# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_ld _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H133 K3 La6 Mn3 N3 O185 S2 V39' _chemical_formula_weight 6518.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 24.559(3) _cell_length_b 24.559(3) _cell_length_c 17.082(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8922.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5438 _cell_measurement_theta_min 0.96 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6290 _exptl_absorpt_coefficient_mu 3.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.4654 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45461 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_unetI/netI 0.0508 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5438 _reflns_number_gt 4037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit-3 50' was used to omit the weak reflections above 50 degree. In the structure, the C1, C2 and C5 atoms of the isolated organic molecule (nicotinic acid) reside on the mirror plane and the C4 and N1 centers exhibit the site-occupancy disorder with 50% for each. All the organic molecules are restrained with the command 'DFIX' so as to get a chemically reasonable structural feature. Moreover, all the atoms are restrained with the commands 'simu' and 'isor' so as to avoid the ADP problems. These restrained commands led to a final restraint value of 67. Furthermore, the H atoms on the ligands cannot be added due to the C/N disorder problem. In the final refinement, only four positions of the isolated lattice water molecules can be well confirmed from the residual peaks. Thus, the SQUEEZE program was used to estimate the rest lattice water molecules in the solvent accessible voids. Based on the calculation results, elemental analysis and TG analysis, another fifteen H2O molecules were directly included in the final molecular formula. It is worth mentioning that there is a relatively high residual peak (4.17 eA-3) is close to the O2 and O5 atoms of the POM with the distances of 1.90 A. This peak cannot be assigned as a disordered lattice water molecule, NH4+ or disordered K+ cations due to the obviously unreasonable bond distances to the O atoms of POMs. It is presumed that such a resiual peak is attributed to the series termination errors. ; 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 0.000 0.000 -0.003 353.2 147.3 2 -0.027 0.487 -0.016 1391.8 470.2 _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^)+(0.0725P)^2^+17.8348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5438 _refine_ls_number_parameters 391 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.079 _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 V1 V -0.05714(9) 0.30027(10) 0.7500 0.0326(5) Uani 1 2 d S . . V2 V 0.30764(9) 0.34926(9) 0.7500 0.0309(5) Uani 1 2 d S . . V3 V 0.12793(7) 0.33179(6) 0.55884(7) 0.0301(3) Uani 1 1 d . . . V4 V 0.18358(7) 0.26551(6) 0.65811(7) 0.0287(3) Uani 1 1 d . . . V5 V 0.06331(6) 0.39266(6) 0.65666(7) 0.0238(3) Uani 1 1 d . . . V6 V 0.01131(6) 0.24224(6) 0.65812(7) 0.0293(3) Uani 1 1 d . . . V7 V 0.24983(6) 0.41741(6) 0.65640(7) 0.0230(3) Uani 1 1 d . . . V8 V 0.18643(8) 0.48130(8) 0.7500 0.0214(4) Uani 1 2 d S . . Mn1 Mn 0.12886(7) 0.33426(7) 0.7500 0.0183(3) Uani 1 2 d S . . La1 La 0.19822(2) 0.51207(2) 0.52133(3) 0.03385(17) Uani 1 1 d . . . O1W O 0.2247(4) 0.5923(4) 0.4100(5) 0.095(3) Uani 1 1 d . . . O2W O 0.1115(3) 0.4729(4) 0.4192(4) 0.067(2) Uani 1 1 d . . . O3W O 0.1616(3) 0.5907(3) 0.5584(5) 0.066(2) Uani 1 1 d . . . O4W O 0.2639(4) 0.4963(4) 0.4162(4) 0.071(2) Uani 1 1 d . . . O1 O -0.1258(4) 0.2912(4) 0.7500 0.044(2) Uani 1 2 d S . . O2 O 0.1597(4) 0.2206(3) 0.7500 0.0294(18) Uani 1 2 d S . . O3 O 0.1057(3) 0.2745(3) 0.4980(3) 0.0408(15) Uani 1 1 d . . . O4 O -0.0590(2) 0.2479(2) 0.6720(3) 0.0302(12) Uani 1 1 d . . . O5 O 0.0005(4) 0.1987(3) 0.7500 0.0298(18) Uani 1 2 d S . . O6 O -0.0082(3) 0.1899(3) 0.5926(3) 0.0394(14) Uani 1 1 d . . . O7 O 0.1055(2) 0.2741(2) 0.6672(3) 0.0247(11) Uani 1 1 d . . . O8 O 0.0887(2) 0.4474(2) 0.5906(3) 0.0278(12) Uani 1 1 d . . . O9 O 0.2667(3) 0.2919(2) 0.6716(3) 0.0310(13) Uani 1 1 d . . . O10 O 0.2090(3) 0.3448(3) 0.7500 0.0222(15) Uani 1 2 d S . . O11 O 0.0484(2) 0.3214(2) 0.5952(3) 0.0258(12) Uani 1 1 d . . . O12 O 0.1617(3) 0.2128(3) 0.5925(3) 0.0387(14) Uani 1 1 d . . . O13 O 0.0485(3) 0.3237(3) 0.7500 0.0206(15) Uani 1 2 d S . . O14 O 0.3770(4) 0.3589(4) 0.7500 0.044(2) Uani 1 2 d S . . O15 O 0.2673(2) 0.4714(2) 0.5907(3) 0.0304(12) Uani 1 1 d . . . O16 O 0.0960(3) 0.4452(3) 0.7500 0.0241(16) Uani 1 2 d S . . O17 O 0.2076(2) 0.3424(2) 0.5951(3) 0.0243(11) Uani 1 1 d . . . O18 O 0.2563(3) 0.4661(3) 0.7500 0.0190(15) Uani 1 2 d S . . O19 O -0.0137(2) 0.3698(3) 0.6736(3) 0.0306(13) Uani 1 1 d . . . O20 O 0.3167(2) 0.4150(2) 0.6732(3) 0.0307(13) Uani 1 1 d . . . O21 O 0.1531(3) 0.3960(3) 0.5038(3) 0.0360(14) Uani 1 1 d . . . O22 O 0.1538(2) 0.3979(2) 0.6730(3) 0.0225(11) Uani 1 1 d . . . O23 O 0.2046(2) 0.5272(2) 0.6727(3) 0.0314(13) Uani 1 1 d . . . S1 S 0.3333 0.6667 0.5784(2) 0.0364(9) Uani 1 3 d S . . O24 O 0.3333 0.6667 0.6629(7) 0.076(4) Uani 1 3 d S . . O25 O 0.3045(3) 0.6024(3) 0.5485(4) 0.0447(16) Uani 1 1 d . . . K1 K 0.3590(3) 0.5859(2) 0.7500 0.150(3) Uani 1 2 d S . . O51 O 0.0594(4) 0.1534(5) 0.3152(5) 0.115(3) Uani 1 1 d DU . . C1 C 0.0720(8) 0.1864(6) 0.2500 0.085(4) Uani 1 2 d SDU . . C2 C 0.0993(7) 0.2548(5) 0.2500 0.080(4) Uani 1 2 d SDU . . C3 C 0.1120(6) 0.2873(6) 0.3211(6) 0.092(3) Uani 1 1 d DU . . C4 C 0.1367(6) 0.3519(5) 0.3212(5) 0.110(4) Uani 0.50 1 d PDU . . N1 N 0.1367(6) 0.3519(5) 0.3212(5) 0.110(4) Uani 0.50 1 d P . . C5 C 0.1485(10) 0.3851(6) 0.2500 0.125(6) Uani 1 2 d SDU . . O5W O 0.0535(3) 0.1411(3) 0.4831(4) 0.0566(18) Uani 1 1 d . . . O6W O 0.0106(3) 0.3563(3) 0.4511(4) 0.066(2) Uani 1 1 d . . . O7W O 0.2789(4) 0.3962(4) 0.4492(5) 0.091(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0189(10) 0.0356(12) 0.0365(11) 0.000 0.000 0.0085(9) V2 0.0310(11) 0.0338(11) 0.0361(11) 0.000 0.000 0.0224(10) V3 0.0344(8) 0.0282(8) 0.0250(7) -0.0004(6) -0.0002(6) 0.0137(6) V4 0.0382(8) 0.0256(7) 0.0270(7) -0.0040(6) -0.0011(6) 0.0195(7) V5 0.0223(7) 0.0222(7) 0.0253(7) 0.0013(5) -0.0025(5) 0.0099(6) V6 0.0274(7) 0.0239(7) 0.0258(7) -0.0032(6) -0.0023(6) 0.0047(6) V7 0.0223(7) 0.0196(7) 0.0261(7) 0.0014(5) 0.0036(5) 0.0097(6) V8 0.0181(9) 0.0158(9) 0.0297(10) 0.000 0.000 0.0080(8) Mn1 0.0184(8) 0.0151(8) 0.0200(7) 0.000 0.000 0.0074(7) La1 0.0323(3) 0.0285(3) 0.0388(3) 0.0084(2) 0.0019(2) 0.0137(2) O1W 0.105(7) 0.073(6) 0.090(6) 0.040(5) -0.002(5) 0.032(5) O2W 0.064(5) 0.075(5) 0.053(4) 0.009(4) -0.017(4) 0.027(4) O3W 0.067(5) 0.040(4) 0.099(6) 0.009(4) -0.004(4) 0.032(4) O4W 0.085(6) 0.076(6) 0.057(4) 0.007(4) 0.027(4) 0.044(5) O1 0.016(4) 0.050(6) 0.055(5) 0.000 0.000 0.009(4) O2 0.046(5) 0.024(4) 0.026(4) 0.000 0.000 0.023(4) O3 0.051(4) 0.040(3) 0.029(3) -0.009(3) -0.005(3) 0.021(3) O4 0.019(3) 0.031(3) 0.030(3) -0.001(2) -0.004(2) 0.005(2) O5 0.036(5) 0.015(4) 0.025(4) 0.000 0.000 0.003(3) O6 0.045(4) 0.033(3) 0.027(3) -0.010(3) -0.003(3) 0.010(3) O7 0.029(3) 0.017(3) 0.027(3) -0.002(2) -0.002(2) 0.010(2) O8 0.029(3) 0.029(3) 0.025(3) 0.007(2) 0.000(2) 0.014(3) O9 0.038(3) 0.029(3) 0.033(3) 0.000(2) 0.003(2) 0.022(3) O10 0.025(4) 0.022(4) 0.023(4) 0.000 0.000 0.014(3) O11 0.024(3) 0.026(3) 0.021(3) 0.001(2) -0.001(2) 0.008(2) O12 0.059(4) 0.033(3) 0.034(3) -0.009(3) -0.001(3) 0.030(3) O13 0.016(4) 0.016(4) 0.022(4) 0.000 0.000 0.002(3) O14 0.031(5) 0.056(6) 0.059(6) 0.000 0.000 0.032(5) O15 0.031(3) 0.030(3) 0.028(3) 0.008(2) 0.010(2) 0.013(3) O16 0.017(4) 0.024(4) 0.028(4) 0.000 0.000 0.008(3) O17 0.027(3) 0.025(3) 0.020(2) -0.002(2) 0.002(2) 0.013(2) O18 0.018(4) 0.013(4) 0.031(4) 0.000 0.000 0.012(3) O19 0.020(3) 0.037(3) 0.033(3) -0.002(2) -0.007(2) 0.013(3) O20 0.026(3) 0.030(3) 0.038(3) 0.003(2) 0.003(2) 0.016(3) O21 0.042(4) 0.037(3) 0.028(3) 0.008(2) 0.003(3) 0.018(3) O22 0.021(3) 0.024(3) 0.022(3) 0.000(2) -0.001(2) 0.010(2) O23 0.023(3) 0.028(3) 0.040(3) 0.010(2) 0.003(2) 0.011(3) S1 0.0284(12) 0.0284(12) 0.052(2) 0.000 0.000 0.0142(6) O24 0.089(6) 0.089(6) 0.051(8) 0.000 0.000 0.044(3) O25 0.029(3) 0.019(3) 0.079(5) 0.006(3) 0.009(3) 0.007(3) K1 0.079(4) 0.076(4) 0.266(8) 0.000 0.000 0.016(3) O51 0.087(6) 0.180(8) 0.086(5) 0.018(6) 0.007(5) 0.072(6) C1 0.061(7) 0.121(8) 0.085(7) 0.000 0.000 0.055(6) C2 0.056(6) 0.118(7) 0.084(6) 0.000 0.000 0.057(5) C3 0.060(5) 0.133(6) 0.096(6) -0.006(5) 0.004(4) 0.059(5) C4 0.077(5) 0.145(7) 0.123(6) -0.013(5) 0.004(5) 0.067(5) N1 0.077(5) 0.145(7) 0.123(6) -0.013(5) 0.004(5) 0.067(5) C5 0.094(8) 0.145(9) 0.143(9) 0.000 0.000 0.065(6) O5W 0.043(4) 0.075(5) 0.056(4) -0.016(4) -0.009(3) 0.032(4) O6W 0.069(5) 0.064(5) 0.060(4) -0.012(4) -0.026(4) 0.030(4) O7W 0.127(8) 0.106(7) 0.063(5) -0.010(5) 0.024(5) 0.075(6) _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 V1 O1 1.587(8) . ? V1 O4 1.836(5) . ? V1 O4 1.836(5) 10_557 ? V1 O19 1.983(6) 10_557 ? V1 O19 1.983(6) . ? V1 O13 2.360(7) . ? V1 V6 3.117(2) . ? V1 V6 3.117(2) 10_557 ? V1 V5 3.119(2) 10_557 ? V1 V5 3.119(2) . ? V2 O14 1.597(8) . ? V2 O9 1.837(5) . ? V2 O9 1.837(5) 10_557 ? V2 O20 2.004(5) 10_557 ? V2 O20 2.004(5) . ? V2 O10 2.371(7) . ? V2 V4 3.116(2) . ? V2 V4 3.116(2) 10_557 ? V3 O3 1.608(6) . ? V3 O21 1.667(5) . ? V3 O17 1.941(5) . ? V3 O11 1.942(5) . ? V3 O7 2.226(5) . ? V3 O22 2.410(5) . ? V3 V6 3.1011(19) . ? V3 V4 3.1013(19) . ? V4 O12 1.589(5) . ? V4 O9 1.821(5) . ? V4 O2 1.838(4) . ? V4 O17 1.990(5) . ? V4 O7 2.038(5) . ? V4 O10 2.330(5) . ? V4 Mn1 3.0643(18) . ? V5 O8 1.623(5) . ? V5 O19 1.706(5) . ? V5 O11 1.912(5) . ? V5 O16 1.954(4) . ? V5 O22 2.180(5) . ? V5 O13 2.219(5) . ? V5 Mn1 3.0823(18) . ? V6 O6 1.588(5) . ? V6 O4 1.817(5) . ? V6 O5 1.842(4) . ? V6 O11 1.999(5) . ? V6 O7 2.043(5) . ? V6 O13 2.340(5) . ? V6 Mn1 3.0628(18) . ? V7 O15 1.623(5) . ? V7 O20 1.698(5) . ? V7 O17 1.911(5) . ? V7 O18 1.955(4) . ? V7 O22 2.177(5) . ? V7 O10 2.226(5) . ? V7 Mn1 3.0798(18) . ? V7 K1 3.971(5) . ? V8 O23 1.646(5) 10_557 ? V8 O23 1.646(5) . ? V8 O18 1.930(6) . ? V8 O16 1.936(7) . ? V8 O22 2.220(5) . ? V8 O22 2.220(5) 10_557 ? V8 Mn1 3.152(2) . ? V8 K1 3.532(5) 3_565 ? V8 K1 3.697(6) . ? Mn1 O10 1.851(7) . ? Mn1 O13 1.858(7) . ? Mn1 O22 1.895(5) 10_557 ? Mn1 O22 1.895(5) . ? Mn1 O7 1.914(5) . ? Mn1 O7 1.914(5) 10_557 ? Mn1 V6 3.0628(18) 10_557 ? Mn1 V4 3.0643(18) 10_557 ? Mn1 V7 3.0798(18) 10_557 ? La1 O25 2.482(6) . ? La1 O21 2.506(6) . ? La1 O2W 2.540(7) . ? La1 O4W 2.569(7) . ? La1 O1W 2.577(7) . ? La1 O3W 2.584(7) . ? La1 O23 2.607(5) . ? La1 O8 2.624(5) . ? La1 O15 2.640(5) . ? O2 V4 1.838(4) 10_557 ? O5 V6 1.842(4) 10_557 ? O10 V7 2.226(5) 10_557 ? O10 V4 2.330(5) 10_557 ? O13 V5 2.219(5) 10_557 ? O13 V6 2.340(5) 10_557 ? O16 V5 1.954(4) 10_557 ? O18 V7 1.955(4) 10_557 ? O18 K1 2.756(8) . ? O23 K1 2.885(7) 3_565 ? S1 O24 1.445(12) . ? S1 O25 1.461(6) 3_565 ? S1 O25 1.461(6) . ? S1 O25 1.461(6) 2_665 ? S1 K1 3.766(5) 3_565 ? S1 K1 3.766(5) 2_665 ? S1 K1 3.766(5) . ? O24 K1 2.793(8) 3_565 ? O24 K1 2.793(8) 2_665 ? O24 K1 2.793(8) . ? K1 O24 2.793(8) 10_557 ? K1 O23 2.885(7) 11_667 ? K1 O23 2.885(7) 2_665 ? K1 V8 3.532(5) 2_665 ? K1 S1 3.766(5) 10_557 ? K1 V7 3.971(5) 10_557 ? K1 K1 4.094(11) 2_665 ? O51 C1 1.321(8) . ? C1 O51 1.321(8) 10_556 ? C1 C2 1.464(9) . ? C2 C3 1.401(8) . ? C2 C3 1.401(8) 10_556 ? C3 C4 1.386(9) . ? C4 C5 1.411(9) . ? C5 N1 1.411(9) 10_556 ? C5 C4 1.411(9) 10_556 ? 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 O1 V1 O4 104.4(3) . . ? O1 V1 O4 104.4(3) . 10_557 ? O4 V1 O4 93.1(3) . 10_557 ? O1 V1 O19 101.4(3) . 10_557 ? O4 V1 O19 153.4(2) . 10_557 ? O4 V1 O19 86.5(2) 10_557 10_557 ? O1 V1 O19 101.4(3) . . ? O4 V1 O19 86.5(2) . . ? O4 V1 O19 153.4(2) 10_557 . ? O19 V1 O19 82.3(3) 10_557 . ? O1 V1 O13 174.7(4) . . ? O4 V1 O13 79.1(2) . . ? O4 V1 O13 79.1(2) 10_557 . ? O19 V1 O13 74.75(19) 10_557 . ? O19 V1 O13 74.75(19) . . ? O1 V1 V6 135.6(2) . . ? O4 V1 V6 31.23(16) . . ? O4 V1 V6 82.87(17) 10_557 . ? O19 V1 V6 122.93(16) 10_557 . ? O19 V1 V6 83.15(16) . . ? O13 V1 V6 48.18(12) . . ? O1 V1 V6 135.6(2) . 10_557 ? O4 V1 V6 82.87(17) . 10_557 ? O4 V1 V6 31.23(16) 10_557 10_557 ? O19 V1 V6 83.15(16) 10_557 10_557 ? O19 V1 V6 122.93(16) . 10_557 ? O13 V1 V6 48.18(12) . 10_557 ? V6 V1 V6 60.46(6) . 10_557 ? O1 V1 V5 131.0(2) . 10_557 ? O4 V1 V5 124.26(18) . 10_557 ? O4 V1 V5 79.68(17) 10_557 10_557 ? O19 V1 V5 29.67(15) 10_557 10_557 ? O19 V1 V5 78.70(15) . 10_557 ? O13 V1 V5 45.20(12) . 10_557 ? V6 V1 V5 93.32(6) . 10_557 ? V6 V1 V5 62.81(4) 10_557 10_557 ? O1 V1 V5 131.0(2) . . ? O4 V1 V5 79.68(17) . . ? O4 V1 V5 124.26(18) 10_557 . ? O19 V1 V5 78.70(15) 10_557 . ? O19 V1 V5 29.67(15) . . ? O13 V1 V5 45.20(12) . . ? V6 V1 V5 62.81(4) . . ? V6 V1 V5 93.32(6) 10_557 . ? V5 V1 V5 61.49(6) 10_557 . ? O14 V2 O9 104.4(3) . . ? O14 V2 O9 104.4(3) . 10_557 ? O9 V2 O9 93.6(3) . 10_557 ? O14 V2 O20 101.5(3) . 10_557 ? O9 V2 O20 153.3(2) . 10_557 ? O9 V2 O20 86.5(2) 10_557 10_557 ? O14 V2 O20 101.5(3) . . ? O9 V2 O20 86.5(2) . . ? O9 V2 O20 153.3(2) 10_557 . ? O20 V2 O20 81.8(3) 10_557 . ? O14 V2 O10 174.9(4) . . ? O9 V2 O10 79.0(2) . . ? O9 V2 O10 79.0(2) 10_557 . ? O20 V2 O10 74.76(19) 10_557 . ? O20 V2 O10 74.76(19) . . ? O14 V2 V4 135.7(2) . . ? O9 V2 V4 31.44(17) . . ? O9 V2 V4 83.19(18) 10_557 . ? O20 V2 V4 122.69(17) 10_557 . ? O20 V2 V4 83.12(16) . . ? O10 V2 V4 47.92(13) . . ? O14 V2 V4 135.7(2) . 10_557 ? O9 V2 V4 83.19(18) . 10_557 ? O9 V2 V4 31.44(17) 10_557 10_557 ? O20 V2 V4 83.12(16) 10_557 10_557 ? O20 V2 V4 122.69(17) . 10_557 ? O10 V2 V4 47.92(13) . 10_557 ? V4 V2 V4 60.49(6) . 10_557 ? O3 V3 O21 105.4(3) . . ? O3 V3 O17 101.7(3) . . ? O21 V3 O17 100.4(2) . . ? O3 V3 O11 102.3(3) . . ? O21 V3 O11 100.2(2) . . ? O17 V3 O11 142.7(2) . . ? O3 V3 O7 96.5(2) . . ? O21 V3 O7 158.1(2) . . ? O17 V3 O7 74.5(2) . . ? O11 V3 O7 74.78(19) . . ? O3 V3 O22 166.2(2) . . ? O21 V3 O22 88.3(2) . . ? O17 V3 O22 75.07(18) . . ? O11 V3 O22 74.85(18) . . ? O7 V3 O22 69.73(17) . . ? O3 V3 V6 86.8(2) . . ? O21 V3 V6 138.9(2) . . ? O17 V3 V6 115.60(15) . . ? O11 V3 V6 38.76(15) . . ? O7 V3 V6 41.14(13) . . ? O22 V3 V6 82.78(12) . . ? O3 V3 V4 86.6(2) . . ? O21 V3 V4 138.8(2) . . ? O17 V3 V4 38.48(15) . . ? O11 V3 V4 115.78(15) . . ? O7 V3 V4 41.01(13) . . ? O22 V3 V4 82.76(12) . . ? V6 V3 V4 79.74(5) . . ? O12 V4 O9 103.9(3) . . ? O12 V4 O2 103.7(3) . . ? O9 V4 O2 94.0(3) . . ? O12 V4 O17 102.1(2) . . ? O9 V4 O17 89.1(2) . . ? O2 V4 O17 152.3(2) . . ? O12 V4 O7 100.7(3) . . ? O9 V4 O7 154.0(2) . . ? O2 V4 O7 87.9(3) . . ? O17 V4 O7 77.9(2) . . ? O12 V4 O10 174.9(3) . . ? O9 V4 O10 80.4(2) . . ? O2 V4 O10 78.3(2) . . ? O17 V4 O10 75.09(18) . . ? O7 V4 O10 74.6(2) . . ? O12 V4 Mn1 138.4(2) . . ? O9 V4 Mn1 117.49(17) . . ? O2 V4 Mn1 78.3(2) . . ? O17 V4 Mn1 75.95(14) . . ? O7 V4 Mn1 37.71(13) . . ? O10 V4 Mn1 37.09(17) . . ? O12 V4 V3 89.1(2) . . ? O9 V4 V3 126.31(17) . . ? O2 V4 V3 133.6(2) . . ? O17 V4 V3 37.36(14) . . ? O7 V4 V3 45.77(14) . . ? O10 V4 V3 86.20(14) . . ? Mn1 V4 V3 63.97(4) . . ? O12 V4 V2 135.5(2) . . ? O9 V4 V2 31.74(16) . . ? O2 V4 V2 83.1(2) . . ? O17 V4 V2 85.31(15) . . ? O7 V4 V2 123.59(14) . . ? O10 V4 V2 49.03(17) . . ? Mn1 V4 V2 86.08(5) . . ? V3 V4 V2 118.10(6) . . ? O8 V5 O19 107.1(3) . . ? O8 V5 O11 101.2(2) . . ? O19 V5 O11 96.7(2) . . ? O8 V5 O16 99.2(3) . . ? O19 V5 O16 95.8(3) . . ? O11 V5 O16 151.7(2) . . ? O8 V5 O22 94.7(2) . . ? O19 V5 O22 158.0(2) . . ? O11 V5 O22 81.2(2) . . ? O16 V5 O22 77.7(2) . . ? O8 V5 O13 168.7(3) . . ? O19 V5 O13 84.0(2) . . ? O11 V5 O13 79.24(19) . . ? O16 V5 O13 76.9(2) . . ? O22 V5 O13 74.1(2) . . ? O8 V5 Mn1 132.21(19) . . ? O19 V5 Mn1 120.63(19) . . ? O11 V5 Mn1 76.35(15) . . ? O16 V5 Mn1 75.4(2) . . ? O22 V5 Mn1 37.49(12) . . ? O13 V5 Mn1 36.66(17) . . ? O8 V5 V1 142.20(19) . . ? O19 V5 V1 35.12(18) . . ? O11 V5 V1 86.38(16) . . ? O16 V5 V1 89.47(18) . . ? O22 V5 V1 123.08(13) . . ? O13 V5 V1 48.99(17) . . ? Mn1 V5 V1 85.59(5) . . ? O6 V6 O4 103.9(3) . . ? O6 V6 O5 103.5(3) . . ? O4 V6 O5 93.8(3) . . ? O6 V6 O11 102.4(3) . . ? O4 V6 O11 89.0(2) . . ? O5 V6 O11 152.4(2) . . ? O6 V6 O7 101.0(3) . . ? O4 V6 O7 153.9(2) . . ? O5 V6 O7 88.0(3) . . ? O11 V6 O7 77.9(2) . . ? O6 V6 O13 175.2(3) . . ? O4 V6 O13 80.0(2) . . ? O5 V6 O13 78.8(2) . . ? O11 V6 O13 74.64(18) . . ? O7 V6 O13 74.8(2) . . ? O6 V6 Mn1 138.7(2) . . ? O4 V6 Mn1 117.25(17) . . ? O5 V6 Mn1 78.5(2) . . ? O11 V6 Mn1 75.80(14) . . ? O7 V6 Mn1 37.77(13) . . ? O13 V6 Mn1 37.28(17) . . ? O6 V6 V3 89.2(2) . . ? O4 V6 V3 126.37(18) . . ? O5 V6 V3 133.8(2) . . ? O11 V6 V3 37.45(15) . . ? O7 V6 V3 45.78(14) . . ? O13 V6 V3 86.16(13) . . ? Mn1 V6 V3 63.99(4) . . ? O6 V6 V1 135.4(2) . . ? O4 V6 V1 31.60(16) . . ? O5 V6 V1 83.2(2) . . ? O11 V6 V1 85.02(15) . . ? O7 V6 V1 123.52(14) . . ? O13 V6 V1 48.73(17) . . ? Mn1 V6 V1 85.96(5) . . ? V3 V6 V1 117.97(6) . . ? O15 V7 O20 106.3(3) . . ? O15 V7 O17 101.7(2) . . ? O20 V7 O17 97.3(2) . . ? O15 V7 O18 99.1(2) . . ? O20 V7 O18 95.7(3) . . ? O17 V7 O18 151.2(2) . . ? O15 V7 O22 94.9(2) . . ? O20 V7 O22 158.6(2) . . ? O17 V7 O22 81.53(19) . . ? O18 V7 O22 77.1(2) . . ? O15 V7 O10 168.7(3) . . ? O20 V7 O10 84.7(2) . . ? O17 V7 O10 79.1(2) . . ? O18 V7 O10 76.6(2) . . ? O22 V7 O10 74.1(2) . . ? O15 V7 Mn1 132.4(2) . . ? O20 V7 Mn1 121.25(18) . . ? O17 V7 Mn1 76.50(15) . . ? O18 V7 Mn1 74.76(19) . . ? O22 V7 Mn1 37.53(13) . . ? O10 V7 Mn1 36.56(17) . . ? O15 V7 K1 70.2(2) . . ? O20 V7 K1 78.9(2) . . ? O17 V7 K1 169.37(16) . . ? O18 V7 K1 39.42(19) . . ? O22 V7 K1 105.64(15) . . ? O10 V7 K1 110.16(14) . . ? Mn1 V7 K1 114.00(7) . . ? O23 V8 O23 106.6(4) 10_557 . ? O23 V8 O18 99.8(2) 10_557 . ? O23 V8 O18 99.8(2) . . ? O23 V8 O16 99.7(2) 10_557 . ? O23 V8 O16 99.7(2) . . ? O18 V8 O16 147.0(3) . . ? O23 V8 O22 163.0(2) 10_557 . ? O23 V8 O22 90.4(2) . . ? O18 V8 O22 76.5(2) . . ? O16 V8 O22 77.0(2) . . ? O23 V8 O22 90.4(2) 10_557 10_557 ? O23 V8 O22 163.0(2) . 10_557 ? O18 V8 O22 76.5(2) . 10_557 ? O16 V8 O22 77.0(2) . 10_557 ? O22 V8 O22 72.7(2) . 10_557 ? O23 V8 Mn1 126.7(2) 10_557 . ? O23 V8 Mn1 126.7(2) . . ? O18 V8 Mn1 73.2(2) . . ? O16 V8 Mn1 73.8(2) . . ? O22 V8 Mn1 36.34(12) . . ? O22 V8 Mn1 36.34(12) 10_557 . ? O23 V8 K1 53.8(2) 10_557 3_565 ? O23 V8 K1 53.8(2) . 3_565 ? O18 V8 K1 115.6(2) . 3_565 ? O16 V8 K1 97.4(2) . 3_565 ? O22 V8 K1 142.77(12) . 3_565 ? O22 V8 K1 142.77(12) 10_557 3_565 ? Mn1 V8 K1 171.23(12) . 3_565 ? O23 V8 K1 72.6(2) 10_557 . ? O23 V8 K1 72.6(2) . . ? O18 V8 K1 46.6(2) . . ? O16 V8 K1 166.4(2) . . ? O22 V8 K1 113.59(15) . . ? O22 V8 K1 113.59(15) 10_557 . ? Mn1 V8 K1 119.83(11) . . ? K1 V8 K1 68.9(2) 3_565 . ? O10 Mn1 O13 180.0(3) . . ? O10 Mn1 O22 90.1(2) . 10_557 ? O13 Mn1 O22 89.9(2) . 10_557 ? O10 Mn1 O22 90.1(2) . . ? O13 Mn1 O22 89.9(2) . . ? O22 Mn1 O22 87.9(3) 10_557 . ? O10 Mn1 O7 89.8(2) . . ? O13 Mn1 O7 90.3(2) . . ? O22 Mn1 O7 176.3(2) 10_557 . ? O22 Mn1 O7 88.4(2) . . ? O10 Mn1 O7 89.8(2) . 10_557 ? O13 Mn1 O7 90.3(2) . 10_557 ? O22 Mn1 O7 88.4(2) 10_557 10_557 ? O22 Mn1 O7 176.3(2) . 10_557 ? O7 Mn1 O7 95.3(3) . 10_557 ? O10 Mn1 V6 130.29(16) . . ? O13 Mn1 V6 49.73(15) . . ? O22 Mn1 V6 139.57(16) 10_557 . ? O22 Mn1 V6 92.85(14) . . ? O7 Mn1 V6 40.84(16) . . ? O7 Mn1 V6 90.05(16) 10_557 . ? O10 Mn1 V6 130.29(16) . 10_557 ? O13 Mn1 V6 49.73(15) . 10_557 ? O22 Mn1 V6 92.85(14) 10_557 10_557 ? O22 Mn1 V6 139.57(16) . 10_557 ? O7 Mn1 V6 90.05(16) . 10_557 ? O7 Mn1 V6 40.84(16) 10_557 10_557 ? V6 Mn1 V6 61.65(6) . 10_557 ? O10 Mn1 V4 49.37(16) . . ? O13 Mn1 V4 130.65(16) . . ? O22 Mn1 V4 139.46(16) 10_557 . ? O22 Mn1 V4 92.79(15) . . ? O7 Mn1 V4 40.66(16) . . ? O7 Mn1 V4 89.92(15) 10_557 . ? V6 Mn1 V4 80.92(5) . . ? V6 Mn1 V4 111.54(6) 10_557 . ? O10 Mn1 V4 49.37(16) . 10_557 ? O13 Mn1 V4 130.65(16) . 10_557 ? O22 Mn1 V4 92.79(15) 10_557 10_557 ? O22 Mn1 V4 139.46(16) . 10_557 ? O7 Mn1 V4 89.92(15) . 10_557 ? O7 Mn1 V4 40.66(16) 10_557 10_557 ? V6 Mn1 V4 111.54(6) . 10_557 ? V6 Mn1 V4 80.92(5) 10_557 10_557 ? V4 Mn1 V4 61.63(6) . 10_557 ? O10 Mn1 V7 45.75(15) . 10_557 ? O13 Mn1 V7 134.23(15) . 10_557 ? O22 Mn1 V7 44.41(15) 10_557 10_557 ? O22 Mn1 V7 90.37(15) . 10_557 ? O7 Mn1 V7 135.49(17) . 10_557 ? O7 Mn1 V7 86.89(15) 10_557 10_557 ? V6 Mn1 V7 174.94(7) . 10_557 ? V6 Mn1 V7 117.65(3) 10_557 10_557 ? V4 Mn1 V7 95.04(5) . 10_557 ? V4 Mn1 V7 63.64(4) 10_557 10_557 ? O10 Mn1 V7 45.75(15) . . ? O13 Mn1 V7 134.23(15) . . ? O22 Mn1 V7 90.37(15) 10_557 . ? O22 Mn1 V7 44.41(15) . . ? O7 Mn1 V7 86.89(15) . . ? O7 Mn1 V7 135.49(17) 10_557 . ? V6 Mn1 V7 117.65(3) . . ? V6 Mn1 V7 174.94(7) 10_557 . ? V4 Mn1 V7 63.64(4) . . ? V4 Mn1 V7 95.04(5) 10_557 . ? V7 Mn1 V7 62.55(5) 10_557 . ? O25 La1 O21 135.09(18) . . ? O25 La1 O2W 140.8(2) . . ? O21 La1 O2W 71.2(2) . . ? O25 La1 O4W 78.8(2) . . ? O21 La1 O4W 72.5(2) . . ? O2W La1 O4W 86.2(3) . . ? O25 La1 O1W 72.8(2) . . ? O21 La1 O1W 125.5(2) . . ? O2W La1 O1W 68.0(3) . . ? O4W La1 O1W 70.3(3) . . ? O25 La1 O3W 83.7(2) . . ? O21 La1 O3W 139.3(2) . . ? O2W La1 O3W 85.0(2) . . ? O4W La1 O3W 139.8(2) . . ? O1W La1 O3W 70.0(3) . . ? O25 La1 O23 74.10(19) . . ? O21 La1 O23 103.98(16) . . ? O2W La1 O23 135.6(2) . . ? O4W La1 O23 135.9(2) . . ? O1W La1 O23 130.5(2) . . ? O3W La1 O23 70.6(2) . . ? O25 La1 O8 139.33(19) . . ? O21 La1 O8 68.23(17) . . ? O2W La1 O8 70.7(2) . . ? O4W La1 O8 139.0(2) . . ? O1W La1 O8 125.8(2) . . ? O3W La1 O8 73.0(2) . . ? O23 La1 O8 66.98(15) . . ? O25 La1 O15 70.52(18) . . ? O21 La1 O15 68.05(17) . . ? O2W La1 O15 137.8(2) . . ? O4W La1 O15 71.7(2) . . ? O1W La1 O15 131.0(2) . . ? O3W La1 O15 134.6(2) . . ? O23 La1 O15 66.72(16) . . ? O8 La1 O15 103.12(15) . . ? V4 O2 V4 117.3(4) 10_557 . ? V6 O4 V1 117.2(3) . . ? V6 O5 V6 116.9(4) 10_557 . ? Mn1 O7 V4 101.6(2) . . ? Mn1 O7 V6 101.4(2) . . ? V4 O7 V6 153.9(3) . . ? Mn1 O7 V3 103.9(2) . . ? V4 O7 V3 93.2(2) . . ? V6 O7 V3 93.08(19) . . ? V5 O8 La1 131.9(3) . . ? V4 O9 V2 116.8(3) . . ? Mn1 O10 V7 97.7(2) . 10_557 ? Mn1 O10 V7 97.7(2) . . ? V7 O10 V7 91.8(3) 10_557 . ? Mn1 O10 V4 93.5(2) . . ? V7 O10 V4 168.1(3) 10_557 . ? V7 O10 V4 90.61(6) . . ? Mn1 O10 V4 93.5(2) . 10_557 ? V7 O10 V4 90.61(6) 10_557 10_557 ? V7 O10 V4 168.1(3) . 10_557 ? V4 O10 V4 84.7(2) . 10_557 ? Mn1 O10 V2 175.4(4) . . ? V7 O10 V2 85.5(2) 10_557 . ? V7 O10 V2 85.5(2) . . ? V4 O10 V2 83.0(2) . . ? V4 O10 V2 83.0(2) 10_557 . ? V5 O11 V3 109.6(2) . . ? V5 O11 V6 112.4(2) . . ? V3 O11 V6 103.8(2) . . ? Mn1 O13 V5 97.8(2) . 10_557 ? Mn1 O13 V5 97.8(2) . . ? V5 O13 V5 91.9(3) 10_557 . ? Mn1 O13 V6 93.0(2) . . ? V5 O13 V6 168.3(3) 10_557 . ? V5 O13 V6 90.89(6) . . ? Mn1 O13 V6 93.0(2) . 10_557 ? V5 O13 V6 90.89(6) 10_557 10_557 ? V5 O13 V6 168.3(3) . 10_557 ? V6 O13 V6 84.2(2) . 10_557 ? Mn1 O13 V1 174.7(4) . . ? V5 O13 V1 85.8(2) 10_557 . ? V5 O13 V1 85.8(2) . . ? V6 O13 V1 83.09(19) . . ? V6 O13 V1 83.09(19) 10_557 . ? V7 O15 La1 131.4(3) . . ? V8 O16 V5 107.5(2) . . ? V8 O16 V5 107.5(2) . 10_557 ? V5 O16 V5 109.4(3) . 10_557 ? V7 O17 V3 109.2(2) . . ? V7 O17 V4 112.3(2) . . ? V3 O17 V4 104.2(2) . . ? V8 O18 V7 108.1(2) . . ? V8 O18 V7 108.1(2) . 10_557 ? V7 O18 V7 109.8(3) . 10_557 ? V8 O18 K1 102.8(3) . . ? V7 O18 K1 113.8(2) . . ? V7 O18 K1 113.8(2) 10_557 . ? V5 O19 V1 115.2(3) . . ? V7 O20 V2 114.7(3) . . ? V3 O21 La1 138.8(3) . . ? Mn1 O22 V7 98.1(2) . . ? Mn1 O22 V5 98.1(2) . . ? V7 O22 V5 163.1(2) . . ? Mn1 O22 V8 99.7(2) . . ? V7 O22 V8 91.30(18) . . ? V5 O22 V8 90.97(18) . . ? Mn1 O22 V3 98.0(2) . . ? V7 O22 V3 86.27(17) . . ? V5 O22 V3 86.49(16) . . ? V8 O22 V3 162.3(2) . . ? V8 O23 La1 136.2(3) . . ? V8 O23 K1 98.8(2) . 3_565 ? La1 O23 K1 124.12(19) . 3_565 ? O24 S1 O25 110.4(3) . 3_565 ? O24 S1 O25 110.4(3) . . ? O25 S1 O25 108.5(3) 3_565 . ? O24 S1 O25 110.4(3) . 2_665 ? O25 S1 O25 108.5(3) 3_565 2_665 ? O25 S1 O25 108.5(3) . 2_665 ? O24 S1 K1 38.87(8) . 3_565 ? O25 S1 K1 79.7(3) 3_565 3_565 ? O25 S1 K1 99.8(3) . 3_565 ? O25 S1 K1 145.5(3) 2_665 3_565 ? O24 S1 K1 38.87(8) . 2_665 ? O25 S1 K1 99.8(3) 3_565 2_665 ? O25 S1 K1 145.5(3) . 2_665 ? O25 S1 K1 79.7(3) 2_665 2_665 ? K1 S1 K1 65.84(13) 3_565 2_665 ? O24 S1 K1 38.87(8) . . ? O25 S1 K1 145.5(3) 3_565 . ? O25 S1 K1 79.7(3) . . ? O25 S1 K1 99.8(3) 2_665 . ? K1 S1 K1 65.84(13) 3_565 . ? K1 S1 K1 65.84(13) 2_665 . ? S1 O24 K1 122.2(2) . 3_565 ? S1 O24 K1 122.2(2) . 2_665 ? K1 O24 K1 94.3(3) 3_565 2_665 ? S1 O24 K1 122.2(2) . . ? K1 O24 K1 94.3(3) 3_565 . ? K1 O24 K1 94.3(3) 2_665 . ? S1 O25 La1 139.1(3) . . ? O18 K1 O24 110.3(2) . 10_557 ? O18 K1 O24 110.3(2) . . ? O24 K1 O24 64.4(4) 10_557 . ? O18 K1 O23 147.62(18) . 11_667 ? O24 K1 O23 71.20(16) 10_557 11_667 ? O24 K1 O23 99.5(2) . 11_667 ? O18 K1 O23 147.62(18) . 2_665 ? O24 K1 O23 99.5(2) 10_557 2_665 ? O24 K1 O23 71.20(16) . 2_665 ? O23 K1 O23 54.4(2) 11_667 2_665 ? O18 K1 V8 158.3(3) . 2_665 ? O24 K1 V8 87.83(13) 10_557 2_665 ? O24 K1 V8 87.83(13) . 2_665 ? O23 K1 V8 27.42(11) 11_667 2_665 ? O23 K1 V8 27.42(11) 2_665 2_665 ? O18 K1 V8 30.60(15) . . ? O24 K1 V8 84.61(14) 10_557 . ? O24 K1 V8 84.61(14) . . ? O23 K1 V8 150.30(14) 11_667 . ? O23 K1 V8 150.30(14) 2_665 . ? V8 K1 V8 171.07(19) 2_665 . ? O18 K1 S1 104.92(14) . 10_557 ? O24 K1 S1 18.9(2) 10_557 10_557 ? O24 K1 S1 83.3(3) . 10_557 ? O23 K1 S1 65.52(12) 11_667 10_557 ? O23 K1 S1 107.33(17) 2_665 10_557 ? V8 K1 S1 88.39(10) 2_665 10_557 ? V8 K1 S1 86.00(11) . 10_557 ? O18 K1 S1 104.92(14) . . ? O24 K1 S1 83.3(3) 10_557 . ? O24 K1 S1 18.9(2) . . ? O23 K1 S1 107.33(18) 11_667 . ? O23 K1 S1 65.52(12) 2_665 . ? V8 K1 S1 88.39(10) 2_665 . ? V8 K1 S1 86.00(11) . . ? S1 K1 S1 102.26(16) 10_557 . ? O18 K1 V7 26.76(7) . . ? O24 K1 V7 132.86(18) 10_557 . ? O24 K1 V7 104.55(17) . . ? O23 K1 V7 151.9(2) 11_667 . ? O23 K1 V7 120.91(14) 2_665 . ? V8 K1 V7 139.05(15) 2_665 . ? V8 K1 V7 48.25(7) . . ? S1 K1 V7 131.21(13) 10_557 . ? S1 K1 V7 91.82(7) . . ? O18 K1 V7 26.76(7) . 10_557 ? O24 K1 V7 104.55(17) 10_557 10_557 ? O24 K1 V7 132.86(18) . 10_557 ? O23 K1 V7 120.91(14) 11_667 10_557 ? O23 K1 V7 151.9(2) 2_665 10_557 ? V8 K1 V7 139.05(15) 2_665 10_557 ? V8 K1 V7 48.25(7) . 10_557 ? S1 K1 V7 91.82(7) 10_557 10_557 ? S1 K1 V7 131.21(13) . 10_557 ? V7 K1 V7 47.49(7) . 10_557 ? O18 K1 K1 144.2(3) . 2_665 ? O24 K1 K1 42.87(15) 10_557 2_665 ? O24 K1 K1 42.87(15) . 2_665 ? O23 K1 K1 58.50(18) 11_667 2_665 ? O23 K1 K1 58.50(18) 2_665 2_665 ? V8 K1 K1 57.44(15) 2_665 2_665 ? V8 K1 K1 113.63(16) . 2_665 ? S1 K1 K1 57.08(7) 10_557 2_665 ? S1 K1 K1 57.08(7) . 2_665 ? V7 K1 K1 147.38(13) . 2_665 ? V7 K1 K1 147.38(13) 10_557 2_665 ? O51 C1 O51 115.0(14) 10_556 . ? O51 C1 C2 122.5(7) 10_556 . ? O51 C1 C2 122.5(7) . . ? C3 C2 C3 120.3(11) . 10_556 ? C3 C2 C1 119.8(5) . . ? C3 C2 C1 119.8(5) 10_556 . ? C4 C3 C2 119.9(10) . . ? C3 C4 C5 120.4(9) . . ? N1 C5 C4 0.0(9) 10_556 10_556 ? N1 C5 C4 119.0(10) 10_556 . ? C4 C5 C4 119.0(10) 10_556 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.175 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.156 _database_code_depnum_ccdc_archive 'CCDC 937961' ####################################################################### # # 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H109.50 Ce6 K1.50 Mn3 N3 O172.50 S2 V39' _chemical_formula_weight 6243.56 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 24.707(4) _cell_length_b 24.707(4) _cell_length_c 17.215(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9101(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5525 _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 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5998 _exptl_absorpt_coefficient_mu 3.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.365 _exptl_absorpt_correction_T_max 0.423 _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 65771 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5525 _reflns_number_gt 4125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit-3 50' was used to omit the weak reflections above 50 degree. In the structure, the C1, C2 and C5 atoms of the isolated organic molecule (nicotinic acid) reside on the mirror plane and the C4 and N1 centers exhibit the site-occupancy disorder with 50% for each. All the organic molecules are restrained with the command 'DFIX' so as to get a chemically reasonable structural feature. Moreover, all the atoms are restrained with the commands 'simu' and 'isor' so as to avoid the ADP problems. The V8 is disordered into two parts with the occupancies of 91.6 % and 8.4 % for V8 and V11, respectively. These restrained commands led to a final restraint value of 61. Furthermore, the H atoms on the ligands cannot be added due to the C/N disorder problem. In the final refinement, only four positions of the isolated lattice water molecules can be well confirmed from the residual peaks. Thus, the SQUEEZE program was used to estimate the rest lattice water molecules in the solvent accessible voids. Based on the calculation results, elemental analysis and TG analysis, another eleven H2O molecules were directly included in the final molecular formula. ; 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 0.000 0.500 -0.002 1539.7 108.3 _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^+300.0000P] 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_number_reflns 5525 _refine_ls_number_parameters 395 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.991 _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 Ce1 Ce 0.48920(3) 0.79948(3) 0.52426(5) 0.0400(2) Uani 1 1 d . . . Mn1 Mn 0.66627(10) 0.86981(10) 0.7500 0.0211(5) Uani 1 2 d S . . V3 V 0.51982(11) 0.81189(11) 0.7500 0.0221(5) Uani 1 2 d S . . V4 V 0.58398(8) 0.74976(8) 0.65724(11) 0.0250(4) Uani 1 1 d . . . V5 V 0.60719(8) 0.93371(8) 0.65737(11) 0.0261(4) Uani 1 1 d . . . V6 V 0.75660(9) 0.98682(9) 0.65895(12) 0.0313(5) Uani 1 1 d . . . V7 V 0.73466(9) 0.81580(10) 0.65866(12) 0.0311(5) Uani 1 1 d . . . V8 V 0.66795(9) 0.87046(10) 0.56045(12) 0.0280(5) Uani 0.92 1 d P . . V9 V 0.65203(14) 0.69266(13) 0.7500 0.0340(7) Uani 1 2 d S . . V10 V 0.69802(14) 1.05386(13) 0.7500 0.0353(7) Uani 1 2 d S . . O23 O 0.5553(4) 0.9011(4) 0.7500 0.023(2) Uani 1 2 d S . . O22 O 0.5355(4) 0.7430(5) 0.7500 0.023(2) Uani 1 2 d S . . O21 O 0.6035(3) 0.8449(3) 0.6737(4) 0.0228(15) Uani 1 1 d . . . O20 O 0.4738(3) 0.7933(4) 0.6730(5) 0.0326(19) Uani 1 1 d . . . O19 O 0.5876(4) 0.6832(3) 0.6742(5) 0.0321(18) Uani 1 1 d . . . O18 O 0.6583(3) 0.7915(3) 0.5963(4) 0.0258(16) Uani 1 1 d . . . O17 O 0.5525(4) 0.9081(3) 0.5916(5) 0.0313(18) Uani 1 1 d . . . O16 O 0.6563(4) 0.7907(5) 0.7500 0.023(2) Uani 1 2 d S . . O15 O 0.5302(3) 0.7316(4) 0.5924(5) 0.0308(18) Uani 1 1 d . . . O14 O 0.6289(4) 1.0102(4) 0.6744(5) 0.0345(19) Uani 1 1 d . . . O13 O 0.6770(5) 0.9493(5) 0.7500 0.025(2) Uani 1 2 d S . . O12 O 0.6791(3) 0.9497(3) 0.5967(4) 0.0278(17) Uani 1 1 d . . . O11 O 0.6032(4) 0.8445(4) 0.5078(5) 0.035(2) Uani 0.92 1 d P . . O10 O 0.7503(4) 1.0562(3) 0.6730(5) 0.0348(19) Uani 1 1 d . . . O9 O 0.7264(3) 0.8939(3) 0.6682(5) 0.0285(17) Uani 1 1 d . . . O8 O 0.7094(4) 0.7334(4) 0.6733(5) 0.0346(19) Uani 1 1 d . . . O7 O 0.8081(4) 1.0065(4) 0.5937(5) 0.044(2) Uani 1 1 d . . . O6 O 0.7869(4) 0.8375(4) 0.5936(5) 0.043(2) Uani 1 1 d . . . O5 O 0.7997(5) 0.9973(5) 0.7500 0.034(3) Uani 1 2 d S . . O4 O 0.6431(6) 0.6246(6) 0.7500 0.052(4) Uani 1 2 d S . . O3 O 0.7800(5) 0.8400(5) 0.7500 0.031(3) Uani 1 2 d S . . O2 O 0.7242(4) 0.8929(4) 0.4991(5) 0.041(2) Uani 0.92 1 d P . . O1 O 0.7072(7) 1.1224(5) 0.7500 0.048(3) Uani 1 2 d S . . O5W O 0.3974(4) 0.6950(4) 0.5503(6) 0.050(3) Uani 1 1 d . . . O4W O 0.5086(6) 0.7368(6) 0.4250(7) 0.081(4) Uani 1 1 d . . . O3W O 0.4107(5) 0.8334(5) 0.5571(8) 0.073(3) Uani 1 1 d . . . O2W O 0.5277(5) 0.8854(5) 0.4245(8) 0.076(4) Uani 1 1 d . . . O1W O 0.4117(7) 0.7728(7) 0.4150(10) 0.111(5) Uani 1 1 d . . . S1 S 0.3333 0.6667 0.5789(4) 0.0402(13) Uani 1 3 d S . . O25 O 0.3333 0.6667 0.6629(12) 0.073(6) Uani 1 3 d S . . OW2 O 0.0892(6) 0.1446(5) 0.4846(7) 0.073(3) Uani 1 1 d . . . OW1 O 0.3405(6) 0.3541(6) 0.4520(7) 0.084(4) Uani 1 1 d . . . O51 O 0.0997(7) 0.1628(8) 0.3157(8) 0.120(5) Uani 1 1 d DU . . C1 C 0.1174(11) 0.1926(9) 0.2500 0.089(6) Uani 1 2 d SDU . . C2 C 0.1584(10) 0.2602(8) 0.2500 0.089(5) Uani 1 2 d SDU . . C4 C 0.2169(9) 0.3569(8) 0.3204(6) 0.115(5) Uani 0.50 1 d PDU . . N1 N 0.2169(9) 0.3569(8) 0.3204(6) 0.115(5) Uani 0.50 1 d P . . C3 C 0.1773(9) 0.2924(8) 0.3209(7) 0.100(5) Uani 1 1 d DU . . C5 C 0.2364(16) 0.3899(9) 0.2500 0.130(7) Uani 1 2 d SDU . . OW3 O 0.1130(6) 0.3905(6) 0.4512(8) 0.087(4) Uiso 1 1 d . . . OW4 O 0.0281(14) 0.0491(13) 0.2500 0.056(7) Uiso 0.50 2 d SP . . V11 V 0.8204(8) 0.9312(8) 0.7500 0.032(4) Uiso 0.17 2 d SP . . O53 O 0.8836(19) 0.9562(19) 0.696(3) 0.024(9) Uiso 0.17 1 d P . . O6W O 0.0000 0.0000 0.381(3) 0.085(13) Uiso 0.50 3 d SP . . K1 K 0.3586(6) 0.7714(6) 0.7500 0.072(3) Uiso 0.50 2 d SP . . 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 0.0348(4) 0.0403(4) 0.0400(4) 0.0001(3) -0.0083(3) 0.0152(3) Mn1 0.0184(11) 0.0232(11) 0.0204(12) 0.000 0.000 0.0094(9) V3 0.0162(12) 0.0211(13) 0.0268(14) 0.000 0.000 0.0077(10) V4 0.0231(9) 0.0281(9) 0.0244(10) -0.0034(8) -0.0016(8) 0.0132(8) V5 0.0248(9) 0.0252(9) 0.0241(10) 0.0028(8) -0.0011(8) 0.0093(8) V6 0.0242(10) 0.0308(10) 0.0263(11) 0.0021(8) 0.0045(8) 0.0043(8) V7 0.0270(10) 0.0443(12) 0.0267(11) 0.0018(9) 0.0048(8) 0.0213(9) V8 0.0273(11) 0.0335(11) 0.0200(11) -0.0002(9) 0.0008(8) 0.0129(9) V9 0.0383(16) 0.0331(15) 0.0387(18) 0.000 0.000 0.0240(14) V10 0.0376(16) 0.0233(14) 0.0355(17) 0.000 0.000 0.0082(12) O23 0.022(5) 0.020(5) 0.025(6) 0.000 0.000 0.009(4) O22 0.018(5) 0.021(5) 0.028(6) 0.000 0.000 0.008(4) O21 0.018(3) 0.025(4) 0.024(4) 0.000(3) -0.002(3) 0.009(3) O20 0.026(4) 0.030(4) 0.044(5) -0.005(4) -0.009(4) 0.015(3) O19 0.034(4) 0.029(4) 0.036(5) -0.006(3) -0.002(4) 0.017(4) O18 0.025(4) 0.034(4) 0.021(4) -0.003(3) 0.001(3) 0.017(3) O17 0.034(4) 0.031(4) 0.030(5) 0.002(3) -0.003(4) 0.016(4) O16 0.019(5) 0.028(5) 0.023(6) 0.000 0.000 0.012(4) O15 0.029(4) 0.033(4) 0.030(5) -0.006(4) -0.005(3) 0.016(3) O14 0.040(5) 0.028(4) 0.036(5) 0.003(4) -0.001(4) 0.018(4) O13 0.022(5) 0.020(5) 0.028(6) 0.000 0.000 0.007(4) O12 0.031(4) 0.026(4) 0.020(4) 0.005(3) 0.004(3) 0.010(3) O11 0.039(5) 0.040(5) 0.022(5) -0.001(4) -0.008(4) 0.016(4) O10 0.035(4) 0.023(4) 0.033(5) 0.004(3) -0.003(4) 0.005(3) O9 0.019(4) 0.030(4) 0.033(5) 0.001(3) 0.006(3) 0.009(3) O8 0.031(4) 0.039(5) 0.042(5) -0.003(4) 0.002(4) 0.024(4) O7 0.037(5) 0.055(6) 0.027(5) 0.001(4) 0.008(4) 0.012(4) O6 0.035(5) 0.065(6) 0.036(5) 0.003(4) 0.007(4) 0.029(5) O5 0.021(6) 0.032(6) 0.032(7) 0.000 0.000 0.001(5) O4 0.056(8) 0.039(7) 0.073(10) 0.000 0.000 0.033(7) O3 0.023(5) 0.041(6) 0.029(6) 0.000 0.000 0.015(5) O2 0.037(5) 0.047(6) 0.030(5) 0.004(4) 0.010(4) 0.015(4) O1 0.064(9) 0.021(6) 0.054(9) 0.000 0.000 0.017(6) O5W 0.034(5) 0.040(5) 0.077(7) -0.002(5) 0.001(5) 0.019(4) O4W 0.083(9) 0.099(10) 0.056(8) -0.029(7) -0.014(6) 0.044(8) O3W 0.049(6) 0.070(7) 0.105(10) 0.002(7) -0.007(6) 0.034(6) O2W 0.065(7) 0.069(7) 0.076(9) 0.019(6) -0.011(6) 0.020(6) O1W 0.089(10) 0.113(12) 0.108(12) 0.002(10) -0.050(9) 0.035(9) S1 0.0324(17) 0.0324(17) 0.056(4) 0.000 0.000 0.0162(8) O25 0.081(9) 0.081(9) 0.057(13) 0.000 0.000 0.040(4) OW2 0.077(8) 0.072(7) 0.069(8) -0.028(6) -0.012(6) 0.036(6) OW1 0.109(10) 0.076(8) 0.068(9) -0.018(7) 0.016(8) 0.048(8) O51 0.110(8) 0.160(10) 0.117(9) 0.008(8) 0.002(7) 0.088(7) C1 0.079(8) 0.112(9) 0.108(10) 0.000 0.000 0.071(7) C2 0.077(8) 0.120(9) 0.114(10) 0.000 0.000 0.082(7) C4 0.103(7) 0.134(8) 0.134(8) -0.008(6) 0.001(6) 0.078(6) N1 0.103(7) 0.134(8) 0.134(8) -0.008(6) 0.001(6) 0.078(6) C3 0.086(7) 0.126(8) 0.119(8) -0.009(6) 0.001(5) 0.075(6) C5 0.119(9) 0.136(10) 0.143(10) 0.000 0.000 0.071(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 Ce1 O11 2.474(9) . ? Ce1 O5W 2.481(9) . ? Ce1 O4W 2.507(12) . ? Ce1 O2W 2.518(11) . ? Ce1 O1W 2.526(13) . ? Ce1 O3W 2.532(11) . ? Ce1 O20 2.582(9) . ? Ce1 O17 2.608(8) . ? Ce1 O15 2.630(8) . ? Mn1 O16 1.845(10) . ? Mn1 O13 1.846(10) . ? Mn1 O21 1.886(7) . ? Mn1 O21 1.886(7) 10_557 ? Mn1 O9 1.913(7) 10_557 ? Mn1 O9 1.913(7) . ? Mn1 V6 3.057(3) 10_557 ? Mn1 V6 3.057(3) . ? Mn1 V7 3.060(3) . ? Mn1 V7 3.060(3) 10_557 ? Mn1 V4 3.074(3) . ? Mn1 V4 3.074(3) 10_557 ? V3 O20 1.655(8) . ? V3 O20 1.655(8) 10_557 ? V3 O23 1.921(10) . ? V3 O22 1.925(10) . ? V3 O21 2.231(7) 10_557 ? V3 O21 2.231(7) . ? V3 K1 3.590(12) . ? V3 K1 3.687(12) 3_565 ? V4 O15 1.617(8) . ? V4 O19 1.714(8) . ? V4 O18 1.908(7) . ? V4 O22 1.952(6) . ? V4 O21 2.169(7) . ? V4 O16 2.227(7) . ? V4 K1 4.034(11) 3_565 ? V5 O17 1.628(8) . ? V5 O14 1.711(8) . ? V5 O12 1.924(8) . ? V5 O23 1.950(6) . ? V5 O21 2.169(7) . ? V5 O13 2.236(7) . ? V5 V10 3.119(3) . ? V6 O7 1.580(8) . ? V6 O10 1.814(8) . ? V6 O5 1.839(6) . ? V6 O12 1.975(8) . ? V6 O9 2.035(8) . ? V6 O13 2.316(7) . ? V6 V11 3.001(15) . ? V6 V8 3.105(3) . ? V6 V10 3.113(3) . ? V7 O6 1.586(9) . ? V7 O8 1.823(8) . ? V7 O3 1.849(6) . ? V7 O18 1.986(8) . ? V7 O9 2.046(8) . ? V7 O16 2.324(7) . ? V7 V11 3.008(15) . ? V7 V8 3.102(3) . ? V7 V9 3.112(3) . ? V8 O2 1.607(9) . ? V8 O11 1.663(9) . ? V8 O12 1.938(8) . ? V8 O18 1.943(8) . ? V8 O9 2.241(8) . ? V8 O21 2.394(7) . ? V9 O4 1.584(12) . ? V9 O8 1.827(9) 10_557 ? V9 O8 1.827(9) . ? V9 O19 1.981(8) . ? V9 O19 1.981(8) 10_557 ? V9 O16 2.370(10) . ? V9 V7 3.112(3) 10_557 ? V10 O1 1.591(12) . ? V10 O10 1.831(9) 10_557 ? V10 O10 1.831(9) . ? V10 O14 1.983(9) . ? V10 O14 1.983(9) 10_557 ? V10 O13 2.367(10) . ? V10 V6 3.113(3) 10_557 ? V10 V5 3.119(3) 10_557 ? O23 V5 1.950(6) 10_557 ? O22 V4 1.952(6) 10_557 ? O22 K1 2.807(15) 3_565 ? O20 K1 2.935(13) . ? O16 V4 2.227(7) 10_557 ? O16 V7 2.324(7) 10_557 ? O13 V5 2.236(7) 10_557 ? O13 V6 2.316(7) 10_557 ? O9 V11 2.468(16) . ? O5 V6 1.839(6) 10_557 ? O5 V11 1.94(2) . ? O3 V7 1.849(6) 10_557 ? O3 V11 1.95(2) . ? O5W S1 1.459(9) . ? S1 O25 1.45(2) . ? S1 O5W 1.459(9) 2_665 ? S1 O5W 1.459(9) 3_565 ? S1 K1 3.761(9) . ? S1 K1 3.761(9) 2_665 ? S1 K1 3.761(9) 3_565 ? O25 K1 2.779(15) . ? O25 K1 2.779(15) 2_665 ? O25 K1 2.779(15) 3_565 ? O51 C1 1.300(9) . ? C1 O51 1.300(9) 10_556 ? C1 C2 1.459(10) . ? C2 C3 1.403(10) . ? C2 C3 1.403(10) 10_556 ? C4 C3 1.393(10) . ? C4 C5 1.404(10) . ? C5 N1 1.404(10) 10_556 ? C5 C4 1.404(10) 10_556 ? V11 O53 1.65(4) 10_557 ? V11 O53 1.65(4) . ? V11 O9 2.468(16) 10_557 ? V11 V6 3.001(15) 10_557 ? V11 V7 3.008(15) 10_557 ? K1 O25 2.779(15) 10_557 ? K1 O22 2.807(15) 2_665 ? K1 O20 2.935(13) 10_557 ? K1 V3 3.687(12) 2_665 ? K1 S1 3.761(9) 10_557 ? K1 V4 4.034(11) 2_665 ? K1 V4 4.034(11) 11_667 ? K1 K1 4.05(2) 2_665 ? 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 O11 Ce1 O5W 137.1(3) . . ? O11 Ce1 O4W 70.9(4) . . ? O5W Ce1 O4W 80.7(4) . . ? O11 Ce1 O2W 71.1(3) . . ? O5W Ce1 O2W 139.8(4) . . ? O4W Ce1 O2W 87.0(5) . . ? O11 Ce1 O1W 125.2(5) . . ? O5W Ce1 O1W 71.5(4) . . ? O4W Ce1 O1W 71.7(5) . . ? O2W Ce1 O1W 68.3(4) . . ? O11 Ce1 O3W 139.9(3) . . ? O5W Ce1 O3W 81.4(3) . . ? O4W Ce1 O3W 140.4(4) . . ? O2W Ce1 O3W 84.4(4) . . ? O1W Ce1 O3W 69.3(5) . . ? O11 Ce1 O20 104.0(3) . . ? O5W Ce1 O20 74.2(3) . . ? O4W Ce1 O20 135.0(4) . . ? O2W Ce1 O20 135.1(4) . . ? O1W Ce1 O20 130.8(4) . . ? O3W Ce1 O20 71.6(3) . . ? O11 Ce1 O17 68.0(3) . . ? O5W Ce1 O17 139.2(3) . . ? O4W Ce1 O17 137.5(3) . . ? O2W Ce1 O17 69.9(3) . . ? O1W Ce1 O17 125.9(4) . . ? O3W Ce1 O17 74.0(3) . . ? O20 Ce1 O17 67.3(2) . . ? O11 Ce1 O15 67.9(3) . . ? O5W Ce1 O15 72.5(3) . . ? O4W Ce1 O15 69.9(4) . . ? O2W Ce1 O15 137.6(3) . . ? O1W Ce1 O15 130.5(4) . . ? O3W Ce1 O15 135.6(3) . . ? O20 Ce1 O15 67.2(2) . . ? O17 Ce1 O15 103.5(2) . . ? O16 Mn1 O13 179.5(4) . . ? O16 Mn1 O21 90.1(3) . . ? O13 Mn1 O21 90.3(3) . . ? O16 Mn1 O21 90.1(3) . 10_557 ? O13 Mn1 O21 90.3(3) . 10_557 ? O21 Mn1 O21 88.3(4) . 10_557 ? O16 Mn1 O9 90.0(3) . 10_557 ? O13 Mn1 O9 89.6(3) . 10_557 ? O21 Mn1 O9 176.7(3) . 10_557 ? O21 Mn1 O9 88.4(3) 10_557 10_557 ? O16 Mn1 O9 90.0(3) . . ? O13 Mn1 O9 89.6(3) . . ? O21 Mn1 O9 88.4(3) . . ? O21 Mn1 O9 176.7(3) 10_557 . ? O9 Mn1 O9 94.8(5) 10_557 . ? O16 Mn1 V6 130.5(2) . 10_557 ? O13 Mn1 V6 49.1(2) . 10_557 ? O21 Mn1 V6 139.3(2) . 10_557 ? O21 Mn1 V6 92.5(2) 10_557 10_557 ? O9 Mn1 V6 40.7(2) 10_557 10_557 ? O9 Mn1 V6 89.8(2) . 10_557 ? O16 Mn1 V6 130.5(2) . . ? O13 Mn1 V6 49.1(2) . . ? O21 Mn1 V6 92.5(2) . . ? O21 Mn1 V6 139.3(2) 10_557 . ? O9 Mn1 V6 89.8(2) 10_557 . ? O9 Mn1 V6 40.7(2) . . ? V6 Mn1 V6 61.70(9) 10_557 . ? O16 Mn1 V7 49.3(2) . . ? O13 Mn1 V7 130.3(2) . . ? O21 Mn1 V7 92.5(2) . . ? O21 Mn1 V7 139.4(2) 10_557 . ? O9 Mn1 V7 90.1(2) 10_557 . ? O9 Mn1 V7 41.0(2) . . ? V6 Mn1 V7 112.01(9) 10_557 . ? V6 Mn1 V7 81.24(7) . . ? O16 Mn1 V7 49.3(2) . 10_557 ? O13 Mn1 V7 130.3(2) . 10_557 ? O21 Mn1 V7 139.4(2) . 10_557 ? O21 Mn1 V7 92.5(2) 10_557 10_557 ? O9 Mn1 V7 41.0(2) 10_557 10_557 ? O9 Mn1 V7 90.1(2) . 10_557 ? V6 Mn1 V7 81.24(7) 10_557 10_557 ? V6 Mn1 V7 112.01(9) . 10_557 ? V7 Mn1 V7 61.85(9) . 10_557 ? O16 Mn1 V4 45.9(2) . . ? O13 Mn1 V4 134.5(2) . . ? O21 Mn1 V4 44.3(2) . . ? O21 Mn1 V4 90.4(2) 10_557 . ? O9 Mn1 V4 135.9(2) 10_557 . ? O9 Mn1 V4 87.3(2) . . ? V6 Mn1 V4 175.40(10) 10_557 . ? V6 Mn1 V4 117.65(5) . . ? V7 Mn1 V4 63.60(6) . . ? V7 Mn1 V4 95.11(8) 10_557 . ? O16 Mn1 V4 45.9(2) . 10_557 ? O13 Mn1 V4 134.5(2) . 10_557 ? O21 Mn1 V4 90.4(2) . 10_557 ? O21 Mn1 V4 44.3(2) 10_557 10_557 ? O9 Mn1 V4 87.3(2) 10_557 10_557 ? O9 Mn1 V4 135.9(2) . 10_557 ? V6 Mn1 V4 117.65(5) 10_557 10_557 ? V6 Mn1 V4 175.40(10) . 10_557 ? V7 Mn1 V4 95.11(8) . 10_557 ? V7 Mn1 V4 63.60(6) 10_557 10_557 ? V4 Mn1 V4 62.59(8) . 10_557 ? O20 V3 O20 106.5(6) . 10_557 ? O20 V3 O23 100.0(3) . . ? O20 V3 O23 100.0(3) 10_557 . ? O20 V3 O22 99.7(3) . . ? O20 V3 O22 99.7(3) 10_557 . ? O23 V3 O22 146.7(4) . . ? O20 V3 O21 162.8(4) . 10_557 ? O20 V3 O21 90.7(3) 10_557 10_557 ? O23 V3 O21 76.9(3) . 10_557 ? O22 V3 O21 76.3(3) . 10_557 ? O20 V3 O21 90.7(3) . . ? O20 V3 O21 162.8(4) 10_557 . ? O23 V3 O21 76.9(3) . . ? O22 V3 O21 76.3(3) . . ? O21 V3 O21 72.2(4) 10_557 . ? O20 V3 Mn1 126.8(3) . . ? O20 V3 Mn1 126.8(3) 10_557 . ? O23 V3 Mn1 73.6(3) . . ? O22 V3 Mn1 73.1(3) . . ? O21 V3 Mn1 36.08(18) 10_557 . ? O21 V3 Mn1 36.08(18) . . ? O20 V3 K1 53.8(3) . . ? O20 V3 K1 53.8(3) 10_557 . ? O23 V3 K1 97.2(4) . . ? O22 V3 K1 116.1(4) . . ? O21 V3 K1 142.95(19) 10_557 . ? O21 V3 K1 142.95(19) . . ? Mn1 V3 K1 170.8(2) . . ? O20 V3 K1 71.5(3) . 3_565 ? O20 V3 K1 71.5(3) 10_557 3_565 ? O23 V3 K1 164.9(4) . 3_565 ? O22 V3 K1 48.4(3) . 3_565 ? O21 V3 K1 114.9(2) 10_557 3_565 ? O21 V3 K1 114.9(2) . 3_565 ? Mn1 V3 K1 121.5(2) . 3_565 ? K1 V3 K1 67.7(4) . 3_565 ? O15 V4 O19 106.3(4) . . ? O15 V4 O18 101.8(4) . . ? O19 V4 O18 96.6(4) . . ? O15 V4 O22 99.1(4) . . ? O19 V4 O22 95.9(4) . . ? O18 V4 O22 151.5(4) . . ? O15 V4 O21 95.6(3) . . ? O19 V4 O21 157.9(3) . . ? O18 V4 O21 81.6(3) . . ? O22 V4 O21 77.3(3) . . ? O15 V4 O16 169.2(4) . . ? O19 V4 O16 84.2(4) . . ? O18 V4 O16 79.2(3) . . ? O22 V4 O16 76.8(3) . . ? O21 V4 O16 73.8(3) . . ? O15 V4 Mn1 133.0(3) . . ? O19 V4 Mn1 120.7(3) . . ? O18 V4 Mn1 76.7(2) . . ? O22 V4 Mn1 74.9(3) . . ? O21 V4 Mn1 37.37(19) . . ? O16 V4 Mn1 36.5(3) . . ? O15 V4 K1 69.3(3) . 3_565 ? O19 V4 K1 80.6(3) . 3_565 ? O18 V4 K1 169.2(3) . 3_565 ? O22 V4 K1 39.2(3) . 3_565 ? O21 V4 K1 105.0(3) . 3_565 ? O16 V4 K1 110.8(2) . 3_565 ? Mn1 V4 K1 113.74(13) . 3_565 ? O17 V5 O14 106.8(4) . . ? O17 V5 O12 101.8(4) . . ? O14 V5 O12 96.8(4) . . ? O17 V5 O23 99.3(4) . . ? O14 V5 O23 95.5(4) . . ? O12 V5 O23 151.3(4) . . ? O17 V5 O21 95.2(3) . . ? O14 V5 O21 157.8(3) . . ? O12 V5 O21 81.1(3) . . ? O23 V5 O21 77.8(3) . . ? O17 V5 O13 168.9(4) . . ? O14 V5 O13 84.2(4) . . ? O12 V5 O13 78.3(3) . . ? O23 V5 O13 77.2(3) . . ? O21 V5 O13 73.8(3) . . ? O17 V5 Mn1 132.5(3) . . ? O14 V5 Mn1 120.7(3) . . ? O12 V5 Mn1 76.1(2) . . ? O23 V5 Mn1 75.3(3) . . ? O21 V5 Mn1 37.31(19) . . ? O13 V5 Mn1 36.5(3) . . ? O17 V5 V10 141.9(3) . . ? O14 V5 V10 35.2(3) . . ? O12 V5 V10 86.0(2) . . ? O23 V5 V10 89.2(3) . . ? O21 V5 V10 122.9(2) . . ? O13 V5 V10 49.1(3) . . ? Mn1 V5 V10 85.60(8) . . ? O7 V6 O10 103.9(4) . . ? O7 V6 O5 104.1(4) . . ? O10 V6 O5 94.0(5) . . ? O7 V6 O12 101.6(4) . . ? O10 V6 O12 89.4(3) . . ? O5 V6 O12 152.4(4) . . ? O7 V6 O9 100.8(4) . . ? O10 V6 O9 154.1(3) . . ? O5 V6 O9 87.2(4) . . ? O12 V6 O9 78.1(3) . . ? O7 V6 O13 175.0(4) . . ? O10 V6 O13 80.3(4) . . ? O5 V6 O13 78.2(3) . . ? O12 V6 O13 75.5(3) . . ? O9 V6 O13 74.7(3) . . ? O7 V6 V11 89.2(4) . . ? O10 V6 V11 132.6(4) . . ? O5 V6 V11 38.7(4) . . ? O12 V6 V11 132.8(4) . . ? O9 V6 V11 54.7(4) . . ? O13 V6 V11 89.9(3) . . ? O7 V6 Mn1 138.6(4) . . ? O10 V6 Mn1 117.3(3) . . ? O5 V6 Mn1 78.1(3) . . ? O12 V6 Mn1 76.0(2) . . ? O9 V6 Mn1 37.8(2) . . ? O13 V6 Mn1 37.1(3) . . ? V11 V6 Mn1 66.5(3) . . ? O7 V6 V8 89.0(3) . . ? O10 V6 V8 126.4(3) . . ? O5 V6 V8 133.3(4) . . ? O12 V6 V8 37.1(2) . . ? O9 V6 V8 46.1(2) . . ? O13 V6 V8 86.2(2) . . ? V11 V6 V8 98.6(3) . . ? Mn1 V6 V8 63.95(6) . . ? O7 V6 V10 135.3(4) . . ? O10 V6 V10 31.5(3) . . ? O5 V6 V10 83.5(4) . . ? O12 V6 V10 85.4(2) . . ? O9 V6 V10 123.7(2) . . ? O13 V6 V10 49.0(3) . . ? V11 V6 V10 118.13(19) . . ? Mn1 V6 V10 86.05(8) . . ? V8 V6 V10 117.85(9) . . ? O6 V7 O8 103.9(4) . . ? O6 V7 O3 103.4(4) . . ? O8 V7 O3 93.3(4) . . ? O6 V7 O18 102.2(4) . . ? O8 V7 O18 89.7(3) . . ? O3 V7 O18 152.7(4) . . ? O6 V7 O9 100.8(4) . . ? O8 V7 O9 154.4(3) . . ? O3 V7 O9 87.5(4) . . ? O18 V7 O9 78.5(3) . . ? O6 V7 O16 175.1(4) . . ? O8 V7 O16 80.4(4) . . ? O3 V7 O16 78.5(3) . . ? O18 V7 O16 75.3(3) . . ? O9 V7 O16 74.6(3) . . ? O6 V7 V11 88.9(4) . . ? O8 V7 V11 132.1(4) . . ? O3 V7 V11 39.0(4) . . ? O18 V7 V11 133.0(4) . . ? O9 V7 V11 54.5(4) . . ? O16 V7 V11 89.9(3) . . ? O6 V7 Mn1 138.5(4) . . ? O8 V7 Mn1 117.4(3) . . ? O3 V7 Mn1 78.4(3) . . ? O18 V7 Mn1 76.2(2) . . ? O9 V7 Mn1 37.8(2) . . ? O16 V7 Mn1 37.0(3) . . ? V11 V7 Mn1 66.4(3) . . ? O6 V7 V8 89.4(3) . . ? O8 V7 V8 127.0(3) . . ? O3 V7 V8 133.7(4) . . ? O18 V7 V8 37.4(2) . . ? O9 V7 V8 46.2(2) . . ? O16 V7 V8 86.1(2) . . ? V11 V7 V8 98.5(3) . . ? Mn1 V7 V8 63.95(6) . . ? O6 V7 V9 135.4(4) . . ? O8 V7 V9 31.6(3) . . ? O3 V7 V9 83.2(3) . . ? O18 V7 V9 85.3(2) . . ? O9 V7 V9 123.7(2) . . ? O16 V7 V9 49.1(3) . . ? V11 V7 V9 117.98(19) . . ? Mn1 V7 V9 86.06(8) . . ? V8 V7 V9 117.99(9) . . ? O2 V8 O11 105.9(5) . . ? O2 V8 O12 101.6(4) . . ? O11 V8 O12 100.9(4) . . ? O2 V8 O18 101.9(4) . . ? O11 V8 O18 100.1(4) . . ? O12 V8 O18 142.7(3) . . ? O2 V8 O9 96.9(4) . . ? O11 V8 O9 157.2(4) . . ? O12 V8 O9 74.0(3) . . ? O18 V8 O9 74.7(3) . . ? O2 V8 O21 166.5(4) . . ? O11 V8 O21 87.6(4) . . ? O12 V8 O21 75.2(3) . . ? O18 V8 O21 75.2(3) . . ? O9 V8 O21 69.6(2) . . ? O2 V8 V7 87.3(4) . . ? O11 V8 V7 138.4(3) . . ? O12 V8 V7 115.2(2) . . ? O18 V8 V7 38.3(2) . . ? O9 V8 V7 41.2(2) . . ? O21 V8 V7 82.50(18) . . ? O2 V8 V6 87.2(4) . . ? O11 V8 V6 138.7(3) . . ? O12 V8 V6 37.9(2) . . ? O18 V8 V6 115.6(2) . . ? O9 V8 V6 40.9(2) . . ? O21 V8 V6 82.42(18) . . ? V7 V8 V6 79.81(7) . . ? O4 V9 O8 104.0(4) . 10_557 ? O4 V9 O8 104.0(4) . . ? O8 V9 O8 92.5(5) 10_557 . ? O4 V9 O19 101.5(4) . . ? O8 V9 O19 153.8(4) 10_557 . ? O8 V9 O19 86.9(3) . . ? O4 V9 O19 101.5(4) . 10_557 ? O8 V9 O19 86.9(3) 10_557 10_557 ? O8 V9 O19 153.8(4) . 10_557 ? O19 V9 O19 82.4(5) . 10_557 ? O4 V9 O16 175.3(6) . . ? O8 V9 O16 79.1(3) 10_557 . ? O8 V9 O16 79.1(3) . . ? O19 V9 O16 75.1(3) . . ? O19 V9 O16 75.1(3) 10_557 . ? O4 V9 V7 135.5(4) . 10_557 ? O8 V9 V7 31.5(2) 10_557 10_557 ? O8 V9 V7 83.0(3) . 10_557 ? O19 V9 V7 122.9(2) . 10_557 ? O19 V9 V7 83.0(2) 10_557 10_557 ? O16 V9 V7 47.84(18) . 10_557 ? O4 V9 V7 135.5(4) . . ? O8 V9 V7 83.0(3) 10_557 . ? O8 V9 V7 31.5(2) . . ? O19 V9 V7 83.0(2) . . ? O19 V9 V7 122.9(2) 10_557 . ? O16 V9 V7 47.84(18) . . ? V7 V9 V7 60.70(10) 10_557 . ? O1 V10 O10 104.0(4) . 10_557 ? O1 V10 O10 104.0(4) . . ? O10 V10 O10 92.7(5) 10_557 . ? O1 V10 O14 101.9(5) . . ? O10 V10 O14 153.4(4) 10_557 . ? O10 V10 O14 86.8(3) . . ? O1 V10 O14 101.9(5) . 10_557 ? O10 V10 O14 86.8(3) 10_557 10_557 ? O10 V10 O14 153.4(4) . 10_557 ? O14 V10 O14 82.1(5) . 10_557 ? O1 V10 O13 176.2(6) . . ? O10 V10 O13 78.5(3) 10_557 . ? O10 V10 O13 78.5(3) . . ? O14 V10 O13 75.3(3) . . ? O14 V10 O13 75.3(3) 10_557 . ? O1 V10 V6 135.1(4) . 10_557 ? O10 V10 V6 31.2(2) 10_557 10_557 ? O10 V10 V6 82.7(3) . 10_557 ? O14 V10 V6 122.9(2) . 10_557 ? O14 V10 V6 83.2(2) 10_557 10_557 ? O13 V10 V6 47.63(19) . 10_557 ? O1 V10 V6 135.1(4) . . ? O10 V10 V6 82.7(3) 10_557 . ? O10 V10 V6 31.2(2) . . ? O14 V10 V6 83.2(2) . . ? O14 V10 V6 122.9(2) 10_557 . ? O13 V10 V6 47.63(19) . . ? V6 V10 V6 60.46(10) 10_557 . ? O1 V10 V5 131.7(4) . . ? O10 V10 V5 124.1(3) 10_557 . ? O10 V10 V5 79.7(2) . . ? O14 V10 V5 29.8(2) . . ? O14 V10 V5 78.7(2) 10_557 . ? O13 V10 V5 45.60(18) . . ? V6 V10 V5 93.19(9) 10_557 . ? V6 V10 V5 62.67(7) . . ? O1 V10 V5 131.7(4) . 10_557 ? O10 V10 V5 79.7(2) 10_557 10_557 ? O10 V10 V5 124.1(3) . 10_557 ? O14 V10 V5 78.7(2) . 10_557 ? O14 V10 V5 29.8(2) 10_557 10_557 ? O13 V10 V5 45.60(18) . 10_557 ? V6 V10 V5 62.67(7) 10_557 10_557 ? V6 V10 V5 93.19(9) . 10_557 ? V5 V10 V5 61.49(9) . 10_557 ? V3 O23 V5 107.6(3) . 10_557 ? V3 O23 V5 107.6(3) . . ? V5 O23 V5 109.7(5) 10_557 . ? V3 O22 V4 108.1(3) . 10_557 ? V3 O22 V4 108.1(3) . . ? V4 O22 V4 109.8(5) 10_557 . ? V3 O22 K1 100.7(5) . 3_565 ? V4 O22 K1 114.7(3) 10_557 3_565 ? V4 O22 K1 114.7(3) . 3_565 ? Mn1 O21 V5 98.5(3) . . ? Mn1 O21 V4 98.4(3) . . ? V5 O21 V4 162.5(4) . . ? Mn1 O21 V3 99.8(3) . . ? V5 O21 V3 90.5(3) . . ? V4 O21 V3 91.0(3) . . ? Mn1 O21 V8 98.7(3) . . ? V5 O21 V8 86.6(3) . . ? V4 O21 V8 86.4(3) . . ? V3 O21 V8 161.6(3) . . ? V3 O20 Ce1 135.8(4) . . ? V3 O20 K1 99.1(4) . . ? Ce1 O20 K1 124.0(3) . . ? V4 O19 V9 115.0(4) . . ? V4 O18 V8 108.7(3) . . ? V4 O18 V7 112.2(4) . . ? V8 O18 V7 104.3(3) . . ? V5 O17 Ce1 131.5(4) . . ? Mn1 O16 V4 97.6(3) . . ? Mn1 O16 V4 97.6(3) . 10_557 ? V4 O16 V4 91.6(4) . 10_557 ? Mn1 O16 V7 93.7(3) . 10_557 ? V4 O16 V7 168.1(5) . 10_557 ? V4 O16 V7 90.47(9) 10_557 10_557 ? Mn1 O16 V7 93.7(3) . . ? V4 O16 V7 90.47(9) . . ? V4 O16 V7 168.1(5) 10_557 . ? V7 O16 V7 85.1(3) 10_557 . ? Mn1 O16 V9 175.6(5) . . ? V4 O16 V9 85.4(3) . . ? V4 O16 V9 85.4(3) 10_557 . ? V7 O16 V9 83.0(3) 10_557 . ? V7 O16 V9 83.0(3) . . ? V4 O15 Ce1 131.0(4) . . ? V5 O14 V10 115.0(4) . . ? Mn1 O13 V5 97.4(3) . 10_557 ? Mn1 O13 V5 97.4(3) . . ? V5 O13 V5 91.0(4) 10_557 . ? Mn1 O13 V6 93.9(4) . 10_557 ? V5 O13 V6 90.79(9) 10_557 10_557 ? V5 O13 V6 168.3(5) . 10_557 ? Mn1 O13 V6 93.9(4) . . ? V5 O13 V6 168.3(5) 10_557 . ? V5 O13 V6 90.79(9) . . ? V6 O13 V6 85.2(3) 10_557 . ? Mn1 O13 V10 176.2(6) . . ? V5 O13 V10 85.3(3) 10_557 . ? V5 O13 V10 85.3(3) . . ? V6 O13 V10 83.3(3) 10_557 . ? V6 O13 V10 83.3(3) . . ? V5 O12 V8 108.5(3) . . ? V5 O12 V6 112.5(4) . . ? V8 O12 V6 105.0(4) . . ? V8 O11 Ce1 140.4(5) . . ? V6 O10 V10 117.3(4) . . ? Mn1 O9 V6 101.4(3) . . ? Mn1 O9 V7 101.2(3) . . ? V6 O9 V7 154.7(4) . . ? Mn1 O9 V8 103.3(3) . . ? V6 O9 V8 93.0(3) . . ? V7 O9 V8 92.6(3) . . ? Mn1 O9 V11 97.8(4) . . ? V6 O9 V11 83.0(5) . . ? V7 O9 V11 83.0(5) . . ? V8 O9 V11 158.9(4) . . ? V7 O8 V9 116.9(4) . . ? V6 O5 V6 117.0(6) . 10_557 ? V6 O5 V11 105.0(5) . . ? V6 O5 V11 105.0(5) 10_557 . ? V7 O3 V7 116.6(6) . 10_557 ? V7 O3 V11 104.5(5) . . ? V7 O3 V11 104.5(5) 10_557 . ? S1 O5W Ce1 140.2(5) . . ? O25 S1 O5W 109.7(5) . 2_665 ? O25 S1 O5W 109.7(5) . 3_565 ? O5W S1 O5W 109.2(5) 2_665 3_565 ? O25 S1 O5W 109.7(5) . . ? O5W S1 O5W 109.2(5) 2_665 . ? O5W S1 O5W 109.2(5) 3_565 . ? O25 S1 K1 38.46(15) . . ? O5W S1 K1 79.2(5) 2_665 . ? O5W S1 K1 144.4(5) 3_565 . ? O5W S1 K1 99.6(5) . . ? O25 S1 K1 38.46(16) . 2_665 ? O5W S1 K1 99.6(5) 2_665 2_665 ? O5W S1 K1 79.2(5) 3_565 2_665 ? O5W S1 K1 144.4(5) . 2_665 ? K1 S1 K1 65.2(2) . 2_665 ? O25 S1 K1 38.46(15) . 3_565 ? O5W S1 K1 144.4(5) 2_665 3_565 ? O5W S1 K1 99.6(5) 3_565 3_565 ? O5W S1 K1 79.2(5) . 3_565 ? K1 S1 K1 65.2(2) . 3_565 ? K1 S1 K1 65.2(2) 2_665 3_565 ? S1 O25 K1 122.7(4) . . ? S1 O25 K1 122.7(4) . 2_665 ? K1 O25 K1 93.6(5) . 2_665 ? S1 O25 K1 122.7(4) . 3_565 ? K1 O25 K1 93.6(5) . 3_565 ? K1 O25 K1 93.6(5) 2_665 3_565 ? O51 C1 O51 121(2) 10_556 . ? O51 C1 C2 119.5(11) 10_556 . ? O51 C1 C2 119.5(11) . . ? C3 C2 C3 120.9(13) . 10_556 ? C3 C2 C1 119.5(6) . . ? C3 C2 C1 119.5(6) 10_556 . ? C3 C4 C5 120.7(11) . . ? C4 C3 C2 119.2(12) . . ? N1 C5 C4 0(3) 10_556 10_556 ? N1 C5 C4 119.3(11) 10_556 . ? C4 C5 C4 119.3(11) 10_556 . ? O53 V11 O53 69(3) 10_557 . ? O53 V11 O5 106.5(17) 10_557 . ? O53 V11 O5 106.5(17) . . ? O53 V11 O3 105.9(17) 10_557 . ? O53 V11 O3 105.9(17) . . ? O5 V11 O3 140.5(10) . . ? O53 V11 O9 179.5(16) 10_557 . ? O53 V11 O9 111.0(15) . . ? O5 V11 O9 73.6(6) . . ? O3 V11 O9 74.2(6) . . ? O53 V11 O9 111.0(15) 10_557 10_557 ? O53 V11 O9 179.5(16) . 10_557 ? O5 V11 O9 73.6(6) . 10_557 ? O3 V11 O9 74.2(6) . 10_557 ? O9 V11 O9 69.6(6) . 10_557 ? O53 V11 V6 137.6(17) 10_557 . ? O53 V11 V6 98.6(15) . . ? O5 V11 V6 36.3(3) . . ? O3 V11 V6 116.5(6) . . ? O9 V11 V6 42.3(3) . . ? O9 V11 V6 81.8(5) 10_557 . ? O53 V11 V6 98.6(15) 10_557 10_557 ? O53 V11 V6 137.6(17) . 10_557 ? O5 V11 V6 36.3(3) . 10_557 ? O3 V11 V6 116.5(6) . 10_557 ? O9 V11 V6 81.8(5) . 10_557 ? O9 V11 V6 42.3(3) 10_557 10_557 ? V6 V11 V6 63.0(3) . 10_557 ? O53 V11 V7 137.4(17) 10_557 . ? O53 V11 V7 98.5(16) . . ? O5 V11 V7 116.1(7) . . ? O3 V11 V7 36.5(3) . . ? O9 V11 V7 42.5(3) . . ? O9 V11 V7 81.9(5) 10_557 . ? V6 V11 V7 83.0(3) . . ? V6 V11 V7 115.1(5) 10_557 . ? O53 V11 V7 98.5(16) 10_557 10_557 ? O53 V11 V7 137.4(17) . 10_557 ? O5 V11 V7 116.1(7) . 10_557 ? O3 V11 V7 36.5(3) . 10_557 ? O9 V11 V7 81.9(5) . 10_557 ? O9 V11 V7 42.5(3) 10_557 10_557 ? V6 V11 V7 115.1(5) . 10_557 ? V6 V11 V7 83.0(3) 10_557 10_557 ? V7 V11 V7 63.0(4) . 10_557 ? O25 K1 O25 65.3(8) . 10_557 ? O25 K1 O22 111.6(4) . 2_665 ? O25 K1 O22 111.6(4) 10_557 2_665 ? O25 K1 O20 99.2(4) . 10_557 ? O25 K1 O20 70.9(3) 10_557 10_557 ? O22 K1 O20 147.2(3) 2_665 10_557 ? O25 K1 O20 70.9(3) . . ? O25 K1 O20 99.2(4) 10_557 . ? O22 K1 O20 147.2(3) 2_665 . ? O20 K1 O20 53.7(4) 10_557 . ? O25 K1 V3 87.7(3) . . ? O25 K1 V3 87.7(3) 10_557 . ? O22 K1 V3 156.8(5) 2_665 . ? O20 K1 V3 27.07(19) 10_557 . ? O20 K1 V3 27.07(19) . . ? O25 K1 V3 85.8(3) . 2_665 ? O25 K1 V3 85.8(3) 10_557 2_665 ? O22 K1 V3 30.9(2) 2_665 2_665 ? O20 K1 V3 151.0(2) 10_557 2_665 ? O20 K1 V3 151.0(2) . 2_665 ? V3 K1 V3 172.3(4) . 2_665 ? O25 K1 S1 18.9(4) . . ? O25 K1 S1 84.2(5) 10_557 . ? O22 K1 S1 105.8(3) 2_665 . ? O20 K1 S1 107.0(3) 10_557 . ? O20 K1 S1 65.5(2) . . ? V3 K1 S1 88.3(2) . . ? V3 K1 S1 86.9(2) 2_665 . ? O25 K1 S1 84.2(5) . 10_557 ? O25 K1 S1 18.9(4) 10_557 10_557 ? O22 K1 S1 105.8(3) 2_665 10_557 ? O20 K1 S1 65.5(2) 10_557 10_557 ? O20 K1 S1 107.0(3) . 10_557 ? V3 K1 S1 88.3(2) . 10_557 ? V3 K1 S1 86.9(2) 2_665 10_557 ? S1 K1 S1 103.1(3) . 10_557 ? O25 K1 V4 105.2(3) . 2_665 ? O25 K1 V4 133.5(4) 10_557 2_665 ? O22 K1 V4 26.08(12) 2_665 2_665 ? O20 K1 V4 151.3(4) 10_557 2_665 ? O20 K1 V4 121.3(2) . 2_665 ? V3 K1 V4 138.6(3) . 2_665 ? V3 K1 V4 47.71(14) 2_665 2_665 ? S1 K1 V4 92.35(15) . 2_665 ? S1 K1 V4 131.4(3) 10_557 2_665 ? O25 K1 V4 133.5(4) . 11_667 ? O25 K1 V4 105.2(3) 10_557 11_667 ? O22 K1 V4 26.08(12) 2_665 11_667 ? O20 K1 V4 121.3(2) 10_557 11_667 ? O20 K1 V4 151.3(4) . 11_667 ? V3 K1 V4 138.6(3) . 11_667 ? V3 K1 V4 47.71(14) 2_665 11_667 ? S1 K1 V4 131.4(3) . 11_667 ? S1 K1 V4 92.35(15) 10_557 11_667 ? V4 K1 V4 46.64(14) 2_665 11_667 ? O25 K1 K1 43.2(3) . 2_665 ? O25 K1 K1 43.2(3) 10_557 2_665 ? O22 K1 K1 85.9(5) 2_665 2_665 ? O20 K1 K1 111.0(3) 10_557 2_665 ? O20 K1 K1 111.0(3) . 2_665 ? V3 K1 K1 117.3(3) . 2_665 ? V3 K1 K1 55.0(3) 2_665 2_665 ? S1 K1 K1 57.41(12) . 2_665 ? S1 K1 K1 57.41(12) 10_557 2_665 ? V4 K1 K1 97.3(4) 2_665 2_665 ? V4 K1 K1 97.3(4) 11_667 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.251 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.221 _database_code_depnum_ccdc_archive 'CCDC 937962' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H107 K3 Mn3 N3 Nd6 O172 S2 V39' _chemical_formula_weight 6316.41 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' _cell_length_a 24.603(3) _cell_length_b 24.603(3) _cell_length_c 17.343(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9091(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5523 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6066 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.400 _exptl_absorpt_correction_T_max 0.550 _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 65554 _diffrn_reflns_av_R_equivalents 0.1043 _diffrn_reflns_av_unetI/netI 0.0546 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5523 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit-3 50' was used to omit the weak reflections above 50 degree. In the structure, the C1, C2 and C5 atoms of the isolated organic molecule (nicotinic acid) reside on the mirror plane and the C4 and N1 centers exhibit the site-occupancy disorder with 50% for each. All the organic molecules are restrained with the command 'DFIX' so as to get a chemically reasonable structural feature. Moreover, all the atoms are restrained with the commands 'simu' and 'isor' so as to avoid the ADP problems. These restrained commands led to a final restraint value of 73. Furthermore, the H atoms on the ligands cannot be added due to the C/N disorder problem. In the final refinement, only four positions of the isolated lattice water molecules can be well confirmed from the residual peaks. Thus, the SQUEEZE program was used to estimate the rest lattice water molecules in the solvent accessible voids. Based on the calculation results, elemental analysis and TG analysis, another fifteen H2O molecules were directly included in the final molecular formula. It is worth mentioning that there is a relatively high residual peak (3.88 eA-3) is close to the O21 and O22 atoms of the POM with the distances of 1.90 A. This peak cannot be assigned as a disordered lattice water molecule, NH4+ or disordered K+ cations due to the obviously unreasonable bond distances to the O atoms of POMs. It is presumed that such a resiual peak is attributed to the series termination errors. ; 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 0.000 0.000 0.000 62.1 8.2 2 -0.022 0.488 -0.014 1549.5 134.7 3 0.000 0.000 0.500 62.2 8.4 _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^)+(0.0840P)^2^+200.7340P] 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_number_reflns 5523 _refine_ls_number_parameters 393 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.050 _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 Nd1 Nd 0.79997(3) 1.48848(3) -0.97164(5) 0.0435(3) Uani 1 1 d . . . Mn1 Mn 0.87027(11) 1.66593(10) -0.7500 0.0234(5) Uani 1 2 d S . . V1 V 0.87104(10) 1.66738(9) -0.93803(11) 0.0338(5) Uani 1 1 d . . . V2 V 1.05601(13) 1.69841(14) -0.7500 0.0375(7) Uani 1 2 d S . . V3 V 0.98804(10) 1.75717(9) -0.84048(11) 0.0336(5) Uani 1 1 d . . . V4 V 0.74909(9) 1.58344(9) -0.84210(11) 0.0286(4) Uani 1 1 d . . . V5 V 0.93527(9) 1.60669(9) -0.84181(11) 0.0289(4) Uani 1 1 d . . . V6 V 0.81207(12) 1.51932(12) -0.7500 0.0259(6) Uani 1 2 d S . . V7 V 0.81650(11) 1.73529(9) -0.84051(12) 0.0346(5) Uani 1 1 d . . . V8 V 0.69252(15) 1.65267(15) -0.7500 0.0378(7) Uani 1 2 d S . . O1 O 0.8446(4) 1.6019(4) -0.9888(5) 0.041(2) Uani 1 1 d . . . O2 O 0.9086(4) 1.5510(4) -0.9066(5) 0.039(2) Uani 1 1 d . . . O3 O 1.0079(5) 1.8092(4) -0.9049(5) 0.048(2) Uani 1 1 d . . . O4 O 1.1247(6) 1.7088(7) -0.7500 0.052(4) Uani 1 2 d S . . O5 O 0.9507(4) 1.6782(4) -0.9023(4) 0.0298(17) Uani 1 1 d . . . O6 O 1.0583(4) 1.7506(4) -0.6735(5) 0.038(2) Uani 1 1 d . . . O7 O 1.0120(4) 1.6287(4) -0.6749(5) 0.0377(19) Uani 1 1 d . . . O8 O 0.8945(4) 1.7256(3) -0.8321(4) 0.0280(16) Uani 1 1 d . . . O9 O 0.8389(5) 1.7879(4) -0.9058(5) 0.048(2) Uani 1 1 d . . . O10 O 0.7928(4) 1.4731(4) -0.8269(5) 0.0339(18) Uani 1 1 d . . . O11 O 0.7426(5) 1.5347(5) -0.7500 0.028(2) Uani 1 2 d S . . O12 O 0.6829(4) 1.5871(4) -0.8248(5) 0.0360(19) Uani 1 1 d . . . O13 O 0.9022(5) 1.5545(5) -0.7500 0.027(2) Uani 1 2 d S . . O14 O 0.9501(5) 1.6760(5) -0.7500 0.026(2) Uani 1 2 d S . . O15 O 0.7312(4) 1.5289(4) -0.9060(5) 0.0351(18) Uani 1 1 d . . . O16 O 0.8935(5) 1.7235(4) -0.9996(5) 0.045(2) Uani 1 1 d . . . O17 O 0.7911(5) 1.6557(5) -0.7500 0.028(2) Uani 1 2 d S . . O18 O 0.8450(3) 1.6029(3) -0.8258(4) 0.0248(16) Uani 1 1 d . . . O19 O 0.7917(4) 1.6579(4) -0.9024(4) 0.0318(17) Uani 1 1 d . . . O20 O 0.7336(4) 1.7096(4) -0.8270(5) 0.038(2) Uani 1 1 d . . . O21 O 0.9989(6) 1.8007(5) -0.7500 0.035(3) Uani 1 2 d S . . O22 O 0.8404(6) 1.7808(5) -0.7500 0.034(3) Uani 1 2 d S . . O23 O 0.6241(7) 1.6445(7) -0.7500 0.056(4) Uani 1 2 d S . . O1W O 0.7749(7) 1.4112(7) -1.0805(9) 0.101(5) Uani 1 1 d . . . O2W O 0.7359(6) 1.5054(6) -1.0702(7) 0.076(4) Uani 1 1 d . . . O3W O 0.8860(5) 1.5254(6) -1.0706(7) 0.070(3) Uani 1 1 d . . . O4W O 0.8340(5) 1.4099(5) -0.9374(8) 0.068(3) Uani 1 1 d . . . O5W O 0.6959(4) 1.3982(4) -0.9473(6) 0.049(2) Uani 1 1 d . . . K1 K 0.5865(4) 1.2278(4) -0.7500 0.125(3) Uani 1 2 d SU . . S1 S 0.6667 1.3333 -0.9177(4) 0.0427(13) Uani 1 3 d S . . O24 O 0.6667 1.3333 -0.8343(11) 0.075(6) Uani 1 3 d S . . O51 O 0.8588(9) 1.9132(9) -0.8131(9) 0.138(7) Uani 1 1 d DU . . C2 C 0.7561(8) 1.8521(13) -0.7500 0.099(6) Uani 1 2 d SDU . . C4 C 0.6587(8) 1.7919(9) -0.6804(6) 0.099(5) Uani 0.50 1 d PDU . . N1 N 0.6587(8) 1.7919(9) -0.6804(6) 0.099(5) Uani 0.50 1 d P . . C1 C 0.8253(9) 1.8915(15) -0.7500 0.109(7) Uani 1 2 d SDU . . C5 C 0.6257(9) 1.7722(14) -0.7500 0.104(7) Uani 1 2 d SDU . . C3 C 0.7232(8) 1.8311(10) -0.6806(7) 0.097(5) Uani 1 1 d DU . . OW3 O 0.8578(6) 1.9119(6) -0.9809(7) 0.077(3) Uani 1 1 d . . . OW2 O 0.9866(6) 1.6452(6) -1.0487(7) 0.078(4) Uani 1 1 d . . . OW4 O 0.9899(17) 1.9726(10) -0.7500 0.078 Uiso 0.67 2 d SP . . OW1 O 0.7231(7) 1.6089(6) -1.0491(7) 0.083(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0370(4) 0.0338(4) 0.0547(5) -0.0124(3) -0.0004(3) 0.0139(3) Mn1 0.0268(12) 0.0192(11) 0.0229(11) 0.000 0.000 0.0106(10) V1 0.0388(12) 0.0290(11) 0.0289(10) -0.0012(8) -0.0003(8) 0.0134(9) V2 0.0239(15) 0.0345(16) 0.0443(17) 0.000 0.000 0.0074(13) V3 0.0322(11) 0.0245(10) 0.0321(10) 0.0034(8) 0.0028(8) 0.0051(8) V4 0.0304(10) 0.0250(10) 0.0320(10) -0.0037(8) -0.0048(8) 0.0151(8) V5 0.0256(10) 0.0245(10) 0.0328(10) -0.0026(8) 0.0035(8) 0.0095(8) V6 0.0208(13) 0.0171(12) 0.0385(15) 0.000 0.000 0.0085(11) V7 0.0477(13) 0.0290(11) 0.0324(10) 0.0043(8) 0.0005(9) 0.0233(10) V8 0.0382(17) 0.0412(17) 0.0444(17) 0.000 0.000 0.0277(15) O1 0.044(5) 0.040(5) 0.036(5) -0.008(4) 0.000(4) 0.019(4) O2 0.040(5) 0.031(5) 0.044(5) -0.007(4) 0.001(4) 0.017(4) O3 0.052(6) 0.035(5) 0.040(5) 0.007(4) 0.001(4) 0.008(4) O4 0.027(7) 0.051(8) 0.065(9) 0.000 0.000 0.010(6) O5 0.031(4) 0.028(4) 0.026(4) 0.001(3) 0.004(3) 0.012(3) O6 0.024(4) 0.033(5) 0.041(5) 0.000(4) -0.005(3) 0.003(4) O7 0.030(4) 0.038(5) 0.043(5) 0.003(4) -0.004(4) 0.016(4) O8 0.034(4) 0.018(4) 0.028(4) 0.001(3) 0.000(3) 0.009(3) O9 0.074(7) 0.037(5) 0.039(5) 0.008(4) 0.003(5) 0.033(5) O10 0.030(4) 0.023(4) 0.045(5) -0.009(3) -0.007(4) 0.010(3) O11 0.031(6) 0.032(6) 0.029(6) 0.000 0.000 0.022(5) O12 0.035(5) 0.036(5) 0.040(5) -0.004(4) -0.003(4) 0.019(4) O13 0.025(6) 0.024(6) 0.028(5) 0.000 0.000 0.010(5) O14 0.024(5) 0.020(5) 0.026(5) 0.000 0.000 0.006(4) O15 0.036(5) 0.031(4) 0.039(5) -0.006(4) -0.007(4) 0.017(4) O16 0.057(6) 0.043(5) 0.032(4) 0.006(4) 0.000(4) 0.022(5) O17 0.030(6) 0.031(6) 0.023(5) 0.000 0.000 0.015(5) O18 0.027(4) 0.018(4) 0.027(4) -0.003(3) -0.002(3) 0.010(3) O19 0.036(4) 0.035(4) 0.027(4) -0.002(3) -0.004(3) 0.020(4) O20 0.042(5) 0.037(5) 0.045(5) 0.000(4) -0.003(4) 0.027(4) O21 0.045(7) 0.023(6) 0.031(6) 0.000 0.000 0.011(5) O22 0.050(7) 0.027(6) 0.032(6) 0.000 0.000 0.026(6) O23 0.049(8) 0.057(9) 0.075(10) 0.000 0.000 0.036(8) O1W 0.114(12) 0.081(9) 0.094(10) -0.045(8) 0.003(9) 0.037(9) O2W 0.093(9) 0.076(8) 0.061(7) -0.021(6) -0.032(7) 0.044(7) O3W 0.060(7) 0.074(8) 0.077(8) -0.019(6) 0.010(6) 0.034(6) O4W 0.064(7) 0.040(6) 0.107(9) -0.008(6) 0.007(6) 0.031(6) O5W 0.036(5) 0.028(5) 0.079(7) -0.003(4) -0.004(5) 0.014(4) K1 0.091(5) 0.113(6) 0.191(7) 0.000 0.000 0.066(4) S1 0.0339(18) 0.0339(18) 0.060(4) 0.000 0.000 0.0170(9) O24 0.089(10) 0.089(10) 0.047(11) 0.000 0.000 0.045(5) O51 0.159(11) 0.130(10) 0.142(10) 0.005(8) 0.008(8) 0.086(8) C2 0.119(8) 0.094(8) 0.103(8) 0.000 0.000 0.066(6) C4 0.128(7) 0.090(7) 0.098(7) 0.000(5) -0.001(6) 0.069(6) N1 0.128(7) 0.090(7) 0.098(7) 0.000(5) -0.001(6) 0.069(6) C1 0.123(9) 0.104(9) 0.110(9) 0.000 0.000 0.064(7) C5 0.126(9) 0.094(9) 0.101(9) 0.000 0.000 0.062(7) C3 0.122(7) 0.090(7) 0.099(7) -0.002(5) 0.003(6) 0.068(6) OW3 0.086(9) 0.078(9) 0.071(8) -0.008(6) -0.014(7) 0.043(7) OW2 0.078(9) 0.070(8) 0.072(8) 0.010(6) 0.024(7) 0.026(7) OW1 0.105(10) 0.087(9) 0.068(8) 0.013(7) -0.019(7) 0.055(8) _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 Nd1 O5W 2.446(9) . ? Nd1 O1 2.452(9) . ? Nd1 O2W 2.496(11) . ? Nd1 O3W 2.516(11) . ? Nd1 O1W 2.527(12) . ? Nd1 O4W 2.531(11) . ? Nd1 O10 2.531(9) . ? Nd1 O2 2.582(9) . ? Nd1 O15 2.613(8) . ? Mn1 O17 1.835(11) . ? Mn1 O14 1.852(11) . ? Mn1 O18 1.886(7) . ? Mn1 O18 1.886(7) 10_554 ? Mn1 O8 1.913(7) 10_554 ? Mn1 O8 1.913(7) . ? Mn1 V7 3.063(3) 10_554 ? Mn1 V7 3.063(3) . ? Mn1 V3 3.065(3) 10_554 ? Mn1 V3 3.065(3) . ? Mn1 V4 3.083(3) . ? Mn1 V4 3.083(3) 10_554 ? V1 O16 1.609(9) . ? V1 O1 1.658(8) . ? V1 O5 1.942(8) . ? V1 O19 1.947(8) . ? V1 O8 2.221(7) . ? V1 O18 2.388(7) . ? V1 V3 3.110(3) . ? V1 V7 3.114(3) . ? V2 O4 1.577(14) . ? V2 O6 1.828(9) 10_554 ? V2 O6 1.828(9) . ? V2 O7 1.989(9) 10_554 ? V2 O7 1.989(9) . ? V2 O14 2.379(11) . ? V3 O3 1.581(9) . ? V3 O6 1.830(9) 10_554 ? V3 O21 1.842(6) . ? V3 O5 1.996(8) . ? V3 O8 2.033(8) . ? V3 O14 2.336(8) . ? V4 O15 1.622(8) . ? V4 O12 1.702(8) . ? V4 O19 1.905(8) . ? V4 O11 1.955(6) . ? V4 O18 2.179(8) . ? V4 O17 2.224(8) . ? V4 K1 3.996(8) 8_574 ? V5 O2 1.635(8) . ? V5 O7 1.708(8) 10_554 ? V5 O5 1.916(8) . ? V5 O13 1.949(6) . ? V5 O18 2.193(8) . ? V5 O14 2.226(7) . ? V6 O10 1.662(8) . ? V6 O10 1.662(8) 10_554 ? V6 O11 1.926(11) . ? V6 O13 1.935(11) . ? V6 O18 2.223(7) 10_554 ? V6 O18 2.223(7) . ? V6 K1 3.564(8) 3_775 ? V6 K1 3.673(8) 8_574 ? V7 O9 1.596(9) . ? V7 O20 1.825(9) . ? V7 O22 1.846(6) . ? V7 O19 1.998(8) . ? V7 O8 2.054(8) . ? V7 O17 2.337(8) . ? V7 V8 3.115(4) . ? V8 O23 1.593(14) . ? V8 O20 1.831(9) 10_554 ? V8 O20 1.831(9) . ? V8 O12 1.990(8) . ? V8 O12 1.990(8) 10_554 ? V8 O17 2.388(11) . ? V8 V7 3.115(4) 10_554 ? O6 V3 1.830(9) 10_554 ? O7 V5 1.708(8) 10_554 ? O10 K1 2.920(11) 3_775 ? O11 V4 1.955(6) 10_554 ? O11 K1 2.770(14) 8_574 ? O13 V5 1.949(6) 10_554 ? O14 V5 2.226(7) 10_554 ? O14 V3 2.336(8) 10_554 ? O17 V4 2.224(8) 10_554 ? O17 V7 2.337(8) 10_554 ? O21 V3 1.842(6) 10_554 ? O22 V7 1.846(6) 10_554 ? O5W S1 1.476(9) . ? K1 O24 2.766(13) 8_574 ? K1 O24 2.766(13) . ? K1 O11 2.770(14) 3_775 ? K1 O10 2.920(11) 5_575 ? K1 O10 2.920(11) 8_574 ? K1 V6 3.564(8) 8_574 ? K1 V6 3.673(8) 3_775 ? K1 S1 3.738(8) 8_574 ? K1 S1 3.738(8) . ? K1 V4 3.996(8) 3_775 ? K1 V4 3.996(8) 12_774 ? K1 K1 4.068(16) 8_574 ? S1 O24 1.45(2) . ? S1 O5W 1.476(9) 5_575 ? S1 O5W 1.476(9) 3_775 ? S1 K1 3.738(8) 3_775 ? S1 K1 3.738(8) 8_574 ? O24 K1 2.766(13) 3_775 ? O24 K1 2.766(13) 8_574 ? O51 C1 1.313(9) . ? C2 C3 1.398(9) 10_554 ? C2 C3 1.398(9) . ? C2 C1 1.478(10) . ? C4 C3 1.385(10) . ? C4 C5 1.399(9) . ? C1 O51 1.313(10) 10_554 ? C5 N1 1.399(9) 10_554 ? C5 C4 1.399(9) 10_554 ? OW4 OW4 1.02(4) 8_584 ? OW4 OW4 1.02(4) 3_885 ? 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 O5W Nd1 O1 136.4(3) . . ? O5W Nd1 O2W 78.9(4) . . ? O1 Nd1 O2W 71.8(4) . . ? O5W Nd1 O3W 139.1(4) . . ? O1 Nd1 O3W 71.9(3) . . ? O2W Nd1 O3W 87.7(4) . . ? O5W Nd1 O1W 72.2(4) . . ? O1 Nd1 O1W 124.5(4) . . ? O2W Nd1 O1W 71.1(5) . . ? O3W Nd1 O1W 66.9(4) . . ? O5W Nd1 O4W 82.0(3) . . ? O1 Nd1 O4W 140.0(3) . . ? O2W Nd1 O4W 139.9(4) . . ? O3W Nd1 O4W 84.0(4) . . ? O1W Nd1 O4W 69.6(5) . . ? O5W Nd1 O10 74.3(3) . . ? O1 Nd1 O10 104.4(3) . . ? O2W Nd1 O10 134.5(4) . . ? O3W Nd1 O10 135.5(3) . . ? O1W Nd1 O10 131.0(4) . . ? O4W Nd1 O10 71.2(3) . . ? O5W Nd1 O2 140.1(3) . . ? O1 Nd1 O2 68.5(3) . . ? O2W Nd1 O2 138.7(4) . . ? O3W Nd1 O2 69.5(3) . . ? O1W Nd1 O2 124.4(4) . . ? O4W Nd1 O2 73.3(3) . . ? O10 Nd1 O2 68.3(3) . . ? O5W Nd1 O15 71.8(3) . . ? O1 Nd1 O15 68.1(3) . . ? O2W Nd1 O15 69.6(3) . . ? O3W Nd1 O15 138.4(3) . . ? O1W Nd1 O15 130.6(4) . . ? O4W Nd1 O15 135.4(3) . . ? O10 Nd1 O15 67.4(3) . . ? O2 Nd1 O15 104.9(3) . . ? O17 Mn1 O14 179.8(5) . . ? O17 Mn1 O18 89.8(3) . . ? O14 Mn1 O18 90.1(3) . . ? O17 Mn1 O18 89.8(3) . 10_554 ? O14 Mn1 O18 90.1(3) . 10_554 ? O18 Mn1 O18 88.3(4) . 10_554 ? O17 Mn1 O8 90.4(3) . 10_554 ? O14 Mn1 O8 89.7(3) . 10_554 ? O18 Mn1 O8 176.1(3) . 10_554 ? O18 Mn1 O8 87.7(3) 10_554 10_554 ? O17 Mn1 O8 90.4(3) . . ? O14 Mn1 O8 89.7(3) . . ? O18 Mn1 O8 87.7(3) . . ? O18 Mn1 O8 176.1(3) 10_554 . ? O8 Mn1 O8 96.2(4) 10_554 . ? O17 Mn1 V7 49.6(3) . 10_554 ? O14 Mn1 V7 130.5(2) . 10_554 ? O18 Mn1 V7 139.4(2) . 10_554 ? O18 Mn1 V7 92.6(2) 10_554 10_554 ? O8 Mn1 V7 41.2(2) 10_554 10_554 ? O8 Mn1 V7 90.6(2) . 10_554 ? O17 Mn1 V7 49.6(3) . . ? O14 Mn1 V7 130.5(2) . . ? O18 Mn1 V7 92.6(2) . . ? O18 Mn1 V7 139.4(2) 10_554 . ? O8 Mn1 V7 90.6(2) 10_554 . ? O8 Mn1 V7 41.2(2) . . ? V7 Mn1 V7 61.66(9) 10_554 . ? O17 Mn1 V3 130.6(3) . 10_554 ? O14 Mn1 V3 49.6(2) . 10_554 ? O18 Mn1 V3 139.6(2) . 10_554 ? O18 Mn1 V3 92.7(2) 10_554 10_554 ? O8 Mn1 V3 40.5(2) 10_554 10_554 ? O8 Mn1 V3 90.1(2) . 10_554 ? V7 Mn1 V3 80.97(7) 10_554 10_554 ? V7 Mn1 V3 111.59(9) . 10_554 ? O17 Mn1 V3 130.6(3) . . ? O14 Mn1 V3 49.6(2) . . ? O18 Mn1 V3 92.7(2) . . ? O18 Mn1 V3 139.6(2) 10_554 . ? O8 Mn1 V3 90.1(2) 10_554 . ? O8 Mn1 V3 40.5(2) . . ? V7 Mn1 V3 111.59(9) 10_554 . ? V7 Mn1 V3 80.97(7) . . ? V3 Mn1 V3 61.60(9) 10_554 . ? O17 Mn1 V4 45.5(2) . . ? O14 Mn1 V4 134.4(2) . . ? O18 Mn1 V4 44.4(2) . . ? O18 Mn1 V4 90.4(2) 10_554 . ? O8 Mn1 V4 135.9(3) 10_554 . ? O8 Mn1 V4 87.0(2) . . ? V7 Mn1 V4 95.02(8) 10_554 . ? V7 Mn1 V4 63.68(6) . . ? V3 Mn1 V4 175.01(10) 10_554 . ? V3 Mn1 V4 117.76(5) . . ? O17 Mn1 V4 45.5(2) . 10_554 ? O14 Mn1 V4 134.4(2) . 10_554 ? O18 Mn1 V4 90.4(2) . 10_554 ? O18 Mn1 V4 44.4(2) 10_554 10_554 ? O8 Mn1 V4 87.0(2) 10_554 10_554 ? O8 Mn1 V4 135.9(3) . 10_554 ? V7 Mn1 V4 63.68(6) 10_554 10_554 ? V7 Mn1 V4 95.02(8) . 10_554 ? V3 Mn1 V4 117.76(5) 10_554 10_554 ? V3 Mn1 V4 175.01(10) . 10_554 ? V4 Mn1 V4 62.40(9) . 10_554 ? O16 V1 O1 106.3(5) . . ? O16 V1 O5 101.8(4) . . ? O1 V1 O5 100.4(4) . . ? O16 V1 O19 101.9(4) . . ? O1 V1 O19 99.8(4) . . ? O5 V1 O19 142.9(3) . . ? O16 V1 O8 97.4(4) . . ? O1 V1 O8 156.3(4) . . ? O5 V1 O8 74.3(3) . . ? O19 V1 O8 74.7(3) . . ? O16 V1 O18 167.0(4) . . ? O1 V1 O18 86.7(4) . . ? O5 V1 O18 75.4(3) . . ? O19 V1 O18 75.0(3) . . ? O8 V1 O18 69.6(3) . . ? O16 V1 V3 87.3(3) . . ? O1 V1 V3 138.9(3) . . ? O5 V1 V3 38.5(2) . . ? O19 V1 V3 115.4(2) . . ? O8 V1 V3 40.7(2) . . ? O18 V1 V3 82.76(18) . . ? O16 V1 V7 87.4(4) . . ? O1 V1 V7 138.2(3) . . ? O5 V1 V7 115.4(2) . . ? O19 V1 V7 38.5(2) . . ? O8 V1 V7 41.2(2) . . ? O18 V1 V7 82.50(18) . . ? V3 V1 V7 79.48(7) . . ? O4 V2 O6 103.4(4) . 10_554 ? O4 V2 O6 103.4(4) . . ? O6 V2 O6 93.1(5) 10_554 . ? O4 V2 O7 102.5(5) . 10_554 ? O6 V2 O7 86.7(4) 10_554 10_554 ? O6 V2 O7 153.3(4) . 10_554 ? O4 V2 O7 102.5(5) . . ? O6 V2 O7 153.3(4) 10_554 . ? O6 V2 O7 86.7(4) . . ? O7 V2 O7 81.8(5) 10_554 . ? O4 V2 O14 176.5(6) . . ? O6 V2 O14 78.9(3) 10_554 . ? O6 V2 O14 78.9(3) . . ? O7 V2 O14 74.9(3) 10_554 . ? O7 V2 O14 74.9(3) . . ? O3 V3 O6 104.0(5) . 10_554 ? O3 V3 O21 103.6(5) . . ? O6 V3 O21 93.9(5) 10_554 . ? O3 V3 O5 102.4(4) . . ? O6 V3 O5 88.9(4) 10_554 . ? O21 V3 O5 152.3(4) . . ? O3 V3 O8 101.1(4) . . ? O6 V3 O8 153.5(3) 10_554 . ? O21 V3 O8 88.2(4) . . ? O5 V3 O8 77.5(3) . . ? O3 V3 O14 175.0(4) . . ? O6 V3 O14 80.0(4) 10_554 . ? O21 V3 O14 78.7(3) . . ? O5 V3 O14 74.7(3) . . ? O8 V3 O14 74.5(3) . . ? O3 V3 Mn1 138.6(4) . . ? O6 V3 Mn1 117.1(3) 10_554 . ? O21 V3 Mn1 78.4(3) . . ? O5 V3 Mn1 75.8(2) . . ? O8 V3 Mn1 37.7(2) . . ? O14 V3 Mn1 37.1(3) . . ? O3 V3 V1 89.5(3) . . ? O6 V3 V1 126.1(3) 10_554 . ? O21 V3 V1 133.7(4) . . ? O5 V3 V1 37.2(2) . . ? O8 V3 V1 45.4(2) . . ? O14 V3 V1 85.7(2) . . ? Mn1 V3 V1 63.76(6) . . ? O15 V4 O12 107.1(4) . . ? O15 V4 O19 102.2(4) . . ? O12 V4 O19 97.3(4) . . ? O15 V4 O11 98.4(4) . . ? O12 V4 O11 95.8(4) . . ? O19 V4 O11 151.1(4) . . ? O15 V4 O18 94.9(4) . . ? O12 V4 O18 157.7(3) . . ? O19 V4 O18 81.1(3) . . ? O11 V4 O18 77.0(4) . . ? O15 V4 O17 167.9(4) . . ? O12 V4 O17 84.6(4) . . ? O19 V4 O17 79.2(3) . . ? O11 V4 O17 76.5(3) . . ? O18 V4 O17 73.3(3) . . ? O15 V4 Mn1 132.2(3) . . ? O12 V4 Mn1 120.6(3) . . ? O19 V4 Mn1 76.4(2) . . ? O11 V4 Mn1 74.7(3) . . ? O18 V4 Mn1 37.23(19) . . ? O17 V4 Mn1 36.1(3) . . ? O15 V4 K1 69.2(3) . 8_574 ? O12 V4 K1 80.3(3) . 8_574 ? O19 V4 K1 169.6(3) . 8_574 ? O11 V4 K1 39.1(3) . 8_574 ? O18 V4 K1 104.9(2) . 8_574 ? O17 V4 K1 110.5(2) . 8_574 ? Mn1 V4 K1 113.52(10) . 8_574 ? O2 V5 O7 107.4(4) . 10_554 ? O2 V5 O5 101.8(4) . . ? O7 V5 O5 97.0(4) 10_554 . ? O2 V5 O13 98.6(4) . . ? O7 V5 O13 95.8(4) 10_554 . ? O5 V5 O13 151.3(4) . . ? O2 V5 O18 94.5(4) . . ? O7 V5 O18 158.0(3) 10_554 . ? O5 V5 O18 80.8(3) . . ? O13 V5 O18 77.7(4) . . ? O2 V5 O14 167.8(4) . . ? O7 V5 O14 84.5(4) 10_554 . ? O5 V5 O14 78.9(3) . . ? O13 V5 O14 77.0(3) . . ? O18 V5 O14 73.5(3) . . ? O2 V5 Mn1 131.6(3) . . ? O7 V5 Mn1 120.9(3) 10_554 . ? O5 V5 Mn1 76.2(2) . . ? O13 V5 Mn1 75.3(3) . . ? O18 V5 Mn1 37.16(18) . . ? O14 V5 Mn1 36.4(3) . . ? O10 V6 O10 106.8(6) . 10_554 ? O10 V6 O11 99.1(4) . . ? O10 V6 O11 99.1(4) 10_554 . ? O10 V6 O13 100.2(4) . . ? O10 V6 O13 100.2(4) 10_554 . ? O11 V6 O13 147.4(5) . . ? O10 V6 O18 162.8(4) . 10_554 ? O10 V6 O18 90.3(3) 10_554 10_554 ? O11 V6 O18 76.5(3) . 10_554 ? O13 V6 O18 77.3(3) . 10_554 ? O10 V6 O18 90.3(3) . . ? O10 V6 O18 162.8(4) 10_554 . ? O11 V6 O18 76.5(3) . . ? O13 V6 O18 77.3(3) . . ? O18 V6 O18 72.5(4) 10_554 . ? O10 V6 Mn1 126.6(3) . . ? O10 V6 Mn1 126.6(3) 10_554 . ? O11 V6 Mn1 73.4(3) . . ? O13 V6 Mn1 74.0(3) . . ? O18 V6 Mn1 36.24(18) 10_554 . ? O18 V6 Mn1 36.24(18) . . ? O10 V6 K1 54.2(3) . 3_775 ? O10 V6 K1 54.2(3) 10_554 3_775 ? O11 V6 K1 116.0(4) . 3_775 ? O13 V6 K1 96.6(4) . 3_775 ? O18 V6 K1 142.76(19) 10_554 3_775 ? O18 V6 K1 142.76(19) . 3_775 ? Mn1 V6 K1 170.56(18) . 3_775 ? O10 V6 K1 71.4(3) . 8_574 ? O10 V6 K1 71.4(3) 10_554 8_574 ? O11 V6 K1 47.7(4) . 8_574 ? O13 V6 K1 165.0(4) . 8_574 ? O18 V6 K1 114.5(2) 10_554 8_574 ? O18 V6 K1 114.5(2) . 8_574 ? Mn1 V6 K1 121.06(17) . 8_574 ? K1 V6 K1 68.4(3) 3_775 8_574 ? O9 V7 O20 104.1(5) . . ? O9 V7 O22 103.6(5) . . ? O20 V7 O22 93.5(5) . . ? O9 V7 O19 102.0(4) . . ? O20 V7 O19 89.1(4) . . ? O22 V7 O19 152.7(4) . . ? O9 V7 O8 100.4(4) . . ? O20 V7 O8 154.0(3) . . ? O22 V7 O8 88.8(4) . . ? O19 V7 O8 77.6(3) . . ? O9 V7 O17 174.2(5) . . ? O20 V7 O17 80.8(4) . . ? O22 V7 O17 78.9(3) . . ? O19 V7 O17 74.7(3) . . ? O8 V7 O17 74.3(3) . . ? O9 V7 Mn1 138.2(4) . . ? O20 V7 Mn1 117.5(3) . . ? O22 V7 Mn1 78.9(3) . . ? O19 V7 Mn1 75.8(2) . . ? O8 V7 Mn1 37.8(2) . . ? O17 V7 Mn1 36.7(3) . . ? O9 V7 V1 89.0(4) . . ? O20 V7 V1 126.3(3) . . ? O22 V7 V1 134.1(4) . . ? O19 V7 V1 37.3(2) . . ? O8 V7 V1 45.4(2) . . ? O17 V7 V1 85.5(2) . . ? Mn1 V7 V1 63.73(6) . . ? O9 V7 V8 135.6(4) . . ? O20 V7 V8 31.6(3) . . ? O22 V7 V8 83.0(4) . . ? O19 V7 V8 85.2(2) . . ? O8 V7 V8 123.7(2) . . ? O17 V7 V8 49.5(3) . . ? Mn1 V7 V8 86.16(8) . . ? V1 V7 V8 117.89(9) . . ? O23 V8 O20 103.9(5) . 10_554 ? O23 V8 O20 103.9(5) . . ? O20 V8 O20 93.7(6) 10_554 . ? O23 V8 O12 102.0(5) . . ? O20 V8 O12 153.2(4) 10_554 . ? O20 V8 O12 86.7(4) . . ? O23 V8 O12 102.0(5) . 10_554 ? O20 V8 O12 86.7(4) 10_554 10_554 ? O20 V8 O12 153.2(4) . 10_554 ? O12 V8 O12 81.3(5) . 10_554 ? O23 V8 O17 175.3(6) . . ? O20 V8 O17 79.2(3) 10_554 . ? O20 V8 O17 79.2(3) . . ? O12 V8 O17 74.5(3) . . ? O12 V8 O17 74.5(3) 10_554 . ? O23 V8 V7 135.3(4) . 10_554 ? O20 V8 V7 31.5(3) 10_554 10_554 ? O20 V8 V7 83.3(3) . 10_554 ? O12 V8 V7 122.6(3) . 10_554 ? O12 V8 V7 83.2(3) 10_554 10_554 ? O17 V8 V7 48.1(2) . 10_554 ? O23 V8 V7 135.3(4) . . ? O20 V8 V7 83.3(3) 10_554 . ? O20 V8 V7 31.5(3) . . ? O12 V8 V7 83.2(3) . . ? O12 V8 V7 122.6(3) 10_554 . ? O17 V8 V7 48.1(2) . . ? V7 V8 V7 60.53(10) 10_554 . ? V1 O1 Nd1 140.9(5) . . ? V5 O2 Nd1 131.4(4) . . ? V5 O5 V1 109.0(4) . . ? V5 O5 V3 112.5(4) . . ? V1 O5 V3 104.3(4) . . ? V2 O6 V3 117.4(4) . 10_554 ? V5 O7 V2 115.0(4) 10_554 . ? Mn1 O8 V3 101.8(4) . . ? Mn1 O8 V7 101.0(3) . . ? V3 O8 V7 153.5(4) . . ? Mn1 O8 V1 103.9(3) . . ? V3 O8 V1 93.8(3) . . ? V7 O8 V1 93.4(3) . . ? V6 O10 Nd1 136.0(4) . . ? V6 O10 K1 98.4(4) . 3_775 ? Nd1 O10 K1 124.3(3) . 3_775 ? V6 O11 V4 108.2(4) . 10_554 ? V6 O11 V4 108.2(4) . . ? V4 O11 V4 109.6(5) 10_554 . ? V6 O11 K1 101.4(5) . 8_574 ? V4 O11 K1 114.4(4) 10_554 8_574 ? V4 O11 K1 114.4(4) . 8_574 ? V4 O12 V8 115.4(4) . . ? V6 O13 V5 107.6(4) . 10_554 ? V6 O13 V5 107.6(4) . . ? V5 O13 V5 109.5(5) 10_554 . ? Mn1 O14 V5 98.1(4) . . ? Mn1 O14 V5 98.1(4) . 10_554 ? V5 O14 V5 91.4(4) . 10_554 ? Mn1 O14 V3 93.3(4) . 10_554 ? V5 O14 V3 167.9(5) . 10_554 ? V5 O14 V3 90.96(9) 10_554 10_554 ? Mn1 O14 V3 93.3(4) . . ? V5 O14 V3 90.96(9) . . ? V5 O14 V3 167.9(5) 10_554 . ? V3 O14 V3 84.4(3) 10_554 . ? Mn1 O14 V2 175.0(6) . . ? V5 O14 V2 85.3(3) . . ? V5 O14 V2 85.3(3) 10_554 . ? V3 O14 V2 83.0(3) 10_554 . ? V3 O14 V2 83.0(3) . . ? V4 O15 Nd1 130.8(4) . . ? Mn1 O17 V4 98.4(4) . . ? Mn1 O17 V4 98.4(4) . 10_554 ? V4 O17 V4 91.8(4) . 10_554 ? Mn1 O17 V7 93.7(4) . 10_554 ? V4 O17 V7 167.2(5) . 10_554 ? V4 O17 V7 90.59(10) 10_554 10_554 ? Mn1 O17 V7 93.7(4) . . ? V4 O17 V7 90.59(10) . . ? V4 O17 V7 167.2(5) 10_554 . ? V7 O17 V7 84.4(4) 10_554 . ? Mn1 O17 V8 174.8(6) . . ? V4 O17 V8 85.2(3) . . ? V4 O17 V8 85.2(3) 10_554 . ? V7 O17 V8 82.5(3) 10_554 . ? V7 O17 V8 82.5(3) . . ? Mn1 O18 V4 98.4(3) . . ? Mn1 O18 V5 98.2(3) . . ? V4 O18 V5 162.8(4) . . ? Mn1 O18 V6 99.6(3) . . ? V4 O18 V6 91.1(3) . . ? V5 O18 V6 90.4(3) . . ? Mn1 O18 V1 98.8(3) . . ? V4 O18 V1 86.6(3) . . ? V5 O18 V1 86.5(3) . . ? V6 O18 V1 161.6(3) . . ? V4 O19 V1 109.1(4) . . ? V4 O19 V7 112.4(4) . . ? V1 O19 V7 104.2(4) . . ? V7 O20 V8 116.9(4) . . ? V3 O21 V3 116.8(6) . 10_554 ? V7 O22 V7 116.5(6) . 10_554 ? S1 O5W Nd1 139.9(5) . . ? O24 K1 O24 63.8(7) 8_574 . ? O24 K1 O11 111.4(3) 8_574 3_775 ? O24 K1 O11 111.4(3) . 3_775 ? O24 K1 O10 98.6(3) 8_574 5_575 ? O24 K1 O10 70.5(3) . 5_575 ? O11 K1 O10 147.5(3) 3_775 5_575 ? O24 K1 O10 70.5(2) 8_574 8_574 ? O24 K1 O10 98.6(3) . 8_574 ? O11 K1 O10 147.5(3) 3_775 8_574 ? O10 K1 O10 54.4(3) 5_575 8_574 ? O24 K1 V6 87.5(2) 8_574 8_574 ? O24 K1 V6 87.5(2) . 8_574 ? O11 K1 V6 157.4(4) 3_775 8_574 ? O10 K1 V6 27.47(17) 5_575 8_574 ? O10 K1 V6 27.47(17) 8_574 8_574 ? O24 K1 V6 85.4(2) 8_574 3_775 ? O24 K1 V6 85.4(2) . 3_775 ? O11 K1 V6 30.9(2) 3_775 3_775 ? O10 K1 V6 150.3(2) 5_575 3_775 ? O10 K1 V6 150.3(2) 8_574 3_775 ? V6 K1 V6 171.6(3) 8_574 3_775 ? O24 K1 S1 19.2(3) 8_574 8_574 ? O24 K1 S1 83.0(4) . 8_574 ? O11 K1 S1 105.7(2) 3_775 8_574 ? O10 K1 S1 106.7(3) 5_575 8_574 ? O10 K1 S1 64.95(19) 8_574 8_574 ? V6 K1 S1 88.17(15) 8_574 8_574 ? V6 K1 S1 86.57(16) 3_775 8_574 ? O24 K1 S1 83.0(4) 8_574 . ? O24 K1 S1 19.2(3) . . ? O11 K1 S1 105.7(2) 3_775 . ? O10 K1 S1 64.95(19) 5_575 . ? O10 K1 S1 106.7(3) 8_574 . ? V6 K1 S1 88.17(15) 8_574 . ? V6 K1 S1 86.57(16) 3_775 . ? S1 K1 S1 102.1(3) 8_574 . ? O24 K1 V4 133.5(3) 8_574 3_775 ? O24 K1 V4 105.5(3) . 3_775 ? O11 K1 V4 26.45(12) 3_775 3_775 ? O10 K1 V4 121.1(2) 5_575 3_775 ? O10 K1 V4 151.9(3) 8_574 3_775 ? V6 K1 V4 138.7(2) 8_574 3_775 ? V6 K1 V4 48.17(10) 3_775 3_775 ? S1 K1 V4 131.64(19) 8_574 3_775 ? S1 K1 V4 92.44(11) . 3_775 ? O24 K1 V4 105.5(3) 8_574 12_774 ? O24 K1 V4 133.5(3) . 12_774 ? O11 K1 V4 26.45(12) 3_775 12_774 ? O10 K1 V4 151.9(3) 5_575 12_774 ? O10 K1 V4 121.1(2) 8_574 12_774 ? V6 K1 V4 138.7(2) 8_574 12_774 ? V6 K1 V4 48.17(10) 3_775 12_774 ? S1 K1 V4 92.44(11) 8_574 12_774 ? S1 K1 V4 131.64(19) . 12_774 ? V4 K1 V4 47.12(11) 3_775 12_774 ? O24 K1 K1 42.7(2) 8_574 8_574 ? O24 K1 K1 42.7(2) . 8_574 ? O11 K1 K1 85.5(4) 3_775 8_574 ? O10 K1 K1 110.4(3) 5_575 8_574 ? O10 K1 K1 110.4(3) 8_574 8_574 ? V6 K1 K1 117.1(2) 8_574 8_574 ? V6 K1 K1 54.5(2) 3_775 8_574 ? S1 K1 K1 57.03(10) 8_574 8_574 ? S1 K1 K1 57.03(10) . 8_574 ? V4 K1 K1 97.2(3) 3_775 8_574 ? V4 K1 K1 97.2(3) 12_774 8_574 ? O24 S1 O5W 110.4(5) . 5_575 ? O24 S1 O5W 110.4(5) . 3_775 ? O5W S1 O5W 108.5(5) 5_575 3_775 ? O24 S1 O5W 110.4(5) . . ? O5W S1 O5W 108.5(5) 5_575 . ? O5W S1 O5W 108.5(5) 3_775 . ? O24 S1 K1 38.93(13) . 3_775 ? O5W S1 K1 79.6(4) 5_575 3_775 ? O5W S1 K1 145.6(5) 3_775 3_775 ? O5W S1 K1 99.7(4) . 3_775 ? O24 S1 K1 38.93(13) . . ? O5W S1 K1 99.7(4) 5_575 . ? O5W S1 K1 79.6(4) 3_775 . ? O5W S1 K1 145.6(5) . . ? K1 S1 K1 65.9(2) 3_775 . ? O24 S1 K1 38.93(13) . 8_574 ? O5W S1 K1 145.6(5) 5_575 8_574 ? O5W S1 K1 99.7(4) 3_775 8_574 ? O5W S1 K1 79.6(4) . 8_574 ? K1 S1 K1 65.9(2) 3_775 8_574 ? K1 S1 K1 65.9(2) . 8_574 ? S1 O24 K1 121.9(3) . 3_775 ? S1 O24 K1 121.9(3) . . ? K1 O24 K1 94.7(5) 3_775 . ? S1 O24 K1 121.9(3) . 8_574 ? K1 O24 K1 94.7(5) 3_775 8_574 ? K1 O24 K1 94.7(5) . 8_574 ? C3 C2 C3 118.9(13) 10_554 . ? C3 C2 C1 120.5(7) 10_554 . ? C3 C2 C1 120.5(7) . . ? C3 C4 C5 120.2(10) . . ? O51 C1 O51 113(2) . 10_554 ? O51 C1 C2 123.3(12) . . ? O51 C1 C2 123.3(12) 10_554 . ? N1 C5 C4 0.0(18) 10_554 10_554 ? N1 C5 C4 119.3(11) 10_554 . ? C4 C5 C4 119.3(11) 10_554 . ? C4 C3 C2 120.7(12) . . ? OW4 OW4 OW4 60.000(6) 8_584 3_885 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.566 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.245 _database_code_depnum_ccdc_archive 'CCDC 937963'