2W 82.1(4) . . ? O3W La1 O2W 135.6(3) . . ? O17 La1 O2W 137.5(3) . . ? O1W La1 O2W 85.1(3) . . ? O6 La1 O2W 71.5(3) . . ? O4W La1 O12 75.1(3) . 3_674 ? O3W La1 O12 70.4(2) . 3_674 ? O17 La1 O12 127.6(2) . 3_674 ? O1W La1 O12 66.8(3) . 3_674 ? O6 La1 O12 128.7(2) . 3_674 ? O2W La1 O12 65.7(3) . 3_674 ? O4W La1 O9 136.9(3) . . ? O3W La1 O9 141.4(3) . . ? O17 La1 O9 68.0(2) . . ? O1W La1 O9 69.9(3) . . ? O6 La1 O9 67.6(2) . . ? O2W La1 O9 71.3(3) . . ? O12 La1 O9 120.1(2) 3_674 . ? O4W La1 O5 74.3(3) . 5_853 ? O3W La1 O5 75.0(2) . 5_853 ? O17 La1 O5 65.8(2) . 5_853 ? O1W La1 O5 134.2(3) . 5_853 ? O6 La1 O5 67.7(2) . 5_853 ? O2W La1 O5 137.3(3) . 5_853 ? O12 La1 O5 136.7(2) 3_674 5_853 ? O9 La1 O5 103.2(2) . 5_853 ? O13 Mn1 O13 179.0(5) . 5_853 ? O13 Mn1 O18 90.2(3) . 5_853 ? O13 Mn1 O18 90.5(3) 5_853 5_853 ? O13 Mn1 O18 90.5(3) . . ? O13 Mn1 O18 90.2(3) 5_853 . ? O18 Mn1 O18 88.5(4) 5_853 . ? O13 Mn1 O14 88.9(3) . . ? O13 Mn1 O14 90.4(3) 5_853 . ? O18 Mn1 O14 175.7(3) 5_853 . ? O18 Mn1 O14 87.2(3) . . ? O13 Mn1 O14 90.4(3) . 5_853 ? O13 Mn1 O14 88.9(3) 5_853 5_853 ? O18 Mn1 O14 87.2(3) 5_853 5_853 ? O18 Mn1 O14 175.7(3) . 5_853 ? O14 Mn1 O14 97.1(4) . 5_853 ? O13 Mn1 V5 49.6(2) . . ? O13 Mn1 V5 129.7(2) 5_853 . ? O18 Mn1 V5 92.8(2) 5_853 . ? O18 Mn1 V5 140.1(2) . . ? O14 Mn1 V5 89.9(2) . . ? O14 Mn1 V5 41.2(2) 5_853 . ? O13 Mn1 V5 129.7(2) . 5_853 ? O13 Mn1 V5 49.6(2) 5_853 5_853 ? O18 Mn1 V5 140.1(2) 5_853 5_853 ? O18 Mn1 V5 92.8(2) . 5_853 ? O14 Mn1 V5 41.2(2) . 5_853 ? O14 Mn1 V5 89.9(2) 5_853 5_853 ? V5 Mn1 V5 110.61(10) . 5_853 ? O13 Mn1 V9 49.2(2) . . ? O13 Mn1 V9 130.1(2) 5_853 . ? O18 Mn1 V9 139.4(2) 5_853 . ? O18 Mn1 V9 92.8(2) . . ? O14 Mn1 V9 40.1(2) . . ? O14 Mn1 V9 91.0(2) 5_853 . ? V5 Mn1 V9 61.51(6) . . ? V5 Mn1 V9 80.46(7) 5_853 . ? O13 Mn1 V9 130.1(2) . 5_853 ? O13 Mn1 V9 49.2(2) 5_853 5_853 ? O18 Mn1 V9 92.8(2) 5_853 5_853 ? O18 Mn1 V9 139.4(2) . 5_853 ? O14 Mn1 V9 91.0(2) . 5_853 ? O14 Mn1 V9 40.1(2) 5_853 5_853 ? V5 Mn1 V9 80.46(7) . 5_853 ? V5 Mn1 V9 61.51(6) 5_853 5_853 ? V9 Mn1 V9 111.26(11) . 5_853 ? O13 Mn1 V4 135.2(2) . 5_853 ? O13 Mn1 V4 45.5(2) 5_853 5_853 ? O18 Mn1 V4 45.1(2) 5_853 5_853 ? O18 Mn1 V4 90.0(2) . 5_853 ? O14 Mn1 V4 135.8(2) . 5_853 ? O14 Mn1 V4 86.3(2) 5_853 5_853 ? V5 Mn1 V4 118.27(5) . 5_853 ? V5 Mn1 V4 95.01(5) 5_853 5_853 ? V9 Mn1 V4 174.74(9) . 5_853 ? V9 Mn1 V4 63.94(5) 5_853 5_853 ? O13 Mn1 V4 45.5(2) . . ? O13 Mn1 V4 135.2(2) 5_853 . ? O18 Mn1 V4 90.0(2) 5_853 . ? O18 Mn1 V4 45.1(2) . . ? O14 Mn1 V4 86.3(2) . . ? O14 Mn1 V4 135.8(2) 5_853 . ? V5 Mn1 V4 95.01(5) . . ? V5 Mn1 V4 118.27(5) 5_853 . ? V9 Mn1 V4 63.94(5) . . ? V9 Mn1 V4 174.74(9) 5_853 . ? V4 Mn1 V4 120.95(10) 5_853 . ? O5 V3 O11 107.7(4) . . ? O5 V3 O16 102.2(3) . 5_853 ? O11 V3 O16 97.0(4) . 5_853 ? O5 V3 O19 99.2(4) . . ? O11 V3 O19 96.2(3) . . ? O16 V3 O19 150.0(3) 5_853 . ? O5 V3 O18 95.6(3) . 5_853 ? O11 V3 O18 156.5(3) . 5_853 ? O16 V3 O18 80.8(3) 5_853 5_853 ? O19 V3 O18 76.4(3) . 5_853 ? O5 V3 O13 169.0(4) . . ? O11 V3 O13 83.0(3) . . ? O16 V3 O13 78.8(3) 5_853 . ? O19 V3 O13 76.2(3) . . ? O18 V3 O13 73.6(2) 5_853 . ? O5 V3 Mn1 132.4(3) . . ? O11 V3 Mn1 119.9(3) . . ? O16 V3 Mn1 76.0(2) 5_853 . ? O19 V3 Mn1 74.1(2) . . ? O18 V3 Mn1 36.74(17) 5_853 . ? O13 V3 Mn1 36.92(18) . . ? O5 V3 V7 87.2(3) . 5_853 ? O11 V3 V7 132.6(3) . 5_853 ? O16 V3 V7 35.7(2) 5_853 5_853 ? O19 V3 V7 126.2(2) . 5_853 ? O18 V3 V7 49.79(18) 5_853 5_853 ? O13 V3 V7 87.5(2) . 5_853 ? Mn1 V3 V7 63.46(5) . 5_853 ? O9 V4 O15 106.8(4) . . ? O9 V4 O19 99.3(3) . . ? O15 V4 O19 97.2(4) . . ? O9 V4 O10 100.9(3) . . ? O15 V4 O10 97.5(4) . . ? O19 V4 O10 150.3(3) . . ? O9 V4 O18 94.9(3) . . ? O15 V4 O18 158.2(3) . . ? O19 V4 O18 76.9(3) . . ? O10 V4 O18 79.9(3) . . ? O9 V4 O13 168.9(4) . . ? O15 V4 O13 84.2(3) . . ? O19 V4 O13 77.5(3) . . ? O10 V4 O13 78.4(3) . . ? O18 V4 O13 74.0(3) . . ? O9 V4 Mn1 132.0(3) . . ? O15 V4 Mn1 121.2(3) . . ? O19 V4 Mn1 74.6(2) . . ? O10 V4 Mn1 75.7(2) . . ? O18 V4 Mn1 37.04(17) . . ? O13 V4 Mn1 37.01(18) . . ? O9 V4 V8 142.2(3) . . ? O15 V4 V8 35.4(3) . . ? O19 V4 V8 90.5(2) . . ? O10 V4 V8 86.7(2) . . ? O18 V4 V8 122.91(19) . . ? O13 V4 V8 48.89(19) . . ? Mn1 V4 V8 85.87(7) . . ? O4 V5 O2 104.5(5) . . ? O4 V5 O8 104.7(4) . . ? O2 V5 O8 93.3(4) . . ? O4 V5 O16 100.5(4) . 5_853 ? O2 V5 O16 89.2(3) . 5_853 ? O8 V5 O16 153.2(3) . 5_853 ? O4 V5 O14 99.7(4) . 5_853 ? O2 V5 O14 153.8(4) . 5_853 ? O8 V5 O14 90.1(3) . 5_853 ? O16 V5 O14 76.6(3) 5_853 5_853 ? O4 V5 O13 174.4(4) . . ? O2 V5 O13 79.3(3) . . ? O8 V5 O13 79.0(3) . . ? O16 V5 O13 75.2(3) 5_853 . ? O14 V5 O13 75.9(3) 5_853 . ? O4 V5 Mn1 138.3(4) . . ? O2 V5 Mn1 116.8(3) . . ? O8 V5 Mn1 79.3(3) . . ? O16 V5 Mn1 75.8(2) 5_853 . ? O14 V5 Mn1 38.7(2) 5_853 . ? O13 V5 Mn1 37.54(18) . . ? O4 V5 V8 135.5(4) . . ? O2 V5 V8 31.0(3) . . ? O8 V5 V8 83.2(3) . . ? O16 V5 V8 85.3(2) 5_853 . ? O14 V5 V8 124.4(2) 5_853 . ? O13 V5 V8 48.57(18) . . ? Mn1 V5 V8 86.08(6) . . ? O4 V5 V7 88.3(3) . 5_853 ? O2 V5 V7 125.6(3) . 5_853 ? O8 V5 V7 134.8(3) . 5_853 ? O16 V5 V7 36.5(2) 5_853 5_853 ? O14 V5 V7 44.8(2) 5_853 5_853 ? O13 V5 V7 86.14(18) . 5_853 ? Mn1 V5 V7 63.81(5) . 5_853 ? V8 V5 V7 117.29(8) . 5_853 ? O6 V6 O6 107.8(5) . 5_853 ? O6 V6 O19 100.2(3) . . ? O6 V6 O19 100.5(3) 5_853 . ? O6 V6 O19 100.5(3) . 5_853 ? O6 V6 O19 100.2(3) 5_853 5_853 ? O19 V6 O19 144.5(5) . 5_853 ? O6 V6 O18 90.7(3) . . ? O6 V6 O18 161.5(3) 5_853 . ? O19 V6 O18 75.9(3) . . ? O19 V6 O18 75.3(3) 5_853 . ? O6 V6 O18 161.5(3) . 5_853 ? O6 V6 O18 90.7(3) 5_853 5_853 ? O19 V6 O18 75.3(3) . 5_853 ? O19 V6 O18 75.9(3) 5_853 5_853 ? O18 V6 O18 70.9(3) . 5_853 ? O6 V6 Mn1 126.1(3) . . ? O6 V6 Mn1 126.1(3) 5_853 . ? O19 V6 Mn1 72.2(2) . . ? O19 V6 Mn1 72.2(2) 5_853 . ? O18 V6 Mn1 35.43(17) . . ? O18 V6 Mn1 35.43(17) 5_853 . ? O12 V7 O17 105.5(4) . . ? O12 V7 O10 101.5(4) . . ? O17 V7 O10 102.5(4) . . ? O12 V7 O16 101.7(4) . . ? O17 V7 O16 99.6(4) . . ? O10 V7 O16 142.1(3) . . ? O12 V7 O14 97.3(3) . . ? O17 V7 O14 157.2(3) . . ? O10 V7 O14 73.3(3) . . ? O16 V7 O14 74.4(3) . . ? O12 V7 O18 166.9(3) . . ? O17 V7 O18 87.5(3) . . ? O10 V7 O18 75.4(3) . . ? O16 V7 O18 75.3(3) . . ? O14 V7 O18 69.7(2) . . ? O12 V7 V9 87.4(3) . . ? O17 V7 V9 140.3(3) . . ? O10 V7 V9 37.8(2) . . ? O16 V7 V9 114.6(2) . . ? O14 V7 V9 40.2(2) . . ? O18 V7 V9 82.52(17) . . ? O12 V7 V5 87.8(3) . 5_853 ? O17 V7 V5 137.7(3) . 5_853 ? O10 V7 V5 114.1(2) . 5_853 ? O16 V7 V5 38.1(2) . 5_853 ? O14 V7 V5 40.9(2) . 5_853 ? O18 V7 V5 82.10(17) . 5_853 ? V9 V7 V5 78.81(7) . 5_853 ? O12 V7 V3 136.5(3) . 5_853 ? O17 V7 V3 81.4(3) . 5_853 ? O10 V7 V3 119.2(2) . 5_853 ? O16 V7 V3 35.8(2) . 5_853 ? O14 V7 V3 81.5(2) . 5_853 ? O18 V7 V3 43.91(17) . 5_853 ? V9 V7 V3 114.86(7) . 5_853 ? V5 V7 V3 62.90(6) 5_853 5_853 ? O1 V8 O2 105.3(5) . . ? O1 V8 O3 105.1(4) . . ? O2 V8 O3 92.0(4) . . ? O1 V8 O11 101.4(4) . . ? O2 V8 O11 86.9(3) . . ? O3 V8 O11 152.9(4) . . ? O1 V8 O15 101.7(5) . . ? O2 V8 O15 152.2(4) . . ? O3 V8 O15 87.0(3) . . ? O11 V8 O15 81.7(3) . . ? O1 V8 O13 174.9(5) . . ? O2 V8 O13 78.3(3) . . ? O3 V8 O13 78.2(3) . . ? O11 V8 O13 75.0(3) . . ? O15 V8 O13 74.3(3) . . ? O1 V8 V4 131.1(4) . . ? O2 V8 V4 123.3(3) . . ? O3 V8 V4 79.9(3) . . ? O11 V8 V4 78.2(2) . . ? O15 V8 V4 29.4(2) . . ? O13 V8 V4 45.05(19) . . ? O1 V8 V5 135.8(4) . . ? O2 V8 V5 30.6(3) . . ? O3 V8 V5 81.9(3) . . ? O11 V8 V5 83.5(2) . . ? O15 V8 V5 122.4(2) . . ? O13 V8 V5 48.02(19) . . ? V4 V8 V5 93.03(7) . . ? O1 V8 V9 135.7(4) . . ? O2 V8 V9 82.2(3) . . ? O3 V8 V9 30.7(3) . . ? O11 V8 V9 122.8(2) . . ? O15 V8 V9 83.0(2) . . ? O13 V8 V9 47.77(19) . . ? V4 V8 V9 62.83(6) . . ? V5 V8 V9 60.28(7) . . ? O7 V9 O3 104.9(4) . . ? O7 V9 O8 102.9(4) . . ? O3 V9 O8 92.9(4) . . ? O7 V9 O10 102.4(4) . . ? O3 V9 O10 90.4(4) . . ? O8 V9 O10 152.7(3) . . ? O7 V9 O14 99.5(4) . . ? O3 V9 O14 154.2(3) . . ? O8 V9 O14 89.4(3) . . ? O10 V9 O14 76.4(3) . . ? O7 V9 O13 174.7(4) . . ? O3 V9 O13 79.8(3) . . ? O8 V9 O13 79.0(3) . . ? O10 V9 O13 74.9(3) . . ? O14 V9 O13 75.5(3) . . ? O7 V9 Mn1 137.8(3) . . ? O3 V9 Mn1 117.2(3) . . ? O8 V9 Mn1 79.0(3) . . ? O10 V9 Mn1 75.4(2) . . ? O14 V9 Mn1 38.4(2) . . ? O13 V9 Mn1 37.41(18) . . ? O7 V9 V7 89.1(3) . . ? O3 V9 V7 126.8(3) . . ? O8 V9 V7 134.3(3) . . ? O10 V9 V7 36.4(2) . . ? O14 V9 V7 44.9(2) . . ? O13 V9 V7 86.06(19) . . ? Mn1 V9 V7 63.81(5) . . ? O7 V9 V8 136.4(3) . . ? O3 V9 V8 31.6(2) . . ? O8 V9 V8 83.0(3) . . ? O10 V9 V8 85.8(2) . . ? O14 V9 V8 123.9(2) . . ? O13 V9 V8 48.51(18) . . ? Mn1 V9 V8 85.87(6) . . ? V7 V9 V8 117.75(8) . . ? V6 O19 V4 109.4(4) . . ? V6 O19 V3 109.1(3) . . ? V4 O19 V3 109.5(4) . . ? Mn1 O18 V3 99.2(3) . 5_853 ? Mn1 O18 V4 97.9(3) . . ? V3 O18 V4 162.3(3) 5_853 . ? Mn1 O18 V6 100.3(3) . . ? V3 O18 V6 91.2(3) 5_853 . ? V4 O18 V6 90.1(3) . . ? Mn1 O18 V7 99.3(3) . . ? V3 O18 V7 86.3(2) 5_853 . ? V4 O18 V7 86.6(2) . . ? V6 O18 V7 160.3(3) . . ? V7 O17 La1 140.6(4) . . ? V3 O16 V7 108.5(4) 5_853 . ? V3 O16 V5 112.4(3) 5_853 5_853 ? V7 O16 V5 105.4(3) . 5_853 ? V4 O15 V8 115.2(4) . . ? Mn1 O14 V9 101.5(3) . . ? Mn1 O14 V5 100.1(3) . 5_853 ? V9 O14 V5 153.6(4) . 5_853 ? Mn1 O14 V7 103.8(3) . . ? V9 O14 V7 94.9(3) . . ? V5 O14 V7 94.4(3) 5_853 . ? Mn1 O13 V4 97.5(3) . . ? Mn1 O13 V3 96.9(3) . . ? V4 O13 V3 91.2(3) . . ? Mn1 O13 V9 93.4(3) . . ? V4 O13 V9 91.5(2) . . ? V3 O13 V9 168.9(4) . . ? Mn1 O13 V5 92.9(3) . . ? V4 O13 V5 169.1(4) . . ? V3 O13 V5 90.8(2) . . ? V9 O13 V5 84.5(3) . . ? Mn1 O13 V8 175.5(5) . . ? V4 O13 V8 86.1(3) . . ? V3 O13 V8 85.8(3) . . ? V9 O13 V8 83.7(2) . . ? V5 O13 V8 83.4(2) . . ? V7 O12 La1 153.0(4) . 4_744 ? V3 O11 V8 115.9(4) . . ? V7 O10 V4 109.4(4) . . ? V7 O10 V9 105.8(4) . . ? V4 O10 V9 112.0(3) . . ? V4 O9 La1 132.2(4) . . ? V5 O8 V9 116.5(4) . . ? V6 O6 La1 137.8(4) . . ? V3 O5 La1 131.1(4) . 5_853 ? V9 O3 V8 117.8(4) . . ? V5 O2 V8 118.4(5) . . ? C5 C3 C5 72.5(18) . 2_865 ? C5 C3 C2 106.8(8) . . ? C5 C3 C2 39.4(14) 2_865 . ? C5 C3 C2 39.4(14) . 2_865 ? C5 C3 C2 106.8(8) 2_865 2_865 ? C2 C3 C2 145.1(12) . 2_865 ? OW1 C1 C5 143.4(9) . 2_865 ? OW1 C1 C5 143.4(9) . . ? C5 C1 C5 73.2(18) 2_865 . ? OW1 C1 N1 108.5(10) . 2_865 ? C5 C1 N1 107.9(17) 2_865 2_865 ? C5 C1 N1 35.2(7) . 2_865 ? OW1 C1 N1 108.5(10) . . ? C5 C1 N1 35.2(7) 2_865 . ? C5 C1 N1 107.9(17) . . ? N1 C1 N1 143.0(19) 2_865 . ? N1 C5 C2 102(3) 2_865 2_865 ? N1 C5 C1 75.4(10) 2_865 . ? C2 C5 C1 151(6) 2_865 . ? N1 C5 C3 170(7) 2_865 . ? C2 C5 C3 70.5(10) 2_865 . ? C1 C5 C3 107.2(17) . . ? N1 C5 C5 128(2) 2_865 2_865 ? C2 C5 C5 117(4) 2_865 2_865 ? C1 C5 C5 53.4(9) . 2_865 ? C3 C5 C5 53.8(9) . 2_865 ? C5 C2 N1 36.5(12) 2_865 . ? C5 C2 C3 70.1(11) 2_865 . ? N1 C2 C3 106.3(8) . . ? C5 N1 C2 41(2) 2_865 . ? C5 N1 C4 166(3) 2_865 . ? C2 N1 C4 128.0(12) . . ? C5 N1 C1 69.4(9) 2_865 . ? C2 N1 C1 105.7(16) . . ? C4 N1 C1 123.9(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.598 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.147 data_3 _database_code_depnum_ccdc_archive 'CCDC 912016' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H19 La2 Mn O47 V13' _chemical_formula_weight 1766.13 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 0.0106 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4m2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 39.9678(16) _cell_length_b 39.9678(16) _cell_length_c 26.249(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 41931(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18811 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13328 _exptl_absorpt_coefficient_mu 2.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.676 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 64899 _diffrn_reflns_av_R_equivalents 0.1155 _diffrn_reflns_av_sigmaI/netI 0.1287 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18811 _reflns_number_gt 12546 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.012 -0.006 -0.001 28789.2 1312.6 _platon_squeeze_details ; ; _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^)+(0.0300P)^2^+850.0000P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_number_reflns 18811 _refine_ls_number_parameters 588 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 0.16681(2) 0.23280(2) 0.15383(4) 0.0391(2) Uani 1 1 d . . . La2 La 0.09494(2) 0.23888(2) -0.07169(4) 0.0402(2) Uani 1 1 d . . . Mn1 Mn 0.0000 0.23555(7) 0.07303(12) 0.0325(7) Uani 1 2 d S . . V4 V 0.22930(6) 0.27070(6) 0.2500 0.0339(8) Uani 1 2 d S . . V5 V 0.03977(6) 0.18295(6) 0.01381(9) 0.0345(6) Uani 1 1 d . . . V6 V 0.0000 0.23778(9) -0.04540(13) 0.0353(8) Uani 1 2 d S . . V7 V 0.03939(6) 0.29050(7) 0.01845(10) 0.0395(6) Uani 1 1 d . . . V8 V 0.03868(6) 0.18501(7) 0.13554(10) 0.0421(7) Uani 1 1 d . . . V9 V 0.08086(5) 0.23550(6) 0.07376(10) 0.0370(6) Uani 1 1 d . . . V10 V 0.0000 0.13079(9) 0.07598(17) 0.0467(10) Uani 1 2 d S . . V11 V 0.33846(7) 0.26131(8) 0.13329(11) 0.0549(8) Uani 1 1 d . . . Mn2 Mn 0.28492(5) 0.21508(5) 0.2500 0.0347(7) Uani 1 2 d S . . V13 V 0.31869(6) 0.18799(7) 0.15597(12) 0.0503(7) Uani 1 1 d . . . V14 V 0.24316(6) 0.17292(6) 0.16783(10) 0.0389(6) Uani 1 1 d . . . V15 V 0.0000 0.34019(11) 0.08570(18) 0.0587(12) Uani 1 2 d S . . V16 V 0.21208(6) 0.19568(6) 0.27021(10) 0.0396(6) Uani 1 1 d . . . V17 V 0.26303(6) 0.24645(6) 0.14953(10) 0.0361(6) Uani 1 1 d . . . V18 V 0.35921(6) 0.22876(8) 0.23510(11) 0.0501(8) Uani 1 1 d . . . V19 V 0.03897(7) 0.28357(8) 0.13980(11) 0.0498(7) Uani 1 1 d . . . O42 O 0.0000 0.2823(4) -0.0233(6) 0.041(4) Uani 1 2 d S . . O41 O 0.2171(2) 0.2395(2) 0.3001(4) 0.031(2) Uani 1 1 d . . . O40 O 0.1027(2) 0.2358(2) 0.0209(3) 0.036(2) Uani 1 1 d . . . O39 O 0.0000 0.1918(3) -0.0268(5) 0.033(3) Uani 1 2 d S . . O38 O 0.2443(2) 0.2215(2) 0.2169(4) 0.033(2) Uani 1 1 d . . . O37 O 0.0654(2) 0.1903(2) 0.0743(4) 0.036(2) Uani 1 1 d . . . O36 O 0.0332(2) 0.2363(2) 0.0225(3) 0.027(2) Uani 1 1 d . . . O35 O 0.0000 0.2791(4) 0.1754(6) 0.043(4) Uani 1 2 d S . . O34 O 0.0000 0.1899(3) 0.0734(5) 0.036(3) Uani 1 2 d S . . O33 O 0.2503(3) 0.1370(3) 0.1395(4) 0.049(3) Uani 1 1 d . . . O32 O 0.0325(2) 0.1415(2) 0.0222(4) 0.042(3) Uani 1 1 d . . . O31 O 0.0000 0.2820(4) 0.0758(6) 0.043(4) Uani 1 2 d S . . O30 O 0.0000 0.1886(4) 0.1713(5) 0.041(4) Uani 1 2 d S . . O29 O 0.2299(3) 0.1585(2) 0.2330(4) 0.042(2) Uani 1 1 d . . . O28 O 0.2081(2) 0.1862(2) 0.1438(4) 0.042(3) Uani 1 1 d . . . O27 O 0.0000 0.0911(4) 0.0747(7) 0.063(4) Uani 1 2 d S . . O26 O 0.0668(2) 0.2891(3) -0.0254(4) 0.044(3) Uani 1 1 d . . . O25 O 0.1949(2) 0.2709(2) 0.2179(4) 0.042(3) Uani 1 1 d . . . O24 O 0.2271(2) 0.2513(2) 0.1244(4) 0.042(3) Uani 1 1 d . . . O23 O 0.0657(2) 0.2811(2) 0.0772(4) 0.042(2) Uani 1 1 d . . . O8W O 0.1686(3) 0.2231(3) 0.0603(4) 0.054(3) Uani 1 1 d . . . O22 O 0.1084(2) 0.2355(3) 0.1182(4) 0.046(3) Uani 1 1 d . . . O21 O 0.0330(2) 0.1421(3) 0.1212(4) 0.045(3) Uani 1 1 d . . . O20 O 0.2009(3) 0.1750(2) 0.3226(4) 0.049(3) Uani 1 1 d . . . O19 O 0.0672(2) 0.1863(3) -0.0294(4) 0.045(3) Uani 1 1 d . . . O18 O -0.0323(2) 0.2386(3) -0.0819(4) 0.047(3) Uani 1 1 d . . . O17 O 0.2735(2) 0.2009(2) 0.1323(4) 0.041(2) Uani 1 1 d . . . O16 O 0.3544(2) 0.1898(3) 0.1990(4) 0.048(3) Uani 1 1 d . . . O15 O 0.2884(2) 0.1740(2) 0.2139(3) 0.034(2) Uani 1 1 d . . . O14 O 0.2923(3) 0.2649(3) 0.1119(4) 0.053(3) Uani 1 1 d . . . O13 O 0.0680(3) 0.2823(3) 0.1813(5) 0.057(3) Uani 1 1 d . . . O12 O 0.0355(2) 0.2351(3) 0.1211(4) 0.038(2) Uani 1 1 d . . . O11 O 0.0329(3) 0.3321(3) 0.0307(5) 0.055(3) Uani 1 1 d . . . O10 O 0.3075(2) 0.2363(3) 0.1986(4) 0.039(2) Uani 1 1 d . . . O9 O 0.1782(2) 0.2034(2) 0.2393(4) 0.041(3) Uani 1 1 d . . . O8 O 0.0666(2) 0.1856(3) 0.1770(4) 0.055(3) Uani 1 1 d . . . O7 O 0.0331(3) 0.3277(3) 0.1290(5) 0.057(3) Uani 1 1 d . . . O7W O 0.1410(3) 0.1985(3) -0.0627(5) 0.055(3) Uani 1 1 d . . . O6 O 0.3925(3) 0.2227(3) 0.2653(5) 0.069(4) Uani 1 1 d . . . O5 O 0.3372(2) 0.2175(3) 0.1139(5) 0.054(3) Uani 1 1 d . . . O4 O 0.3713(3) 0.2519(3) 0.1806(4) 0.057(3) Uani 1 1 d . . . O3 O 0.3225(3) 0.1530(3) 0.1279(5) 0.063(4) Uani 1 1 d . . . O2 O 0.3578(3) 0.2798(4) 0.0887(4) 0.075(4) Uani 1 1 d . . . O6W O 0.1241(3) 0.2511(4) 0.2190(5) 0.081(5) Uani 1 1 d . . . O5W O 0.0806(3) 0.1997(4) -0.1415(5) 0.075(4) Uani 1 1 d . . . O4W O 0.1611(3) 0.2918(3) 0.1245(6) 0.072(4) Uani 1 1 d . . . O3W O 0.0776(3) 0.2836(3) -0.1344(5) 0.072(4) Uani 1 1 d . . . O1 O 0.0000 0.3789(4) 0.0881(9) 0.080(6) Uani 1 2 d S . . O2W O 0.1365(3) 0.1770(3) 0.1561(5) 0.060(3) Uani 1 1 d . . . O1W O 0.1388(3) 0.2809(3) -0.0448(5) 0.075(4) Uani 1 1 d . . . OW2 O 0.2210(3) 0.2210(3) 0.0000 0.072(5) Uani 1 2 d S . . OW1 O 0.1441(4) 0.1441(4) 0.0000 0.080(5) Uani 1 2 d SU . . 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 0.0298(5) 0.0479(5) 0.0397(5) -0.0087(4) -0.0069(4) 0.0008(4) La2 0.0270(4) 0.0573(6) 0.0364(5) 0.0060(5) 0.0043(4) -0.0013(4) Mn1 0.0253(15) 0.0408(17) 0.0312(16) -0.0021(15) 0.000 0.000 V4 0.0338(12) 0.0338(12) 0.0342(19) -0.0058(11) -0.0058(11) -0.0005(15) V5 0.0245(13) 0.0455(15) 0.0334(14) 0.0015(12) 0.0017(10) 0.0019(11) V6 0.0213(18) 0.052(2) 0.0328(19) 0.0058(17) 0.000 0.000 V7 0.0299(14) 0.0444(16) 0.0441(15) 0.0020(12) 0.0006(12) -0.0041(12) V8 0.0277(14) 0.0588(18) 0.0398(15) 0.0120(13) -0.0023(11) 0.0008(12) V9 0.0235(12) 0.0558(16) 0.0317(13) -0.0015(13) -0.0013(11) -0.0038(11) V10 0.036(2) 0.046(2) 0.058(3) 0.015(2) 0.000 0.000 V11 0.0401(16) 0.084(2) 0.0406(16) -0.0088(15) 0.0033(13) -0.0075(15) Mn2 0.0342(10) 0.0342(10) 0.0356(17) -0.0067(10) -0.0067(10) 0.0044(13) V13 0.0366(15) 0.0644(19) 0.0500(17) -0.0238(15) -0.0066(14) 0.0093(13) V14 0.0407(15) 0.0359(14) 0.0399(15) -0.0129(12) -0.0111(12) 0.0048(11) V15 0.051(3) 0.054(3) 0.071(3) -0.018(2) 0.000 0.000 V16 0.0437(16) 0.0355(15) 0.0395(14) -0.0075(12) -0.0045(12) -0.0040(12) V17 0.0344(13) 0.0432(14) 0.0307(13) -0.0072(12) -0.0063(11) 0.0001(11) V18 0.0324(15) 0.073(2) 0.0453(17) -0.0201(15) -0.0092(13) 0.0075(14) V19 0.0365(15) 0.069(2) 0.0435(17) -0.0177(14) -0.0042(13) -0.0004(14) O42 0.023(7) 0.054(9) 0.046(9) 0.018(7) 0.000 0.000 O41 0.032(5) 0.030(5) 0.030(5) -0.010(4) -0.005(4) 0.003(4) O40 0.028(5) 0.051(6) 0.029(5) 0.008(5) -0.008(4) -0.004(4) O39 0.026(7) 0.041(8) 0.032(8) -0.007(6) 0.000 0.000 O38 0.035(5) 0.026(5) 0.037(6) -0.019(4) -0.002(4) 0.002(4) O37 0.025(5) 0.045(6) 0.039(6) 0.014(5) 0.001(5) 0.004(4) O36 0.017(5) 0.035(5) 0.030(5) 0.000(4) -0.001(4) 0.001(4) O35 0.027(8) 0.058(10) 0.042(9) -0.004(7) 0.000 0.000 O34 0.029(7) 0.048(8) 0.030(7) 0.003(7) 0.000 0.000 O33 0.048(6) 0.047(6) 0.052(7) -0.020(5) -0.011(5) 0.004(5) O32 0.032(6) 0.042(6) 0.053(7) 0.004(5) -0.006(5) 0.002(5) O31 0.032(8) 0.057(9) 0.039(8) 0.009(8) 0.000 0.000 O30 0.037(8) 0.052(9) 0.036(8) 0.007(7) 0.000 0.000 O29 0.053(6) 0.024(5) 0.048(6) -0.009(5) -0.001(5) -0.006(4) O28 0.040(6) 0.038(6) 0.048(7) -0.017(5) -0.014(5) -0.002(4) O27 0.077(12) 0.043(9) 0.070(12) 0.002(9) 0.000 0.000 O26 0.041(6) 0.045(6) 0.047(7) 0.000(5) 0.006(5) -0.014(5) O25 0.031(6) 0.044(6) 0.050(7) -0.010(5) -0.016(5) 0.009(5) O24 0.043(6) 0.045(6) 0.037(6) -0.010(5) -0.013(5) 0.006(5) O23 0.035(5) 0.045(6) 0.046(6) -0.011(5) -0.006(5) -0.005(4) O8W 0.037(6) 0.099(9) 0.025(6) 0.000(6) -0.007(5) -0.009(6) O22 0.039(6) 0.068(7) 0.032(6) 0.000(5) -0.012(5) 0.005(5) O21 0.034(6) 0.055(7) 0.047(7) 0.012(5) 0.006(5) -0.007(5) O20 0.070(8) 0.032(6) 0.044(7) -0.007(5) -0.002(6) -0.007(5) O19 0.032(6) 0.053(7) 0.049(7) -0.002(5) 0.010(5) -0.006(5) O18 0.037(6) 0.067(7) 0.038(7) -0.006(6) -0.006(5) 0.001(5) O17 0.040(6) 0.049(6) 0.034(5) -0.006(5) -0.011(5) 0.008(5) O16 0.038(6) 0.058(7) 0.047(7) -0.017(5) -0.007(5) 0.003(5) O15 0.045(6) 0.031(5) 0.027(5) -0.009(4) -0.007(4) 0.013(4) O14 0.067(8) 0.055(7) 0.036(6) -0.005(5) -0.002(6) -0.019(6) O13 0.039(7) 0.073(8) 0.058(8) -0.015(6) 0.000(5) 0.005(6) O12 0.017(5) 0.065(7) 0.031(6) 0.008(5) -0.003(4) -0.002(5) O11 0.044(7) 0.061(8) 0.059(8) -0.007(6) -0.005(6) -0.012(6) O10 0.027(5) 0.050(6) 0.041(6) -0.002(5) -0.010(4) 0.003(5) O9 0.035(6) 0.051(6) 0.038(6) -0.011(5) -0.001(5) -0.001(5) O8 0.035(6) 0.095(9) 0.035(6) 0.014(6) -0.009(5) 0.005(6) O7 0.038(6) 0.066(8) 0.066(8) -0.017(6) 0.002(6) -0.006(5) O7W 0.046(6) 0.051(7) 0.068(8) 0.022(6) 0.011(6) 0.012(5) O6 0.045(7) 0.099(10) 0.061(8) -0.035(7) -0.012(6) 0.016(7) O5 0.029(6) 0.075(8) 0.059(8) -0.025(6) 0.002(5) -0.005(5) O4 0.037(6) 0.092(9) 0.042(7) -0.014(6) -0.007(5) -0.003(6) O3 0.036(6) 0.083(9) 0.071(9) -0.039(7) -0.004(6) 0.010(6) O2 0.072(9) 0.119(11) 0.034(7) 0.001(7) 0.023(6) -0.027(8) O6W 0.044(7) 0.155(14) 0.045(8) -0.036(8) -0.012(6) 0.027(8) O5W 0.051(8) 0.114(11) 0.062(9) -0.017(8) 0.008(6) -0.006(7) O4W 0.063(8) 0.054(8) 0.100(11) 0.011(7) -0.017(7) -0.004(6) O3W 0.061(8) 0.091(10) 0.064(9) 0.035(7) 0.018(7) 0.030(7) O1 0.067(12) 0.046(10) 0.13(2) 0.001(11) 0.000 0.000 O2W 0.041(6) 0.054(7) 0.085(9) -0.011(7) -0.004(7) -0.009(5) O1W 0.075(9) 0.093(10) 0.056(8) 0.001(7) 0.006(7) -0.046(7) OW2 0.072(8) 0.072(8) 0.070(13) -0.017(7) 0.017(7) -0.008(10) OW1 0.084(6) 0.084(6) 0.074(9) 0.006(5) -0.006(5) 0.026(7) _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 O8W 2.486(10) . ? La1 O4W 2.493(12) . ? La1 O28 2.502(9) . ? La1 O6W 2.525(12) . ? La1 O22 2.518(9) . ? La1 O2W 2.540(10) . ? La1 O25 2.531(9) . ? La1 O9 2.575(10) . ? La1 O24 2.638(10) . ? La2 O40 2.454(9) . ? La2 O7W 2.459(10) . ? La2 O5W 2.479(13) . ? La2 O33 2.491(10) 7 ? La2 O18 2.520(10) 6 ? La2 O1W 2.530(11) . ? La2 O3W 2.527(11) . ? La2 O26 2.603(11) . ? La2 O19 2.622(10) . ? Mn1 O34 1.825(13) . ? Mn1 O31 1.860(14) . ? Mn1 O36 1.878(9) . ? Mn1 O36 1.878(9) 6 ? Mn1 O12 1.899(9) . ? Mn1 O12 1.899(9) 6 ? Mn1 V19 3.030(4) . ? Mn1 V19 3.030(4) 6 ? Mn1 V8 3.027(4) 6 ? Mn1 V8 3.027(4) . ? Mn1 V7 3.059(4) . ? Mn1 V7 3.059(4) 6 ? V4 O25 1.612(9) . ? V4 O25 1.612(9) 16 ? V4 O41 1.877(9) 16 ? V4 O41 1.877(9) . ? V4 O38 2.233(8) 16 ? V4 O38 2.233(8) . ? V4 V17 3.116(3) 16 ? V4 V17 3.116(3) . ? V4 V16 3.122(3) 16 ? V4 V16 3.122(3) . ? V4 Mn2 3.144(5) . ? V5 O19 1.583(10) . ? V5 O32 1.697(10) . ? V5 O37 1.914(10) . ? V5 O39 1.947(8) . ? V5 O36 2.159(9) . ? V5 O34 2.247(10) . ? V5 V10 3.088(4) . ? V5 V9 3.096(3) . ? V5 V6 3.122(4) . ? V6 O18 1.606(10) . ? V6 O18 1.606(10) 6 ? V6 O42 1.872(15) . ? V6 O39 1.900(14) . ? V6 O36 2.223(9) . ? V6 O36 2.223(9) 6 ? V6 V7 3.119(4) . ? V6 V7 3.119(4) 6 ? V6 V5 3.122(4) 6 ? V7 O26 1.590(10) . ? V7 O11 1.715(12) . ? V7 O23 1.905(11) . ? V7 O42 1.946(9) . ? V7 O36 2.185(9) . ? V7 O31 2.204(11) . ? V7 V15 3.088(4) . ? V7 V9 3.112(4) . ? V8 O8 1.561(10) . ? V8 O21 1.769(11) . ? V8 O30 1.815(8) . ? V8 O37 1.942(10) . ? V8 O12 2.043(11) . ? V8 O34 2.256(11) . ? V8 V10 3.087(5) . ? V8 V9 3.089(4) . ? V8 V8 3.092(5) 6 ? V9 O22 1.603(10) . ? V9 O40 1.638(10) . ? V9 O37 1.908(9) . ? V9 O23 1.923(10) . ? V9 O12 2.198(9) . ? V9 O36 2.331(9) . ? V9 V19 3.082(4) . ? V10 O27 1.585(15) . ? V10 O21 1.831(11) . ? V10 O21 1.831(11) 6 ? V10 O32 1.965(11) . ? V10 O32 1.965(11) 6 ? V10 O34 2.363(13) . ? V10 V8 3.087(5) 6 ? V10 V5 3.088(4) 6 ? V11 O2 1.585(11) . ? V11 O5 1.824(11) . ? V11 O4 1.846(11) . ? V11 O14 1.935(11) . ? V11 O20 1.976(11) 16 ? V11 O10 2.339(10) . ? V11 V16 3.067(4) 16 ? V11 V18 3.086(4) . ? V11 V13 3.093(5) . ? V11 V17 3.102(4) . ? Mn2 O10 1.831(10) . ? Mn2 O10 1.831(10) 16 ? Mn2 O38 1.858(9) . ? Mn2 O38 1.858(9) 16 ? Mn2 O15 1.900(9) . ? Mn2 O15 1.900(9) 16 ? Mn2 V13 3.014(3) 16 ? Mn2 V13 3.014(3) . ? Mn2 V18 3.044(3) 16 ? Mn2 V18 3.044(3) . ? Mn2 V17 3.048(3) . ? Mn2 V17 3.048(3) 16 ? V13 O3 1.589(11) . ? V13 O5 1.778(12) . ? V13 O16 1.822(10) . ? V13 O17 1.978(10) . ? V13 O15 2.023(10) . ? V13 O10 2.275(10) . ? V13 V14 3.094(4) . ? V13 V18 3.097(4) . ? V14 O28 1.627(9) . ? V14 O33 1.641(10) . ? V14 O29 1.882(10) . ? V14 O17 1.896(10) . ? V14 O15 2.174(9) . ? V14 O38 2.329(8) . ? V14 V18 3.066(4) 16 ? V14 V17 3.082(4) . ? V14 V16 3.097(4) . ? V15 O1 1.548(17) . ? V15 O7 1.815(12) 6 ? V15 O7 1.815(12) . ? V15 O11 1.980(12) 6 ? V15 O11 1.980(12) . ? V15 O31 2.338(15) . ? V15 V7 3.088(4) 6 ? V15 V19 3.093(5) 6 ? V15 V19 3.093(5) . ? V16 O9 1.606(10) . ? V16 O20 1.665(11) . ? V16 O29 1.916(10) . ? V16 O41 1.928(9) . ? V16 O38 2.165(10) . ? V16 O10 2.225(10) 16 ? V16 V11 3.067(4) 16 ? V17 O24 1.591(9) . ? V17 O14 1.699(11) . ? V17 O17 1.921(10) . ? V17 O41 1.970(9) 16 ? V17 O38 2.163(10) . ? V17 O10 2.231(9) . ? V18 O6 1.568(11) . ? V18 O4 1.772(12) . ? V18 O16 1.832(10) . ? V18 O29 1.981(11) 16 ? V18 O15 2.006(10) 16 ? V18 O10 2.299(9) . ? V18 V14 3.066(4) 16 ? V19 O13 1.590(12) . ? V19 O7 1.801(12) . ? V19 O35 1.825(8) . ? V19 O23 1.962(11) . ? V19 O12 2.002(11) . ? V19 O31 2.292(12) . ? V19 V19 3.115(5) 6 ? O42 V7 1.946(9) 6 ? O41 V17 1.970(9) 16 ? O39 V5 1.947(8) 6 ? O35 V19 1.825(8) 6 ? O34 V8 2.256(11) 6 ? O34 V5 2.247(10) 6 ? O33 La2 2.491(10) 7 ? O31 V7 2.204(11) 6 ? O31 V19 2.292(12) 6 ? O30 V8 1.815(8) 6 ? O29 V18 1.981(11) 16 ? O20 V11 1.976(11) 16 ? O18 La2 2.520(10) 6 ? O15 V18 2.006(10) 16 ? O10 V16 2.225(10) 16 ? 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 O8W La1 O4W 81.0(4) . . ? O8W La1 O28 76.2(3) . . ? O4W La1 O28 137.1(4) . . ? O8W La1 O6W 137.2(4) . . ? O4W La1 O6W 82.8(5) . . ? O28 La1 O6W 137.1(4) . . ? O8W La1 O22 70.5(3) . . ? O4W La1 O22 76.0(4) . . ? O28 La1 O22 127.1(3) . . ? O6W La1 O22 67.2(3) . . ? O8W La1 O2W 84.2(4) . . ? O4W La1 O2W 142.6(4) . . ? O28 La1 O2W 70.3(3) . . ? O6W La1 O2W 85.2(4) . . ? O22 La1 O2W 66.7(4) . . ? O8W La1 O25 137.5(4) . . ? O4W La1 O25 71.2(4) . . ? O28 La1 O25 103.0(3) . . ? O6W La1 O25 71.1(4) . . ? O22 La1 O25 129.2(3) . . ? O2W La1 O25 136.4(4) . . ? O8W La1 O9 141.7(4) . . ? O4W La1 O9 135.9(4) . . ? O28 La1 O9 68.6(3) . . ? O6W La1 O9 70.2(4) . . ? O22 La1 O9 120.6(3) . . ? O2W La1 O9 70.3(4) . . ? O25 La1 O9 67.5(3) . . ? O8W La1 O24 74.2(3) . . ? O4W La1 O24 74.2(4) . . ? O28 La1 O24 64.9(3) . . ? O6W La1 O24 137.3(4) . . ? O22 La1 O24 136.6(3) . . ? O2W La1 O24 133.6(3) . . ? O25 La1 O24 67.7(3) . . ? O9 La1 O24 102.8(3) . . ? O40 La2 O7W 77.2(4) . . ? O40 La2 O5W 136.9(4) . . ? O7W La2 O5W 80.1(4) . . ? O40 La2 O33 129.2(3) . 7 ? O7W La2 O33 71.6(3) . 7 ? O5W La2 O33 75.1(4) . 7 ? O40 La2 O18 103.3(3) . 6 ? O7W La2 O18 138.6(4) . 6 ? O5W La2 O18 71.9(4) . 6 ? O33 La2 O18 126.6(4) 7 6 ? O40 La2 O1W 70.7(4) . . ? O7W La2 O1W 83.7(4) . . ? O5W La2 O1W 141.8(4) . . ? O33 La2 O1W 67.0(4) 7 . ? O18 La2 O1W 136.3(4) 6 . ? O40 La2 O3W 135.6(4) . . ? O7W La2 O3W 137.1(4) . . ? O5W La2 O3W 84.4(5) . . ? O33 La2 O3W 65.8(4) 7 . ? O18 La2 O3W 70.2(4) 6 . ? O1W La2 O3W 84.4(5) . . ? O40 La2 O26 68.3(3) . . ? O7W La2 O26 141.7(4) . . ? O5W La2 O26 137.2(4) . . ? O33 La2 O26 119.0(3) 7 . ? O18 La2 O26 67.9(3) 6 . ? O1W La2 O26 69.9(4) . . ? O3W La2 O26 68.9(4) . . ? O40 La2 O19 66.0(3) . . ? O7W La2 O19 75.5(3) . . ? O5W La2 O19 73.1(4) . . ? O33 La2 O19 137.3(3) 7 . ? O18 La2 O19 67.7(3) 6 . ? O1W La2 O19 135.0(4) . . ? O3W La2 O19 136.6(4) . . ? O26 La2 O19 103.7(3) . . ? O34 Mn1 O31 177.5(7) . . ? O34 Mn1 O36 91.1(4) . . ? O31 Mn1 O36 90.7(4) . . ? O34 Mn1 O36 91.1(4) . 6 ? O31 Mn1 O36 90.7(4) . 6 ? O36 Mn1 O36 90.1(5) . 6 ? O34 Mn1 O12 89.3(4) . . ? O31 Mn1 O12 89.0(5) . . ? O36 Mn1 O12 86.6(4) . . ? O36 Mn1 O12 176.7(4) 6 . ? O34 Mn1 O12 89.3(4) . 6 ? O31 Mn1 O12 89.0(5) . 6 ? O36 Mn1 O12 176.7(4) . 6 ? O36 Mn1 O12 86.6(4) 6 6 ? O12 Mn1 O12 96.7(6) . 6 ? O34 Mn1 V19 129.1(4) . . ? O31 Mn1 V19 49.0(4) . . ? O36 Mn1 V19 92.0(3) . . ? O36 Mn1 V19 139.7(3) 6 . ? O12 Mn1 V19 40.3(3) . . ? O12 Mn1 V19 90.3(3) 6 . ? O34 Mn1 V19 129.1(4) . 6 ? O31 Mn1 V19 49.0(4) . 6 ? O36 Mn1 V19 139.7(3) . 6 ? O36 Mn1 V19 92.0(3) 6 6 ? O12 Mn1 V19 90.3(3) . 6 ? O12 Mn1 V19 40.3(3) 6 6 ? V19 Mn1 V19 61.85(12) . 6 ? O34 Mn1 V8 47.9(3) . 6 ? O31 Mn1 V8 130.2(4) . 6 ? O36 Mn1 V8 139.0(3) . 6 ? O36 Mn1 V8 91.8(3) 6 6 ? O12 Mn1 V8 90.9(3) . 6 ? O12 Mn1 V8 41.6(3) 6 6 ? V19 Mn1 V8 111.81(13) . 6 ? V19 Mn1 V8 81.18(10) 6 6 ? O34 Mn1 V8 47.9(3) . . ? O31 Mn1 V8 130.2(4) . . ? O36 Mn1 V8 91.8(3) . . ? O36 Mn1 V8 139.0(3) 6 . ? O12 Mn1 V8 41.6(3) . . ? O12 Mn1 V8 90.9(3) 6 . ? V19 Mn1 V8 81.18(10) . . ? V19 Mn1 V8 111.81(13) 6 . ? V8 Mn1 V8 61.42(11) 6 . ? O34 Mn1 V7 136.1(3) . . ? O31 Mn1 V7 45.6(3) . . ? O36 Mn1 V7 45.1(3) . . ? O36 Mn1 V7 91.3(3) 6 . ? O12 Mn1 V7 86.2(3) . . ? O12 Mn1 V7 134.6(3) 6 . ? V19 Mn1 V7 63.35(9) . . ? V19 Mn1 V7 94.62(11) 6 . ? V8 Mn1 V7 174.86(14) 6 . ? V8 Mn1 V7 118.05(7) . . ? O34 Mn1 V7 136.1(3) . 6 ? O31 Mn1 V7 45.6(3) . 6 ? O36 Mn1 V7 91.3(3) . 6 ? O36 Mn1 V7 45.1(3) 6 6 ? O12 Mn1 V7 134.6(3) . 6 ? O12 Mn1 V7 86.2(3) 6 6 ? V19 Mn1 V7 94.62(11) . 6 ? V19 Mn1 V7 63.35(9) 6 6 ? V8 Mn1 V7 118.05(7) 6 6 ? V8 Mn1 V7 174.86(14) . 6 ? V7 Mn1 V7 61.96(11) . 6 ? O25 V4 O25 105.4(7) . 16 ? O25 V4 O41 101.5(5) . 16 ? O25 V4 O41 98.5(5) 16 16 ? O25 V4 O41 98.5(5) . . ? O25 V4 O41 101.5(5) 16 . ? O41 V4 O41 146.7(6) 16 . ? O25 V4 O38 162.9(4) . 16 ? O25 V4 O38 91.7(4) 16 16 ? O41 V4 O38 75.9(4) 16 16 ? O41 V4 O38 77.1(4) . 16 ? O25 V4 O38 91.7(4) . . ? O25 V4 O38 162.9(4) 16 . ? O41 V4 O38 77.1(4) 16 . ? O41 V4 O38 75.9(4) . . ? O38 V4 O38 71.2(5) 16 . ? O25 V4 V17 135.2(4) . 16 ? O25 V4 V17 85.9(4) 16 16 ? O41 V4 V17 119.9(3) 16 16 ? O41 V4 V17 36.9(3) . 16 ? O38 V4 V17 44.0(3) 16 16 ? O38 V4 V17 82.2(3) . 16 ? O25 V4 V17 85.9(4) . . ? O25 V4 V17 135.2(4) 16 . ? O41 V4 V17 36.9(3) 16 . ? O41 V4 V17 119.9(3) . . ? O38 V4 V17 82.2(3) 16 . ? O38 V4 V17 44.0(3) . . ? V17 V4 V17 116.56(14) 16 . ? O25 V4 V16 136.8(4) . 16 ? O25 V4 V16 84.5(4) 16 16 ? O41 V4 V16 35.4(3) 16 16 ? O41 V4 V16 121.0(3) . 16 ? O38 V4 V16 43.9(3) 16 16 ? O38 V4 V16 82.5(3) . 16 ? V17 V4 V16 86.59(9) 16 16 ? V17 V4 V16 60.62(7) . 16 ? O25 V4 V16 84.5(4) . . ? O25 V4 V16 136.8(4) 16 . ? O41 V4 V16 121.0(3) 16 . ? O41 V4 V16 35.4(3) . . ? O38 V4 V16 82.5(3) 16 . ? O38 V4 V16 43.9(3) . . ? V17 V4 V16 60.62(7) 16 . ? V17 V4 V16 86.59(9) . . ? V16 V4 V16 116.91(14) 16 . ? O25 V4 Mn2 127.3(4) . . ? O25 V4 Mn2 127.3(4) 16 . ? O41 V4 Mn2 73.3(3) 16 . ? O41 V4 Mn2 73.3(3) . . ? O38 V4 Mn2 35.6(2) 16 . ? O38 V4 Mn2 35.6(2) . . ? V17 V4 Mn2 58.28(7) 16 . ? V17 V4 Mn2 58.28(7) . . ? V16 V4 Mn2 58.45(7) 16 . ? V16 V4 Mn2 58.45(7) . . ? O19 V5 O32 107.1(5) . . ? O19 V5 O37 102.2(5) . . ? O32 V5 O37 97.7(4) . . ? O19 V5 O39 99.0(5) . . ? O32 V5 O39 96.3(5) . . ? O37 V5 O39 149.8(5) . . ? O19 V5 O36 94.3(5) . . ? O32 V5 O36 158.4(4) . . ? O37 V5 O36 79.9(4) . . ? O39 V5 O36 77.2(4) . . ? O19 V5 O34 168.0(5) . . ? O32 V5 O34 84.8(5) . . ? O37 V5 O34 77.4(4) . . ? O39 V5 O34 77.4(4) . . ? O36 V5 O34 73.7(4) . . ? O19 V5 Mn1 131.7(4) . . ? O32 V5 Mn1 121.1(4) . . ? O37 V5 Mn1 75.6(3) . . ? O39 V5 Mn1 74.3(4) . . ? O36 V5 Mn1 37.4(2) . . ? O34 V5 Mn1 36.3(3) . . ? O19 V5 V10 142.4(4) . . ? O32 V5 V10 35.3(4) . . ? O37 V5 V10 86.6(3) . . ? O39 V5 V10 89.6(4) . . ? O36 V5 V10 123.3(3) . . ? O34 V5 V10 49.6(3) . . ? Mn1 V5 V10 85.87(10) . . ? O19 V5 V9 86.5(4) . . ? O32 V5 V9 133.4(4) . . ? O37 V5 V9 35.8(3) . . ? O39 V5 V9 126.0(4) . . ? O36 V5 V9 48.8(2) . . ? O34 V5 V9 86.4(3) . . ? Mn1 V5 V9 63.33(7) . . ? V10 V5 V9 117.55(12) . . ? O19 V5 V6 86.3(4) . . ? O32 V5 V6 131.6(3) . . ? O37 V5 V6 125.3(3) . . ? O39 V5 V6 35.3(4) . . ? O36 V5 V6 45.4(2) . . ? O34 V5 V6 84.3(3) . . ? Mn1 V5 V6 60.40(10) . . ? V10 V5 V6 118.36(9) . . ? V9 V5 V6 92.69(10) . . ? O18 V6 O18 106.8(8) . 6 ? O18 V6 O42 99.5(5) . . ? O18 V6 O42 99.5(5) 6 . ? O18 V6 O39 99.9(5) . . ? O18 V6 O39 99.9(5) 6 . ? O42 V6 O39 147.1(6) . . ? O18 V6 O36 163.3(5) . . ? O18 V6 O36 89.9(4) 6 . ? O42 V6 O36 77.2(4) . . ? O39 V6 O36 76.6(4) . . ? O18 V6 O36 89.9(4) . 6 ? O18 V6 O36 163.3(5) 6 6 ? O42 V6 O36 77.2(4) . 6 ? O39 V6 O36 76.6(4) . 6 ? O36 V6 O36 73.4(4) . 6 ? O18 V6 Mn1 126.6(4) . . ? O18 V6 Mn1 126.6(4) 6 . ? O42 V6 Mn1 73.6(4) . . ? O39 V6 Mn1 73.5(4) . . ? O36 V6 Mn1 36.7(2) . . ? O36 V6 Mn1 36.7(2) 6 . ? O18 V6 V7 135.4(4) . . ? O18 V6 V7 84.3(4) 6 . ? O42 V6 V7 36.0(2) . . ? O39 V6 V7 121.0(3) . . ? O36 V6 V7 44.5(2) . . ? O36 V6 V7 83.6(3) 6 . ? Mn1 V6 V7 58.81(9) . . ? O18 V6 V7 84.3(4) . 6 ? O18 V6 V7 135.4(4) 6 6 ? O42 V6 V7 36.0(2) . 6 ? O39 V6 V7 121.0(3) . 6 ? O36 V6 V7 83.6(3) . 6 ? O36 V6 V7 44.5(2) 6 6 ? Mn1 V6 V7 58.81(9) . 6 ? V7 V6 V7 60.63(12) . 6 ? O18 V6 V5 84.4(4) . 6 ? O18 V6 V5 136.0(4) 6 6 ? O42 V6 V5 120.9(4) . 6 ? O39 V6 V5 36.3(2) . 6 ? O36 V6 V5 83.5(2) . 6 ? O36 V6 V5 43.7(2) 6 6 ? Mn1 V6 V5 58.81(9) . 6 ? V7 V6 V5 117.63(13) . 6 ? V7 V6 V5 87.12(9) 6 6 ? O18 V6 V5 136.0(4) . . ? O18 V6 V5 84.4(4) 6 . ? O42 V6 V5 120.9(4) . . ? O39 V6 V5 36.3(2) . . ? O36 V6 V5 43.7(2) . . ? O36 V6 V5 83.5(2) 6 . ? Mn1 V6 V5 58.81(9) . . ? V7 V6 V5 87.12(9) . . ? V7 V6 V5 117.63(13) 6 . ? V5 V6 V5 61.22(11) 6 . ? O26 V7 O11 105.9(5) . . ? O26 V7 O23 101.4(5) . . ? O11 V7 O23 97.1(5) . . ? O26 V7 O42 98.3(5) . . ? O11 V7 O42 98.4(6) . . ? O23 V7 O42 150.4(5) . . ? O26 V7 O36 94.5(4) . . ? O11 V7 O36 159.6(5) . . ? O23 V7 O36 80.0(4) . . ? O42 V7 O36 76.7(5) . . ? O26 V7 O31 168.9(5) . . ? O11 V7 O31 85.0(5) . . ? O23 V7 O31 79.1(4) . . ? O42 V7 O31 77.4(5) . . ? O36 V7 O31 74.6(4) . . ? O26 V7 Mn1 132.0(4) . . ? O11 V7 Mn1 122.1(4) . . ? O23 V7 Mn1 76.3(3) . . ? O42 V7 Mn1 74.2(4) . . ? O36 V7 Mn1 37.5(2) . . ? O31 V7 Mn1 37.1(4) . . ? O26 V7 V15 141.9(4) . . ? O11 V7 V15 36.1(4) . . ? O23 V7 V15 86.9(3) . . ? O42 V7 V15 91.0(4) . . ? O36 V7 V15 123.6(3) . . ? O31 V7 V15 49.0(4) . . ? Mn1 V7 V15 86.09(11) . . ? O26 V7 V9 86.9(4) . . ? O11 V7 V9 132.7(4) . . ? O23 V7 V9 35.8(3) . . ? O42 V7 V9 125.1(4) . . ? O36 V7 V9 48.4(2) . . ? O31 V7 V9 87.3(3) . . ? Mn1 V7 V9 63.16(7) . . ? V15 V7 V9 117.32(13) . . ? O26 V7 V6 86.3(4) . . ? O11 V7 V6 132.9(4) . . ? O23 V7 V6 125.5(3) . . ? O42 V7 V6 34.5(4) . . ? O36 V7 V6 45.5(2) . . ? O31 V7 V6 84.4(4) . . ? Mn1 V7 V6 60.44(10) . . ? V15 V7 V6 118.97(9) . . ? V9 V7 V6 92.42(10) . . ? O8 V8 O21 104.8(6) . . ? O8 V8 O30 104.4(6) . . ? O21 V8 O30 94.4(6) . . ? O8 V8 O37 100.4(5) . . ? O21 V8 O37 90.0(4) . . ? O30 V8 O37 152.7(5) . . ? O8 V8 O12 99.2(5) . . ? O21 V8 O12 154.5(5) . . ? O30 V8 O12 88.0(5) . . ? O37 V8 O12 76.9(4) . . ? O8 V8 O34 173.8(6) . . ? O21 V8 O34 80.9(5) . . ? O30 V8 O34 77.5(5) . . ? O37 V8 O34 76.7(4) . . ? O12 V8 O34 74.9(4) . . ? O8 V8 Mn1 137.3(5) . . ? O21 V8 Mn1 117.7(4) . . ? O30 V8 Mn1 78.0(4) . . ? O37 V8 Mn1 76.1(3) . . ? O12 V8 Mn1 38.1(3) . . ? O34 V8 Mn1 36.9(3) . . ? O8 V8 V10 136.2(5) . . ? O21 V8 V10 31.6(3) . . ? O30 V8 V10 83.8(4) . . ? O37 V8 V10 86.2(3) . . ? O12 V8 V10 124.3(3) . . ? O34 V8 V10 49.5(3) . . ? Mn1 V8 V10 86.46(10) . . ? O8 V8 V9 88.0(4) . . ? O21 V8 V9 126.2(3) . . ? O30 V8 V9 133.2(5) . . ? O37 V8 V9 36.3(3) . . ? O12 V8 V9 45.3(3) . . ? O34 V8 V9 86.4(3) . . ? Mn1 V8 V9 63.78(7) . . ? V10 V8 V9 117.78(12) . . ? O8 V8 V8 135.8(4) . 6 ? O21 V8 V8 82.6(3) . 6 ? O30 V8 V8 31.6(4) . 6 ? O37 V8 V8 123.4(3) . 6 ? O12 V8 V8 86.4(2) . 6 ? O34 V8 V8 46.7(3) . 6 ? Mn1 V8 V8 59.29(6) . 6 ? V10 V8 V8 59.95(6) . 6 ? V9 V8 V8 123.07(6) . 6 ? O22 V9 O40 104.5(5) . . ? O22 V9 O37 102.5(5) . . ? O40 V9 O37 100.7(5) . . ? O22 V9 O23 100.5(5) . . ? O40 V9 O23 101.6(5) . . ? O37 V9 O23 142.6(4) . . ? O22 V9 O12 98.9(5) . . ? O40 V9 O12 156.6(4) . . ? O37 V9 O12 73.9(4) . . ? O23 V9 O12 73.7(4) . . ? O22 V9 O36 168.6(5) . . ? O40 V9 O36 86.9(4) . . ? O37 V9 O36 75.7(3) . . ? O23 V9 O36 76.0(4) . . ? O12 V9 O36 69.7(3) . . ? O22 V9 V19 87.9(4) . . ? O40 V9 V19 139.5(4) . . ? O37 V9 V19 114.2(3) . . ? O23 V9 V19 37.9(3) . . ? O12 V9 V19 40.4(3) . . ? O36 V9 V19 82.7(2) . . ? O22 V9 V8 89.6(4) . . ? O40 V9 V8 137.7(4) . . ? O37 V9 V8 37.0(3) . . ? O23 V9 V8 115.0(3) . . ? O12 V9 V8 41.3(3) . . ? O36 V9 V8 82.3(2) . . ? V19 V9 V8 79.37(10) . . ? O22 V9 V5 137.2(4) . . ? O40 V9 V5 81.8(3) . . ? O37 V9 V5 36.0(3) . . ? O23 V9 V5 120.0(3) . . ? O12 V9 V5 81.1(3) . . ? O36 V9 V5 44.1(2) . . ? V19 V9 V5 114.88(10) . . ? V8 V9 V5 62.23(8) . . ? O22 V9 V7 134.8(4) . . ? O40 V9 V7 83.3(3) . . ? O37 V9 V7 120.0(3) . . ? O23 V9 V7 35.4(3) . . ? O12 V9 V7 80.2(3) . . ? O36 V9 V7 44.5(2) . . ? V19 V9 V7 62.15(9) . . ? V8 V9 V7 114.56(10) . . ? V5 V9 V7 87.69(9) . . ? O27 V10 O21 105.2(6) . . ? O27 V10 O21 105.2(6) . 6 ? O21 V10 O21 92.1(7) . 6 ? O27 V10 O32 101.7(6) . . ? O21 V10 O32 86.3(4) . . ? O21 V10 O32 152.6(5) 6 . ? O27 V10 O32 101.7(6) . 6 ? O21 V10 O32 152.6(5) . 6 ? O21 V10 O32 86.3(4) 6 6 ? O32 V10 O32 82.8(6) . 6 ? O27 V10 O34 177.1(8) . . ? O21 V10 O34 76.8(4) . . ? O21 V10 O34 76.8(4) 6 . ? O32 V10 O34 76.2(4) . . ? O32 V10 O34 76.2(4) 6 . ? O27 V10 V8 135.4(5) . . ? O21 V10 V8 30.4(3) . . ? O21 V10 V8 81.9(4) 6 . ? O32 V10 V8 83.1(3) . . ? O32 V10 V8 122.8(3) 6 . ? O34 V10 V8 46.6(3) . . ? O27 V10 V8 135.4(5) . 6 ? O21 V10 V8 81.9(4) . 6 ? O21 V10 V8 30.4(3) 6 6 ? O32 V10 V8 122.8(3) . 6 ? O32 V10 V8 83.1(3) 6 6 ? O34 V10 V8 46.6(3) . 6 ? V8 V10 V8 60.10(12) . 6 ? O27 V10 V5 131.6(5) . . ? O21 V10 V5 78.7(3) . . ? O21 V10 V5 123.1(4) 6 . ? O32 V10 V5 29.9(3) . . ? O32 V10 V5 79.3(3) 6 . ? O34 V10 V5 46.4(3) . . ? V8 V10 V5 62.35(8) . . ? V8 V10 V5 92.95(12) 6 . ? O27 V10 V5 131.6(5) . 6 ? O21 V10 V5 123.1(4) . 6 ? O21 V10 V5 78.7(3) 6 6 ? O32 V10 V5 79.3(3) . 6 ? O32 V10 V5 29.9(3) 6 6 ? O34 V10 V5 46.4(3) . 6 ? V8 V10 V5 92.95(12) . 6 ? V8 V10 V5 62.35(8) 6 6 ? V5 V10 V5 61.96(11) . 6 ? O2 V11 O5 104.7(6) . . ? O2 V11 O4 104.1(6) . . ? O5 V11 O4 90.8(5) . . ? O2 V11 O14 102.6(6) . . ? O5 V11 O14 87.9(5) . . ? O4 V11 O14 152.8(5) . . ? O2 V11 O20 102.1(6) . 16 ? O5 V11 O20 152.7(5) . 16 ? O4 V11 O20 87.4(5) . 16 ? O14 V11 O20 81.6(4) . 16 ? O2 V11 O10 176.8(6) . . ? O5 V11 O10 77.2(5) . . ? O4 V11 O10 78.3(4) . . ? O14 V11 O10 74.9(4) . . ? O20 V11 O10 75.7(4) 16 . ? O2 V11 V16 131.7(5) . 16 ? O5 V11 V16 123.4(4) . 16 ? O4 V11 V16 80.3(4) . 16 ? O14 V11 V16 77.8(3) . 16 ? O20 V11 V16 29.6(3) 16 16 ? O10 V11 V16 46.2(3) . 16 ? O2 V11 V18 134.8(5) . . ? O5 V11 V18 81.1(4) . . ? O4 V11 V18 30.8(4) . . ? O14 V11 V18 122.6(3) . . ? O20 V11 V18 83.5(3) 16 . ? O10 V11 V18 47.7(2) . . ? V16 V11 V18 63.30(9) 16 . ? O2 V11 V13 135.1(5) . . ? O5 V11 V13 30.4(4) . . ? O4 V11 V13 82.0(4) . . ? O14 V11 V13 83.3(3) . . ? O20 V11 V13 122.8(3) 16 . ? O10 V11 V13 47.0(3) . . ? V16 V11 V13 93.21(11) 16 . ? V18 V11 V13 60.17(10) . . ? O2 V11 V17 131.7(5) . . ? O5 V11 V17 80.0(3) . . ? O4 V11 V17 124.1(4) . . ? O14 V11 V17 29.2(3) . . ? O20 V11 V17 78.6(3) 16 . ? O10 V11 V17 45.8(2) . . ? V16 V11 V17 61.36(8) 16 . ? V18 V11 V17 93.53(11) . . ? V13 V11 V17 62.86(9) . . ? O10 Mn2 O10 177.6(7) . 16 ? O10 Mn2 O38 91.2(4) . . ? O10 Mn2 O38 90.5(4) 16 . ? O10 Mn2 O38 90.5(4) . 16 ? O10 Mn2 O38 91.2(4) 16 16 ? O38 Mn2 O38 88.8(5) . 16 ? O10 Mn2 O15 89.8(4) . . ? O10 Mn2 O15 88.6(4) 16 . ? O38 Mn2 O15 87.1(4) . . ? O38 Mn2 O15 175.8(4) 16 . ? O10 Mn2 O15 88.6(4) . 16 ? O10 Mn2 O15 89.8(4) 16 16 ? O38 Mn2 O15 175.8(4) . 16 ? O38 Mn2 O15 87.1(4) 16 16 ? O15 Mn2 O15 97.1(6) . 16 ? O10 Mn2 V13 129.3(3) . 16 ? O10 Mn2 V13 48.8(3) 16 16 ? O38 Mn2 V13 139.3(3) . 16 ? O38 Mn2 V13 93.3(3) 16 16 ? O15 Mn2 V13 89.8(3) . 16 ? O15 Mn2 V13 41.3(3) 16 16 ? O10 Mn2 V13 48.8(3) . . ? O10 Mn2 V13 129.3(3) 16 . ? O38 Mn2 V13 93.3(3) . . ? O38 Mn2 V13 139.3(3) 16 . ? O15 Mn2 V13 41.3(3) . . ? O15 Mn2 V13 89.8(3) 16 . ? V13 Mn2 V13 110.41(15) 16 . ? O10 Mn2 V18 129.4(3) . 16 ? O10 Mn2 V18 48.9(3) 16 16 ? O38 Mn2 V18 92.2(3) . 16 ? O38 Mn2 V18 140.0(3) 16 16 ? O15 Mn2 V18 40.1(3) . 16 ? O15 Mn2 V18 91.2(3) 16 16 ? V13 Mn2 V18 61.48(8) 16 16 ? V13 Mn2 V18 80.52(10) . 16 ? O10 Mn2 V18 48.9(3) . . ? O10 Mn2 V18 129.4(3) 16 . ? O38 Mn2 V18 140.0(3) . . ? O38 Mn2 V18 92.2(3) 16 . ? O15 Mn2 V18 91.2(3) . . ? O15 Mn2 V18 40.1(3) 16 . ? V13 Mn2 V18 80.52(10) 16 . ? V13 Mn2 V18 61.48(8) . . ? V18 Mn2 V18 111.52(15) 16 . ? O10 Mn2 V17 46.6(3) . . ? O10 Mn2 V17 135.1(3) 16 . ? O38 Mn2 V17 44.6(3) . . ? O38 Mn2 V17 90.4(3) 16 . ? O15 Mn2 V17 86.8(3) . . ? O15 Mn2 V17 135.2(3) 16 . ? V13 Mn2 V17 174.65(12) 16 . ? V13 Mn2 V17 64.40(7) . . ? V18 Mn2 V17 117.43(7) 16 . ? V18 Mn2 V17 95.45(7) . . ? O10 Mn2 V17 135.1(3) . 16 ? O10 Mn2 V17 46.6(3) 16 16 ? O38 Mn2 V17 90.4(3) . 16 ? O38 Mn2 V17 44.6(3) 16 16 ? O15 Mn2 V17 135.2(3) . 16 ? O15 Mn2 V17 86.8(3) 16 16 ? V13 Mn2 V17 64.40(7) 16 16 ? V13 Mn2 V17 174.65(12) . 16 ? V18 Mn2 V17 95.45(7) 16 16 ? V18 Mn2 V17 117.43(7) . 16 ? V17 Mn2 V17 120.83(13) . 16 ? O3 V13 O5 104.9(6) . . ? O3 V13 O16 104.3(5) . . ? O5 V13 O16 91.9(5) . . ? O3 V13 O17 100.0(5) . . ? O5 V13 O17 90.6(5) . . ? O16 V13 O17 154.1(5) . . ? O3 V13 O15 99.4(6) . . ? O5 V13 O15 154.1(4) . . ? O16 V13 O15 90.9(5) . . ? O17 V13 O15 76.2(4) . . ? O3 V13 O10 173.8(5) . . ? O5 V13 O10 79.9(4) . . ? O16 V13 O10 79.4(4) . . ? O17 V13 O10 75.7(4) . . ? O15 V13 O10 75.3(4) . . ? O3 V13 Mn2 137.7(5) . . ? O5 V13 Mn2 117.2(4) . . ? O16 V13 Mn2 80.1(3) . . ? O17 V13 Mn2 75.8(3) . . ? O15 V13 Mn2 38.3(3) . . ? O10 V13 Mn2 37.3(3) . . ? O3 V13 V11 136.1(5) . . ? O5 V13 V11 31.2(3) . . ? O16 V13 V11 83.1(4) . . ? O17 V13 V11 85.7(3) . . ? O15 V13 V11 124.0(3) . . ? O10 V13 V11 48.8(3) . . ? Mn2 V13 V11 86.08(9) . . ? O3 V13 V14 88.3(4) . . ? O5 V13 V14 126.7(4) . . ? O16 V13 V14 135.3(4) . . ? O17 V13 V14 36.1(3) . . ? O15 V13 V14 44.4(3) . . ? O10 V13 V14 85.6(2) . . ? Mn2 V13 V14 63.30(7) . . ? V11 V13 V14 116.94(11) . . ? O3 V13 V18 136.3(4) . . ? O5 V13 V18 81.4(4) . . ? O16 V13 V18 32.1(3) . . ? O17 V13 V18 123.4(3) . . ? O15 V13 V18 87.4(3) . . ? O10 V13 V18 47.7(2) . . ? Mn2 V13 V18 59.74(8) . . ? V11 V13 V18 59.80(9) . . ? V14 V13 V18 123.03(11) . . ? O28 V14 O33 105.0(5) . . ? O28 V14 O29 102.2(5) . . ? O33 V14 O29 101.1(5) . . ? O28 V14 O17 99.7(5) . . ? O33 V14 O17 100.5(5) . . ? O29 V14 O17 143.9(4) . . ? O28 V14 O15 157.7(4) . . ? O33 V14 O15 97.2(4) . . ? O29 V14 O15 74.5(4) . . ? O17 V14 O15 74.3(4) . . ? O28 V14 O38 87.7(4) . . ? O33 V14 O38 167.3(4) . . ? O29 V14 O38 76.0(4) . . ? O17 V14 O38 76.5(4) . . ? O15 V14 O38 70.1(3) . . ? O28 V14 V18 140.8(4) . 16 ? O33 V14 V18 87.0(4) . 16 ? O29 V14 V18 38.6(3) . 16 ? O17 V14 V18 114.9(3) . 16 ? O15 V14 V18 40.7(3) . 16 ? O38 V14 V18 83.2(2) . 16 ? O28 V14 V17 81.4(3) . . ? O33 V14 V17 135.9(4) . . ? O29 V14 V17 120.4(3) . . ? O17 V14 V17 36.4(3) . . ? O15 V14 V17 81.6(3) . . ? O38 V14 V17 44.5(2) . . ? V18 V14 V17 115.76(10) 16 . ? O28 V14 V13 137.6(4) . . ? O33 V14 V13 87.5(4) . . ? O29 V14 V13 115.1(3) . . ? O17 V14 V13 37.9(3) . . ? O15 V14 V13 40.7(3) . . ? O38 V14 V13 82.7(2) . . ? V18 V14 V13 78.93(10) 16 . ? V17 V14 V13 63.08(8) . . ? O28 V14 V16 84.0(4) . . ? O33 V14 V16 136.0(4) . . ? O29 V14 V16 35.7(3) . . ? O17 V14 V16 120.7(3) . . ? O15 V14 V16 81.1(3) . . ? O38 V14 V16 44.3(2) . . ? V18 V14 V16 63.18(9) 16 . ? V17 V14 V16 87.63(9) . . ? V13 V14 V16 114.93(10) . . ? O1 V15 O7 104.4(7) . 6 ? O1 V15 O7 104.4(7) . . ? O7 V15 O7 93.7(8) 6 . ? O1 V15 O11 101.1(7) . 6 ? O7 V15 O11 85.8(5) 6 6 ? O7 V15 O11 153.7(5) . 6 ? O1 V15 O11 101.1(7) . . ? O7 V15 O11 153.7(5) 6 . ? O7 V15 O11 85.8(5) . . ? O11 V15 O11 83.3(7) 6 . ? O1 V15 O31 176.0(10) . . ? O7 V15 O31 78.2(5) 6 . ? O7 V15 O31 78.2(5) . . ? O11 V15 O31 76.0(4) 6 . ? O11 V15 O31 76.0(4) . . ? O1 V15 V7 131.8(6) . 6 ? O7 V15 V7 79.0(4) 6 6 ? O7 V15 V7 123.5(4) . 6 ? O11 V15 V7 30.7(3) 6 6 ? O11 V15 V7 79.5(3) . 6 ? O31 V15 V7 45.4(3) . 6 ? O1 V15 V7 131.8(6) . . ? O7 V15 V7 123.5(4) 6 . ? O7 V15 V7 79.0(4) . . ? O11 V15 V7 79.5(3) 6 . ? O11 V15 V7 30.7(3) . . ? O31 V15 V7 45.4(3) . . ? V7 V15 V7 61.29(12) 6 . ? O1 V15 V19 135.4(6) . 6 ? O7 V15 V19 31.1(4) 6 6 ? O7 V15 V19 83.0(4) . 6 ? O11 V15 V19 83.2(4) 6 6 ? O11 V15 V19 123.4(4) . 6 ? O31 V15 V19 47.5(3) . 6 ? V7 V15 V19 62.30(10) 6 6 ? V7 V15 V19 92.78(13) . 6 ? O1 V15 V19 135.4(6) . . ? O7 V15 V19 83.0(4) 6 . ? O7 V15 V19 31.1(4) . . ? O11 V15 V19 123.4(4) 6 . ? O11 V15 V19 83.2(4) . . ? O31 V15 V19 47.5(3) . . ? V7 V15 V19 92.78(13) 6 . ? V7 V15 V19 62.30(10) . . ? V19 V15 V19 60.48(14) 6 . ? O9 V16 O20 106.7(5) . . ? O9 V16 O29 101.8(5) . . ? O20 V16 O29 97.7(5) . . ? O9 V16 O41 96.9(4) . . ? O20 V16 O41 98.3(5) . . ? O29 V16 O41 150.7(4) . . ? O9 V16 O38 94.8(5) . . ? O20 V16 O38 158.4(5) . . ? O29 V16 O38 79.5(4) . . ? O41 V16 O38 76.6(4) . . ? O9 V16 O10 168.0(5) . 16 ? O20 V16 O10 85.2(5) . 16 ? O29 V16 O10 78.3(4) . 16 ? O41 V16 O10 78.7(4) . 16 ? O38 V16 O10 73.3(4) . 16 ? O9 V16 Mn2 131.7(4) . . ? O20 V16 Mn2 121.6(4) . . ? O29 V16 Mn2 75.7(3) . . ? O41 V16 Mn2 75.0(3) . . ? O38 V16 Mn2 36.9(2) . . ? O10 V16 Mn2 36.4(3) 16 . ? O9 V16 V11 142.5(4) . 16 ? O20 V16 V11 35.9(4) . 16 ? O29 V16 V11 86.9(3) . 16 ? O41 V16 V11 91.8(3) . 16 ? O38 V16 V11 122.6(3) . 16 ? O10 V16 V11 49.4(3) 16 16 ? Mn2 V16 V11 85.75(9) . 16 ? O9 V16 V14 87.5(4) . . ? O20 V16 V14 132.6(4) . . ? O29 V16 V14 35.0(3) . . ? O41 V16 V14 125.3(3) . . ? O38 V16 V14 48.7(2) . . ? O10 V16 V14 86.0(3) 16 . ? Mn2 V16 V14 62.76(7) . . ? V11 V16 V14 116.53(11) 16 . ? O9 V16 V4 85.2(4) . . ? O20 V16 V4 132.6(4) . . ? O29 V16 V4 125.2(3) . . ? O41 V16 V4 34.4(3) . . ? O38 V16 V4 45.7(2) . . ? O10 V16 V4 85.0(3) 16 . ? Mn2 V16 V4 61.13(9) . . ? V11 V16 V4 119.42(10) 16 . ? V14 V16 V4 92.65(9) . . ? O24 V17 O14 109.1(6) . . ? O24 V17 O17 102.5(4) . . ? O14 V17 O17 97.2(5) . . ? O24 V17 O41 98.2(4) . 16 ? O14 V17 O41 95.9(5) . 16 ? O17 V17 O41 150.4(4) . 16 ? O24 V17 O38 94.8(5) . . ? O14 V17 O38 155.9(5) . . ? O17 V17 O38 80.2(4) . . ? O41 V17 O38 77.0(4) 16 . ? O24 V17 O10 168.4(5) . . ? O14 V17 O10 82.3(5) . . ? O17 V17 O10 77.8(4) . . ? O41 V17 O10 77.8(4) 16 . ? O38 V17 O10 73.7(4) . . ? O24 V17 Mn2 131.9(4) . . ? O14 V17 Mn2 118.9(4) . . ? O17 V17 Mn2 75.6(3) . . ? O41 V17 Mn2 74.8(3) 16 . ? O38 V17 Mn2 37.1(2) . . ? O10 V17 Mn2 36.6(3) . . ? O24 V17 V14 87.1(4) . . ? O14 V17 V14 133.0(4) . . ? O17 V17 V14 35.9(3) . . ? O41 V17 V14 126.0(3) 16 . ? O38 V17 V14 49.0(2) . . ? O10 V17 V14 86.6(3) . . ? Mn2 V17 V14 63.06(7) . . ? O24 V17 V11 142.7(4) . . ? O14 V17 V11 33.7(4) . . ? O17 V17 V11 86.4(3) . . ? O41 V17 V11 90.0(3) 16 . ? O38 V17 V11 122.4(3) . . ? O10 V17 V11 48.7(3) . . ? Mn2 V17 V11 85.34(9) . . ? V14 V17 V11 117.03(11) . . ? O24 V17 V4 85.6(4) . . ? O14 V17 V4 130.9(4) . . ? O17 V17 V4 126.0(3) . . ? O41 V17 V4 34.9(3) 16 . ? O38 V17 V4 45.8(2) . . ? O10 V17 V4 85.0(3) . . ? Mn2 V17 V4 61.31(9) . . ? V14 V17 V4 93.04(9) . . ? V11 V17 V4 118.49(9) . . ? O6 V18 O4 104.8(6) . . ? O6 V18 O16 102.7(6) . . ? O4 V18 O16 93.2(5) . . ? O6 V18 O29 102.6(5) . 16 ? O4 V18 O29 90.2(5) . 16 ? O16 V18 O29 152.7(4) . 16 ? O6 V18 O15 100.0(6) . 16 ? O4 V18 O15 153.9(4) . 16 ? O16 V18 O15 89.2(5) . 16 ? O29 V18 O15 76.5(4) 16 16 ? O6 V18 O10 174.1(6) . . ? O4 V18 O10 80.8(4) . . ? O16 V18 O10 78.5(4) . . ? O29 V18 O10 75.3(4) 16 . ? O15 V18 O10 74.2(4) 16 . ? O6 V18 Mn2 137.4(5) . . ? O4 V18 Mn2 117.7(3) . . ? O16 V18 Mn2 79.2(3) . . ? O29 V18 Mn2 75.3(3) 16 . ? O15 V18 Mn2 37.6(2) 16 . ? O10 V18 Mn2 36.9(3) . . ? O6 V18 V14 89.6(4) . 16 ? O4 V18 V14 126.4(4) . 16 ? O16 V18 V14 134.2(4) . 16 ? O29 V18 V14 36.3(3) 16 16 ? O15 V18 V14 45.0(3) 16 16 ? O10 V18 V14 85.5(3) . 16 ? Mn2 V18 V14 63.29(7) . 16 ? O6 V18 V11 136.9(5) . . ? O4 V18 V11 32.2(3) . . ? O16 V18 V11 83.2(4) . . ? O29 V18 V11 85.3(3) 16 . ? O15 V18 V11 122.9(3) 16 . ? O10 V18 V11 48.8(3) . . ? Mn2 V18 V11 85.69(9) . . ? V14 V18 V11 116.92(11) 16 . ? O6 V18 V13 134.6(5) . . ? O4 V18 V13 82.9(4) . . ? O16 V18 V13 32.0(3) . . ? O29 V18 V13 122.3(3) 16 . ? O15 V18 V13 85.5(3) 16 . ? O10 V18 V13 47.0(3) . . ? Mn2 V18 V13 58.78(7) . . ? V14 V18 V13 122.06(11) 16 . ? V11 V18 V13 60.04(10) . . ? O13 V19 O7 103.5(6) . . ? O13 V19 O35 105.6(6) . . ? O7 V19 O35 93.7(6) . . ? O13 V19 O23 100.1(5) . . ? O7 V19 O23 89.3(5) . . ? O35 V19 O23 152.7(5) . . ? O13 V19 O12 100.8(5) . . ? O7 V19 O12 154.0(5) . . ? O35 V19 O12 88.4(5) . . ? O23 V19 O12 77.5(4) . . ? O13 V19 O31 174.8(5) . . ? O7 V19 O31 79.8(5) . . ? O35 V19 O31 78.1(5) . . ? O23 V19 O31 75.8(4) . . ? O12 V19 O31 75.4(4) . . ? O13 V19 Mn1 138.6(5) . . ? O7 V19 Mn1 117.5(4) . . ? O35 V19 Mn1 78.2(4) . . ? O23 V19 Mn1 76.3(3) . . ? O12 V19 Mn1 37.8(3) . . ? O31 V19 Mn1 37.8(4) . . ? O13 V19 V9 88.2(4) . . ? O7 V19 V9 126.3(4) . . ? O35 V19 V9 133.7(5) . . ? O23 V19 V9 37.0(3) . . ? O12 V19 V9 45.3(3) . . ? O31 V19 V9 86.6(3) . . ? Mn1 V19 V9 63.83(8) . . ? O13 V19 V15 134.8(5) . . ? O7 V19 V15 31.4(4) . . ? O35 V19 V15 82.9(4) . . ? O23 V19 V15 85.8(3) . . ? O12 V19 V15 124.1(3) . . ? O31 V19 V15 48.7(4) . . ? Mn1 V19 V15 86.51(11) . . ? V9 V19 V15 118.12(13) . . ? O13 V19 V19 136.8(4) . 6 ? O7 V19 V19 82.6(3) . 6 ? O35 V19 V19 31.4(4) . 6 ? O23 V19 V19 123.0(3) . 6 ? O12 V19 V19 86.0(3) . 6 ? O31 V19 V19 47.2(3) . 6 ? Mn1 V19 V19 59.07(6) . 6 ? V9 V19 V19 122.90(6) . 6 ? V15 V19 V19 59.76(7) . 6 ? V6 O42 V7 109.5(5) . . ? V6 O42 V7 109.5(5) . 6 ? V7 O42 V7 108.0(7) . 6 ? V4 O41 V16 110.2(5) . . ? V4 O41 V17 108.2(4) . 16 ? V16 O41 V17 107.7(4) . 16 ? V9 O40 La2 140.6(5) . . ? V6 O39 V5 108.5(4) . . ? V6 O39 V5 108.5(4) . 6 ? V5 O39 V5 109.5(7) . 6 ? Mn2 O38 V16 98.7(4) . . ? Mn2 O38 V17 98.3(4) . . ? V16 O38 V17 162.6(5) . . ? Mn2 O38 V4 100.0(4) . . ? V16 O38 V4 90.4(3) . . ? V17 O38 V4 90.3(3) . . ? Mn2 O38 V14 99.3(4) . . ? V16 O38 V14 87.1(3) . . ? V17 O38 V14 86.5(3) . . ? V4 O38 V14 160.7(5) . . ? V9 O37 V5 108.2(5) . . ? V9 O37 V8 106.7(5) . . ? V5 O37 V8 112.0(4) . . ? Mn1 O36 V5 98.4(4) . . ? Mn1 O36 V7 97.4(4) . . ? V5 O36 V7 163.9(4) . . ? Mn1 O36 V6 98.3(4) . . ? V5 O36 V6 90.8(3) . . ? V7 O36 V6 90.1(3) . . ? Mn1 O36 V9 99.8(4) . . ? V5 O36 V9 87.1(3) . . ? V7 O36 V9 87.1(3) . . ? V6 O36 V9 162.0(4) . . ? V19 O35 V19 117.2(8) 6 . ? Mn1 O34 V8 95.2(5) . . ? Mn1 O34 V8 95.2(5) . 6 ? V8 O34 V8 86.5(5) . 6 ? Mn1 O34 V5 96.9(5) . 6 ? V8 O34 V5 167.8(7) . 6 ? V8 O34 V5 90.45(11) 6 6 ? Mn1 O34 V5 96.9(5) . . ? V8 O34 V5 90.45(11) . . ? V8 O34 V5 167.8(7) 6 . ? V5 O34 V5 90.0(5) 6 . ? Mn1 O34 V10 178.6(8) . . ? V8 O34 V10 83.9(4) . . ? V8 O34 V10 83.9(4) 6 . ? V5 O34 V10 84.1(4) 6 . ? V5 O34 V10 84.1(4) . . ? V14 O33 La2 152.0(6) . 7 ? V5 O32 V10 114.8(6) . . ? Mn1 O31 V7 97.3(5) . 6 ? Mn1 O31 V7 97.3(5) . . ? V7 O31 V7 91.2(6) 6 . ? Mn1 O31 V19 93.2(5) . . ? V7 O31 V19 169.1(7) 6 . ? V7 O31 V19 90.65(12) . . ? Mn1 O31 V19 93.2(5) . 6 ? V7 O31 V19 90.65(12) 6 6 ? V7 O31 V19 169.1(7) . 6 ? V19 O31 V19 85.6(5) . 6 ? Mn1 O31 V15 175.9(9) . . ? V7 O31 V15 85.6(4) 6 . ? V7 O31 V15 85.6(4) . . ? V19 O31 V15 83.8(5) . . ? V19 O31 V15 83.8(5) 6 . ? V8 O30 V8 116.8(8) 6 . ? V14 O29 V16 109.3(5) . . ? V14 O29 V18 105.1(5) . 16 ? V16 O29 V18 111.9(5) . 16 ? V14 O28 La1 140.3(5) . . ? V7 O26 La2 131.5(5) . . ? V4 O25 La1 136.3(5) . . ? V17 O24 La1 132.0(5) . . ? V7 O23 V9 108.8(5) . . ? V7 O23 V19 111.6(5) . . ? V9 O23 V19 105.0(5) . . ? V9 O22 La1 155.1(6) . . ? V8 O21 V10 118.1(6) . . ? V16 O20 V11 114.5(6) . 16 ? V5 O19 La2 131.6(6) . . ? V6 O18 La2 137.3(6) . 6 ? V14 O17 V17 107.7(5) . . ? V14 O17 V13 106.0(5) . . ? V17 O17 V13 111.9(5) . . ? V13 O16 V18 115.9(6) . . ? Mn2 O15 V18 102.4(4) . 16 ? Mn2 O15 V13 100.4(4) . . ? V18 O15 V13 152.7(5) 16 . ? Mn2 O15 V14 103.6(4) . . ? V18 O15 V14 94.3(4) 16 . ? V13 O15 V14 94.9(4) . . ? V17 O14 V11 117.1(6) . . ? Mn1 O12 V19 101.9(5) . . ? Mn1 O12 V8 100.3(5) . . ? V19 O12 V8 154.0(5) . . ? Mn1 O12 V9 103.9(4) . . ? V19 O12 V9 94.3(4) . . ? V8 O12 V9 93.4(4) . . ? V7 O11 V15 113.2(6) . . ? Mn2 O10 V16 97.4(4) . 16 ? Mn2 O10 V17 96.8(4) . . ? V16 O10 V17 89.9(4) 16 . ? Mn2 O10 V13 93.9(4) . . ? V16 O10 V13 168.4(5) 16 . ? V17 O10 V13 91.6(4) . . ? Mn2 O10 V18 94.3(4) . . ? V16 O10 V18 91.1(3) 16 . ? V17 O10 V18 168.7(5) . . ? V13 O10 V18 85.2(3) . . ? Mn2 O10 V11 177.1(6) . . ? V16 O10 V11 84.4(4) 16 . ? V17 O10 V11 85.5(4) . . ? V13 O10 V11 84.2(4) . . ? V18 O10 V11 83.4(3) . . ? V16 O9 La1 132.6(5) . . ? V15 O7 V19 117.6(6) . . ? V13 O5 V11 118.4(6) . . ? V18 O4 V11 117.0(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.233 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.180