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ISSN: 2056-9890
Volume 71| Part 7| July 2015| Pages 786-790

Double salt crystal structure of nona­sodium di­hydrogen nona­vanadoplatinate(IV) tri­hydrogen nona­vanadoplatinate(IV) tetra­contahydrate: stepwise-protonated nona­vanadoplatinate(IV)

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aDepartment of Chemistry, Pukyong National University, 599-1 Daeyeon 3-dong, Nam-gu, Busan 608-737, Republic of Korea, and bResearch Institute of Natural Science, Gyeongsan National University, 501, Jinju-daero, Jinju, 660-701, Republic of Korea
*Correspondence e-mail: uklee@pknu.ac.kr

Edited by S. Parkin, University of Kentucky, USA (Received 26 May 2015; accepted 5 June 2015; online 13 June 2015)

Nonavanadoplatinate [PtIVV9O28]7−, which is the first heteropolyoxovanadate in the deca­vanadate framework, [V10O28]6−, has been investigated crystallographically. The title compound, Na9[H2PtIVV9O28][H3PtIVV9O28]·40H2O, was obtained by a hydro­thermal reaction at pH = 2. This compound contains two different protonated heteropolyoxovanadates, [H2PtIVV9O28]5− [polyanion (A)] and [H3PtIVV9O28]7− [polyanion (B)]. The locations of the H atoms on the protonated O atoms were observed in difference Fourier maps and confirmed by the inter­polyanion hydrogen bonds, bond-length elongation and bond-valence-sum (VBS) analysis. The two (Pt and V)-bound μ2-O atoms are protonated in both polyanions. The position of the third protonated O atom in polyanion (B) is an inter­esting feature of the structure, being located on one (V2)-bound μ2-O atom. The discrete heteropolyanions form a dimer, {H5[PtV9O28]2}9−, through five inter­polyanion hydrogen bonds. Additional O—H⋯O hydrogen bonds and interactions between Na+ cations and water molecules as well as terminal O atoms of one of the polyanions consolidate the crystal packing.

1. Chemical context

The deca­vanadate, [V10O28]6− (Evans, 1966[Evans, H. T. Jr (1966). Inorg. Chem. 5, 967-977.]), is a common isopolyanion in vanadium systems, although no corresponding framework species have been observed in Mo and W systems. The deca­vanadate framework has been substituted with PtIV, and we have previously reported structural studies and 195Pt and 51V NMR studies of the sodium salt, Na5[H2PtV9O28]·21H2O (Lee et al., 2008[Lee, U., Joo, H.-J., Park, K.-M., Mal, S. S., Kortz, U., Keita, B. & Nadjo, L. (2008). Angew. Chem. Int. Ed. 47, 793-796.]). The same heteropolyanions were also reported as the guanidinium salt, (CH6N3)5[H2PtV9O28] (Joo et al., 2011[Joo, H.-C., Park, K.-M. & Lee, U. (2011). Acta Cryst. E67, m1801-m1802.]) and as the potassium salt, K5[H2PtV9O28]·9H2O (Joo & Lee, 2015[Joo, H.-C. & Lee, U. (2015). Acta Cryst. E71, 647-649.]).

Konaka et al. (2011[Konaka, S., Ozawa, Y., Shonaka, T., Watanabe, S. & Yagasaki, A. (2011). Inorg. Chem. 50, 6183-6188.]) reported heteropolyanions that belong to the deca­vanadate structure type, including the Te derivative, [HnTeV9O28](5−n)− (n = 1 or 2). However, the Te heteroatom in that polyanion was disordered over two sites, which correspond to the Pt1 or Pt2 and V4 or V13 sites in the title compound. In contrast, the Pt atom shows no disorder in any of the three [H2PtV9O28]5− polyanions reported thus far. Recently, the crystal structures of Fe- and Ni-substituted deca­niobates, [H2FeIIINb9O28]6− and [H3NiIINb9O28]6− were reported as tetra­methyl­ammonium salts (Son et al., 2013[Son, J.-H., Ohlin, C. A. & Casey, W. H. (2013). Dalton Trans. 42, 7529-7533.]).

In our studies of Anderson-type heteropolyoxometalates (Anderson, 1937[Anderson, J. S. (1937). Nature, 140, 850.]) containing PtIV, [PtHnM6O24](8−n)− (M = Mo or W), we have found that gradual protonation is a typical characteristic of these compounds (Lee & Joo, 2004[Lee, U. & Joo, H.-C. (2004). Acta Cryst. E60, i86-i88.]; Izarova et al., 2012[Izarova, N. V., Pope, M. T. & Kortz, U. (2012). Angew. Chem. Int. Ed. 51, 9492-9510.]; Joo et al., 2015[Joo, H.-C., Park, K.-M. & Lee, U. (2015). Acta Cryst. E71, 268-271.]). We herein report the crystal structure of the title compound, a double salt containing stepwise-protonated nona­vanadoplatinate(IV) by two and three H+ ions.

2. Structural commentary

The title compound contains doubly and triply protonated nona­vanadoplatinates, [H2PtIVV9O28]5− [polyanion (A)] and [H3PtIVV9O28]4− [polyanion (B)]. Fig. 1[link] shows the structure of the title compound while Fig. 2[link] shows the structure of polyanions (A) and (B). The framework of [V10O28]6− has been studied in detail previously (Evans, 1966[Evans, H. T. Jr (1966). Inorg. Chem. 5, 967-977.]; Nowogrocki et al., 1997[Nowogrocki, G., Baudrin, E., Denis, S. & Touboul, M. (1997). Eur. J. Solid State Inorg. Chem. 34, 1011-1026.]). The O atoms of the polyanions were designated as OT (terminal V=O atom), OB (bridging μ2-O atom; V—O—V or V—O—Pt), OC {μ3-O atom; (V)3—O or (V)2—O—Pt} and OD {μ4-O atom; (V)4—O or (V)3—O—PT}. The nine [VO6] octa­hedra in the polyanions are distorted [V—O ranges 1.578 (6)–2.419 (5)Å], whereas in the [PtO6] octa­hedron, the Pt—O distances are all very similar [Pt—O ranges 1.966 (5)–2.025 (5) Å]. The H atoms of the protonated O atoms were found in difference Fourier maps and confirmed by the presence of inter­polyanion hydrogen bonds (Fig. 2[link]), bond-length elongation of V—OH (Table 1[link]), and the bond-valence sum (BVS; Brown & Altermatt, 1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]; Brese & O'Keeffe, 1991[Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192-197.]) analysis.

Table 1
Selected bond lengths (Å)

Pt1—O7B 2.012 (5) Pt2—O35B 2.015 (5)
Pt1—O8B 2.025 (5) Pt2—O36B 2.017 (5)
V1—O12B 1.830 (5) V10—O41B 1.820 (5)
V1—O16B 1.882 (5) V10—O44B 1.950 (6)
V1—O13B 1.882 (5) V10—O35B 2.059 (5)
V1—O7B 2.058 (5) V11—O42B 1.882 (5)
V2—O14B 1.841 (6) V11—O43B 1.905 (6)
V2—O15B 1.904 (5) V11—O36B 2.035 (5)
V2—O8B 2.076 (5) V12—O46B 1.853 (5)
V3—O19B 1.840 (5) V12—O47B 1.869 (6)
V3—O18B 1.883 (6) V12—O38B 2.103 (5)
V3—O10B 2.054 (5) V13—O38B 1.666 (5)
V4—O11B 1.675 (5) V13—O39B 1.683 (5)
V5—O17B 1.838 (5) V14—O45B 1.854 (5)
V5—O12B 1.842 (6) V14—O48B 1.904 (5)
V5—O20B 1.896 (5) V14—O39B 2.048 (5)
V5—O11B 2.059 (5) V15—O45B 1.824 (5)
V6—O13B 1.805 (5) V15—O41B 1.859 (5)
V6—O17B 1.843 (5) V16—O42B 1.808 (5)
V7—O18B 1.802 (5) V16—O46B 1.834 (5)
V7—O14B 1.847 (5) V17—O47B 1.821 (5)
V8—O15B 1.808 (5) V17—O43B 1.822 (6)
V8—O19B 1.840 (5) V18—O48B 1.779 (5)
V9—O20B 1.805 (5) V18—O44B 1.907 (5)
V9—O16B 1.851 (5)    
[Figure 1]
Figure 1
The mol­ecular entities in the crystal structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. The H atoms of the polyanion are presented as small spheres of arbitrary radius and the H atoms of water mol­ecules have been omitted for clarity.
[Figure 2]
Figure 2
The polyanion structure in the title compound with the atomic numbering scheme and displacement ellipsoids at the 30% probability level for non-H atoms. H atoms are presented as a small spheres of arbitrary radius.

The two (Pt and V)-bound μ2-O atoms, O7B, O8B in polyanion (A) and O35B, O36B in polyanion (B), are proton­ated. In addition, one (V2)-bound μ2-O, O44B in polyanion (B), is also protonated. These protons are particularly important in the solid state. Polyanion A and B are involved in forming a dimeric assembly, {H5[PtV9O28]2}9−, which is held together by two (Pt and V)-bound μ2-O(8B and 35B)–H(8 and 35)⋯(V2)-bound μ2-O(43B and 16B) (bridged O atom), two (Pt and V)-bound μ2-O(7B and 36B)— H(7 and 36)⋯(Pt and V2)-bound μ3-O(4C and 32C), and one (V2)-bound μ2-O44B—H44⋯ μ1-O21T (terminal O atom) hydrogen bonds (Fig. 3[link] and Table 2[link]), respectively. The O44B⋯O21T distance of 2.724 (8) Å is shorter than that of O15B⋯O50T [2.889 (8) Å] because O44B—H44⋯O21T forms hydrogen bonds. Considering the bond-length elongation of V10—O44B and V18—O44B in polyanion (B) and the bond angles of V10—O44B—V18, the O44B atoms should be protonated by H44 in polyanion (B) (Table 1[link]).

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O7B—H7⋯O32C 0.85 (3) 1.79 (3) 2.627 (7) 171 (8)
O8B—H8⋯O43B 0.86 (3) 1.89 (3) 2.737 (7) 169 (8)
O35B—H35⋯O16B 0.85 (3) 1.86 (4) 2.685 (7) 164 (9)
O36B—H36⋯O4C 0.84 (3) 1.79 (3) 2.628 (7) 174 (8)
O44B—H44⋯O21T 0.84 (3) 2.00 (6) 2.724 (8) 144 (8)
O1W—H1B⋯O40Bi 0.90 (3) 2.18 (9) 2.845 (9) 130 (9)
O2W—H2B⋯O47Bii 0.88 (3) 1.88 (3) 2.757 (8) 178 (12)
O3W—H3A⋯O39Bii 0.86 (3) 2.01 (4) 2.856 (9) 168 (10)
O3W—H3B⋯O33Ciii 0.87 (3) 1.97 (6) 2.795 (8) 159 (12)
O4W—H4A⋯O51Tiv 0.84 (3) 2.08 (3) 2.893 (8) 163 (8)
O4W—H4B⋯O41B 0.84 (3) 1.96 (4) 2.780 (8) 165 (10)
O5W—H5B⋯O46Biii 0.86 (3) 1.94 (5) 2.743 (8) 154 (9)
O6W—H6A⋯O7W 0.85 (3) 2.03 (3) 2.872 (9) 170 (9)
O6W—H6B⋯O48Bii 0.84 (3) 2.02 (5) 2.810 (8) 158 (9)
O7W—H7A⋯O28T 0.83 (3) 2.26 (5) 2.951 (8) 141 (8)
O7W—H7B⋯O34Wii 0.84 (3) 2.05 (6) 2.794 (10) 148 (8)
O8W—H8A⋯O17Bv 0.86 (3) 1.93 (5) 2.760 (8) 161 (9)
O8W—H8B⋯O23Tvi 0.85 (3) 2.12 (7) 2.872 (9) 148 (10)
O9W—H9A⋯O7B 0.85 (3) 2.01 (5) 2.826 (8) 161 (9)
O9W—H9B⋯O37W 0.84 (3) 2.39 (6) 3.073 (11) 138 (8)
O10W—H10A⋯O5Cv 0.88 (3) 1.92 (4) 2.782 (9) 165 (11)
O11W—H11A⋯O22Tvii 0.87 (3) 2.23 (5) 3.061 (8) 158 (9)
O12W—H12A⋯O42B 0.99 1.92 2.861 (8) 159
O12W—H12B⋯O53Tiii 0.99 2.00 2.956 (8) 160
O13W—H13A⋯O31C 0.99 1.84 2.831 (7) 176
O13W—H13B⋯O54Tiii 0.99 1.93 2.905 (8) 169
O14W—H14A⋯O35B 0.99 1.96 2.806 (8) 142
O14W—H14B⋯O31W 0.99 2.03 2.928 (8) 151
O15W—H15A⋯O4W 0.99 1.92 2.819 (9) 149
O16W—H16A⋯O20B 0.99 2.51 3.054 (7) 115
O16W—H16B⋯O33Wiv 0.99 1.88 2.764 (9) 147
O17W—H17A⋯O37Biv 0.99 2.06 3.013 (8) 162
O17W—H17A⋯O50Tiv 0.99 2.60 3.205 (8) 119
O18W—H18A⋯O39Wvi 0.99 1.97 2.942 (10) 167
O18W—H18B⋯O12Bviii 0.99 2.01 2.977 (8) 165
O19W—H19A⋯O9W 0.99 2.05 2.949 (9) 149
O19W—H19B⋯O8B 0.99 1.99 2.867 (8) 146
O20W—H20A⋯O32W 0.99 1.94 2.857 (9) 152
O20W—H20B⋯O19Bvi 0.99 1.81 2.753 (8) 157
O21W—H21A⋯O37W 0.99 1.93 2.836 (10) 151
O21W—H21B⋯O6Cvi 0.99 1.90 2.869 (8) 164
O22W—H22A⋯O25Tv 0.99 1.94 2.920 (8) 170
O22W—H22B⋯O3C 0.99 1.83 2.819 (7) 173
O23W—H23A⋯O26Tv 0.99 2.04 2.993 (8) 160
O23W—H23B⋯O13B 0.99 1.87 2.840 (8) 167
O24W—H24A⋯O11Bvi 0.99 1.97 2.887 (9) 152
O24W—H24B⋯O10W 0.99 2.15 3.082 (13) 157
O25W—H25A⋯O9Bvii 0.99 2.07 2.874 (9) 137
O25W—H25B⋯O35W 0.99 1.93 2.880 (10) 160
O26W—H26A⋯O11Wi 0.99 1.88 2.848 (11) 165
O26W—H26B⋯O38W 0.99 1.86 2.811 (12) 161
O27W—H27A⋯O36W 0.98 2.11 2.881 (10) 135
O27W—H27B⋯O29Wix 0.98 2.09 2.891 (10) 138
O28W—H28A⋯O27Wix 0.98 1.78 2.692 (11) 153
O28W—H28B⋯O40Bi 0.98 2.45 2.994 (9) 115
O29W—H29A⋯O38Bii 0.98 2.12 2.992 (8) 147
O29W—H29B⋯O45Biii 0.98 1.93 2.755 (8) 141
O30W—H30A⋯O2W 0.98 2.03 2.877 (10) 143
O30W—H30B⋯O37Wii 0.98 1.93 2.893 (10) 167
O31W—H31B⋯O36B 0.98 2.08 2.812 (8) 130
O32W—H32A⋯O40Wvi 0.98 1.96 2.901 (13) 160
O32W—H32B⋯O2Wvi 0.98 2.01 2.896 (10) 150
O33W—H33A⋯O38W 0.98 2.13 2.833 (11) 128
O33W—H33B⋯O14B 0.98 1.81 2.786 (8) 178
O34W—H34A⋯O55T 0.98 2.29 3.038 (9) 132
O34W—H34B⋯O39Wvii 0.98 2.02 2.979 (12) 166
Symmetry codes: (i) x-1, y-1, z; (ii) x, y-1, z; (iii) -x+1, -y+1, -z; (iv) x+1, y, z; (v) -x+1, -y+2, -z+1; (vi) x, y+1, z; (vii) x+1, y+1, z; (viii) x-1, y, z; (ix) -x, -y, -z.
[Figure 3]
Figure 3
Polyhedral view of the heteropolyanion in the title compound, with O—H⋯O contacts of the inter­anion hydrogen bonds shown as red dashed lines.

Confirmation of the protonated O atoms was strongly supported by the BVS analysis. The BVSs for O7B and O8B in polyanion (A), and for O35B, O36B, and O44B in polyanion (B) are 1.20, 1.15, 1.19, 1.22, and 1.42 valence units (v.u.), respectively, if the valence of the O—H bond is not included. Because the BVS value around the μ2-O (OB) atom should be 2.0 v.u., the missing valences of O7B, O8B, O35B, O36B, and O44B are 0.80, 0.85, 0.81, 0.78, and 0.58 v.u., respectively, corresponding to the valence of the O—H bonds. The BVSs around the other unprotonated μ2-O atoms in polyanion (B) for O41B–-O43B and O45B—O48B are 1.82, 1.80, 1.71, 1.81, 1.79, 1.79, and 1.83 v.u., respectively, if the valence of the OB⋯H—OW hydrogen bonds and OB⋯Na+ inter­actions are not included. The missing valences of these OB atoms correspond to the valences of the OB⋯H—OW hydrogen bonds and OB⋯Na+ inter­actions. The smallest BVS value in the other unprotonated μ2-OB and μ3-OC atoms in polyanion (A) is 1.69 v.u. for O16B. O16B in polyanion (A) corresponds to O44B in polyanion (B), which is protonated. Similar results were observed for the sodium (Lee et al., 2008[Lee, U., Joo, H.-J., Park, K.-M., Mal, S. S., Kortz, U., Keita, B. & Nadjo, L. (2008). Angew. Chem. Int. Ed. 47, 793-796.]), guanidinium (Joo et al., 2011[Joo, H.-C., Park, K.-M. & Lee, U. (2011). Acta Cryst. E67, m1801-m1802.]), and potassium (Joo & Lee, 2015[Joo, H.-C. & Lee, U. (2015). Acta Cryst. E71, 647-649.]) salts of [H2PtV9O28]5−.

The Na1–Na6 ions are coordinated by six OW atoms in the range 2.339 (8)–2.742 (9) Å, and the Na7 and Na8 ions are coord­in­ated by five OW and one OT atoms in the range 2.373 (6)–2.454 (6) Å. The Na9 ions are coordinated by four OW atoms in the range 2.204 (11)–2.410 (9) Å.

3. Supra­molecular features

Polyanions (A) and (B) are involved in forming the dimeric assembly, {H5[PtV9O28]2}9−. Furthermore, the polyanion dimers are three-dimensionally linked via Na+⋯OT inter­actions. All water mol­ecules except O15W, O26W, O27W, O30W and O32W are involved in an extensive hydrogen-bonding network with O atoms of the polyanions. (see Table 2[link]). Potential hydrogen-bond distances of O35W–O40W molecules are: O35W⋯O8Wiv 2.845 (10); O35W⋯O38W 2.735 (12); O36W⋯O1W 2.814 (11); O36W⋯O5Wviii 2.846 (11); O37W⋯O27Tvi 2.844 (9); O37W⋯O55T 2.952 (9); O38W⋯O24Tviii 2.828 (10); O39W⋯O40W 2.793 (14); O40W⋯O1W 2.778 (13); O40W⋯O50T 2.913 (11) Å (symmetry codes correspond to those in Table 2[link]).

4. Database survey

A number of nona­vanadoplatinate(IV) compounds have been reported: Na5[H2PtV9O28]·21H2O (Lee et al., 2008[Lee, U., Joo, H.-J., Park, K.-M., Mal, S. S., Kortz, U., Keita, B. & Nadjo, L. (2008). Angew. Chem. Int. Ed. 47, 793-796.]); (CH6N3)5[H2PtV9O28] (Joo et al., 2011[Joo, H.-C., Park, K.-M. & Lee, U. (2011). Acta Cryst. E67, m1801-m1802.]); K5[H2PtV9O28]·9H2O (Joo & Lee, 2015[Joo, H.-C. & Lee, U. (2015). Acta Cryst. E71, 647-649.]). In addition, related structures of nona­vanadotellurate(VI), and nona­niobatoferrate(III) and nona­niobatonickelate(II) have been reported: [HnTeV9O28](5−n)− (n = 1 or 2) (Konaka et al., 2011[Konaka, S., Ozawa, Y., Shonaka, T., Watanabe, S. & Yagasaki, A. (2011). Inorg. Chem. 50, 6183-6188.]); [H2FeIIINb9O28]6− and [H3NiIINb9O28]6− (Son et al., 2013[Son, J.-H., Ohlin, C. A. & Casey, W. H. (2013). Dalton Trans. 42, 7529-7533.]).

5. Synthesis and crystallization

Single crystals of the title compound were obtained in the same way as the sodium salt reported by Lee et al. (2008[Lee, U., Joo, H.-J., Park, K.-M., Mal, S. S., Kortz, U., Keita, B. & Nadjo, L. (2008). Angew. Chem. Int. Ed. 47, 793-796.]), at pH 2.0.

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3[link]. All H atoms in the polyanions and water mol­ecules O1W–O11W were found in difference Fourier maps, and were refined with 1,2 and 1,3 distance restraints of O—H = 0.85 (3) Å and H⋯H = 1.50 (2) Å, respectively using the command DFIX in SHELXL2014/7 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]) and were included in the refinement with Uiso(H) = 1.5 Ueq(O). The H atoms of O12W–O26W were positioned geometrically and refined using a riding model (HFIX 23), with OW—H = 0.99 Å and Uiso (H) = 1.5Ueq (O). The H atoms of O27W–O34W were positioned geometrically and refined using a riding model (HFIX 137), with OW—H = 0.98 Å and Uiso (H) = 1.5Ueq (O). All invalid H atoms were removed in the final step of refinement. The H atoms of O35W–O40W were omitted in the refinement because they were not coordinated to Na+ ions and because they generated level A alerts in the checkCIF program due to short inter­molecular D—H⋯H—D contacts. The highest peak in the difference map was 1.78 Å from H17B and the largest hole is 0.87 Å from Pt2. The highest peak was considered as a half-occupancy water mol­ecule but it was excluded in the final stage of refinement because it was too close to the neighboring water mol­ecule.

Table 3
Experimental details

Crystal data
Chemical formula Na9[H2PtV9O28][H3PtV9O28]·40H2O
Mr 1567.84
Crystal system, space group Triclinic, P[\overline{1}]
Temperature (K) 173
a, b, c (Å) 12.706 (1), 12.875 (1), 28.319 (2)
α, β, γ (°) 93.760 (1), 98.449 (1), 113.318 (1)
V3) 4168.9 (5)
Z 4
Radiation type Mo Kα
μ (mm−1) 5.44
Crystal size (mm) 0.40 × 0.20 × 0.20
 
Data collection
Diffractometer Bruker SMART CCD
Absorption correction Multi-scan (SADABS; Bruker, 1997[Bruker (1997). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.])
Tmin, Tmax 0.515, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections 37312, 19046, 13416
Rint 0.039
(sin θ/λ)max−1) 0.666
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.053, 0.115, 1.05
No. of reflections 19046
No. of parameters 1203
No. of restraints 38
H-atom treatment Only H-atom coordinates refined
Δρmax, Δρmin (e Å−3) 2.99, −2.15
Computer programs: SMART and SAINT (Bruker, 1997[Bruker (1997). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXL2014 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]), ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and DIAMOND (Brandenburg, 1998[Brandenburg, K. (1998). DIAMOND. Crystal Impact GbR, Bonn, Germany.]).

Supporting information


Chemical context top

The decavanadate, [V10O28]6- (Evans, 1966), is a common isopolyanion in vanadium systems, although no corresponding framework species have been observed in Mo and W systems. The decavanadate framework has been substituted with PtIV, and we have previously reported structural studies and 195Pt and 51V NMR studies of the sodium salt, Na5[H2PtV9O28]·21H2O (Lee et al., 2008). The same heteropolyanions were also reported as the guanidinium salt, (CH6N3)5 [H2PtV9O28] (Joo et al., 2011) and as the potassium salt, K5 [H2PtV9O28]·9H2O (Joo & Lee, 2015).

Konaka et al. (2011) reported heteropolyanions that belong to the decavanadate structure type, including the Te derivative, [HnTeV9O28](5-n)- (n = 1 or 2). However, the Te heteroatom in that polyanion was disordered over two sites, which correspond to the Pt1 or Pt2 and V4 or V13 sites in the title compound. In contrast, the Pt atom shows no disorder in any of the three [H2PtV9O28]5- polyanions reported thus far. Recently, the crystal structures of Fe- and Ni-substituted decaniobates, [H2FeIIINb9O28]6- and [H3NiIINb9O28]6- were reported as tetra­methyl­ammonium salts (Son et al., 2013).

In our studies of Anderson-type heteropolyoxometalates (Anderson, 1937) containing PtIV, [PtHnM6O24](8-n)- (M = Mo or W), we have found that gradual protonation is a typical characteristic of these compounds (Lee & Joo, 2004; Izarova et al., 2012; Joo et al., 2015). We herein report the crystal structure of the title compound, a double salt containing stepwise-protonated nonavanadoplatinate (IV) by two and three H+ ions.

Structural commentary top

The title compound contains doubly and triply protonated nonavanadoplatinates, [H2PtIVV9O28]5- [polyanion (A)] and [H3PtIVV9O28]7- [polyanion (B)]. Fig. 1 shows the structure of the title compound while Fig. 2 shows the structure of polyanions (A) and (B). The framework of [V10O28]6- has been studied in detail previously (Evans, 1966; Nowogrocki et al., 1997). The O atoms of the clusters were designated as OT (terminal VO atom), OB (O-bridged µ2-O atom; V—O—V or V—O—Pt), OC3-O atom; (V)3—O or (V)2—O—Pt} and OD4-O atom; (V)4—O or (V)3—O—PT}. The nine [VO6] o­cta­hedra in the polyanions are distorted [V—O ranges 1.578 (6)–2.419 (5)Å], whereas in the [PtO6] o­cta­hedron, the Pt—O distances are all very similar [Pt—O ranges 1.966 (5)–2.025 (5) Å] . The H atoms of the protonated O atoms were found in difference Fourier maps and confirmed by the presence of inter­polyanion hydrogen bonds (Fig. 2), bond-distance elongation of V—OH (Table 1), and the bond-valence sum (BVS; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991) analysis.

The two (Pt and V)-bound µ2-O atoms, O7B, O8B in polyanion (A) and O35B, O36B in polyanion (B), are protonated. In addition, one (V2)-bound µ2-O, O44B in polyanion (B), is also protonated. These protons are particularly important in the solid state. Polyanion A and B are involved in forming a dimeric assembly, {H5[PtV9O28]2}9-, which is held together by two (Pt and V)-bound µ2-O(8B and 35B)–H(8 and 35)···(V2)-bound µ2-O(43B and 16B) (bridged O atom), two (Pt and V)-bound µ2-O(7B and 36B)— H(7 and 36)···(Pt and V2)-bound µ3-O(4C and 32C), and one (V2)-bound µ2-O44B—H44··· µ1-O21T (terminal O atom) hydrogen bonds (Fig. 2 and Table 2), respectively. The O44B···O21T distance of 2.724 (8) Å is shorter than that of O15B···O50T [2.889 (8) Å] because O44B—H44···O21T forms hydrogen bonds. Considering the bond-distance elongation of V10—O44B and V18—O44B in polyanion (B) and the bond angles of V10—O44B—V18, the O44B atoms should be protonated by H44 in polyanion (B) (Table 1).

Confirmation of the protonated O atoms was strongly supported by the BVS analysis. The BVSs for O7B and O8B in polyanion (A), and for O35B, O36B, and O44B in polyanion (B) are 1.20, 1.15, 1.19, 1.22, and 1.42 valence units (v.u.), respectively, if the valence of the O—H bond is not included. Because the BVS value around the µ2-O (OB) atom should be 2.0 v.u., the missing valences of O7B, O8B, O35B, O36B, and O44B are 0.80, 0.85, 0.81, 0.78, and 0.58 v.u., respectively, corresponding to the valence of the O—H bonds. The BVSs around the other unprotonated µ2-O atoms in polyanion (B) for O41B–-O43B and O45B—O48B are 1.82, 1.80, 1.71, 1.81, 1.79, 1.79, and 1.83 v.u., respectively, if the valence of the OB···H—OW hydrogen bonds and OB···K+ inter­actions are not included. The missing valences of these OB atoms correspond to the valences of the OB···H—OW hydrogen bonds and OB···K+ inter­actions. The smallest BVS value in the other unprotonated µ2-OB and µ3-OC atoms in polyanion (A) is 1.69 v.u. for O16B. O16B in polyanion (A) corresponds to O44B in polyanion (B), which is protonated. Similar results were observed for the sodium (Lee et al., 2008), guanidinium (Joo et al., 2011), and potassium (Joo & Lee, 2015) salts of [H2PtV9O28]5-.

The Na1–Na6 ions are coordinated by six OW in the range 2.339 (8)–2.742 (9) Å, and the Na7 and Na8 ions are coordinated by five OW and one OT atoms in the range 2.373 (6)–2.454 (6) Å. The Na9 ions are coordinated by four OW atoms in the range 2.204 (11)–2.410 (9) Å.

Supra­molecular features top

Polyanions (A) and (B) are involved in forming the dimeric assembly, {H5[PtV9O28]2}9-. Furthermore, the polyanion dimers are three-dimensionally linked via Na+···OT inter­actions. All water molecules except O15W, O26W, O27W, O30W and O32W are involved in an extensive hydrogen-bonding network with O atoms of the polyanions. (see Table 2).

Potential hydrogen-bond distances of O35W–O40W molecules are: O35W···O8Wiv 2.845 (10); O35W···O38W 2.735 (12); O36W···O1W 2.814 (11); O36W···O5Wviii 2.846 (11); O37W···O27Tvi 2.844 (9); O37W···O55T 2.952 (9); O38W···O24Tviii 2.828 (10); O39W···O40W 2.793 (14); O40W···O1W 2.778 (13); O40W···O50T 2.913 (11) (symmetry codes correspond to those in Table 2).

Database survey top

A number of nonavanadoplatinate (IV) heteropolyoxomolybdates have been reported: Na5[H2PtV9O28]·21H2O (Lee et al., 2008); (CH6N3)5 [H2PtV9O28] (Joo et al., 2011); K5 [H2PtV9O28]·9H2O (Joo & Lee, 2015). In addition, related structures of nonavanadotellurate(VI), and nonaniobatoferrate(III) and nonaniobatonickelate(II) have been reported: [HnTeV9O28](5-n)- (n = 1 or 2) (Konaka et al., 2011); [H2FeIIINb9O28]6- and [H3NiIINb9O28]6- (Son et al., 2013).

Synthesis and crystallization top

Single crystals of the title compound were obtained in the same way as the sodium salt reported by Lee et al. (2008), using K2Pt(OH)6 and KVO3 at pH 2.0.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 3. All H atoms in the polyanions and water molecules O1W–O11W were found in difference Fourier maps, and were refined using 1,2 and 1,3 distance restraints of O—H = 0.85 (3) Å and H···H = 1.50 (2) Å, respectively using the command DFIX in SHELXL2014/7 (Sheldrick, 2015) and were included in the refinement with Uiso(H) = 1.5 Ueq(O). The H atoms of O12W–O26W were positioned geometrically and refined using a riding model (HFIX 23), with OW—H = 0.99 Å and Uiso (H) = 1.5Ueq (O). The H atoms of O27W–O34W were positioned geometrically and refined using a riding model (HFIX 137), with OW-–H = 0.98 Å and Uiso (H) = 1.5Ueq (O). All invalid H atoms were removed in the final step of refinement. The H atoms of O35W–O40W were omitted in the refinement because they were not coordinated to Na+ ions and because they generated level A alerts in the checkCIF program due to short inter­molecular D—H···H—D contacts. The highest peak in the difference map was 1.78 Å from H17B and the largest hole is 0.87 Å from Pt2. The highest peak was considered as a half-occupancy water molecule but it was excluded in the final stage of refinement because it was too close to the neighboring water molecule.

Related literature top

For related literature, see: Anderson (1937); Brese & O'Keeffe (1991); Brown & Altermatt (1985); Evans (1966); Izarova et al. (2012); Joo & Lee (2015); Joo et al. (2011); Joo, Park & Lee (2015); Konaka et al. (2011); Lee & Joo (2004); Lee et al. (2008); Sheldrick (2015); Son et al. (2013).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXL2014 (Sheldrick, 2015); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. The H atoms of the polyanion are presented as small spheres of arbitrary radius and the H atoms of water molecules have been omitted for clarity.
[Figure 2] Fig. 2. The polyanion structure in the title compound with the atomic numbering scheme and displacement ellipsoids at the 30% probability level for non-H atoms. H atoms are presented as a small spheres of arbitrary radius.
[Figure 3] Fig. 3. Polyhedral view of the heteropolyanion in the title compound, with O—H···O contacts of the interanion hydrogen bonds shown as red dashed lines.
Nonasodium dihydrogen nonavanadoplatinate(IV) trihydrogen nonavanadoplatinate(IV) tetracontahydrate top
Crystal data top
Na9[H2PtV9O28][H3PtV9O28]·40H2OZ = 4
Mr = 1567.84F(000) = 3044
Triclinic, P1Dx = 2.498 Mg m3
a = 12.706 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.875 (1) ÅCell parameters from 7031 reflections
c = 28.319 (2) Åθ = 2.5–28.3°
α = 93.760 (1)°µ = 5.44 mm1
β = 98.449 (1)°T = 173 K
γ = 113.318 (1)°Block, dark brown
V = 4168.9 (5) Å30.40 × 0.20 × 0.20 mm
Data collection top
Bruker SMART CCD
diffractometer
19046 independent reflections
Radiation source: fine-focus sealed tube13416 reflections with I > 2σ(I)
Detector resolution: 10.0 pixels mm-1Rint = 0.039
ϕ and ω scansθmax = 28.3°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 1997)
h = 1616
Tmin = 0.515, Tmax = 0.746k = 1616
37312 measured reflectionsl = 3636
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053Only H-atom coordinates refined
wR(F2) = 0.115 w = 1/[σ2(Fo2) + (0.0047P)2 + 66.1402P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
19046 reflectionsΔρmax = 2.99 e Å3
1203 parametersΔρmin = 2.15 e Å3
38 restraintsExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00027 (2)
Crystal data top
Na9[H2PtV9O28][H3PtV9O28]·40H2Oγ = 113.318 (1)°
Mr = 1567.84V = 4168.9 (5) Å3
Triclinic, P1Z = 4
a = 12.706 (1) ÅMo Kα radiation
b = 12.875 (1) ŵ = 5.44 mm1
c = 28.319 (2) ÅT = 173 K
α = 93.760 (1)°0.40 × 0.20 × 0.20 mm
β = 98.449 (1)°
Data collection top
Bruker SMART CCD
diffractometer
19046 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1997)
13416 reflections with I > 2σ(I)
Tmin = 0.515, Tmax = 0.746Rint = 0.039
37312 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05338 restraints
wR(F2) = 0.115Only H-atom coordinates refined
S = 1.05 w = 1/[σ2(Fo2) + (0.0047P)2 + 66.1402P]
where P = (Fo2 + 2Fc2)/3
19046 reflectionsΔρmax = 2.99 e Å3
1203 parametersΔρmin = 2.15 e Å3
Special details top

Geometry. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.45003 (2)0.74403 (2)0.33507 (2)0.00550 (7)
V10.71159 (11)0.91128 (11)0.33797 (5)0.0103 (3)
V20.18401 (11)0.58053 (11)0.33073 (5)0.0110 (3)
V30.26993 (11)0.45141 (12)0.40609 (5)0.0121 (3)
V40.53061 (10)0.61272 (11)0.41324 (5)0.0085 (3)
V50.78830 (11)0.78352 (11)0.41622 (5)0.0114 (3)
V60.60439 (11)0.88428 (11)0.43233 (5)0.0092 (3)
V70.34669 (11)0.71757 (11)0.42932 (5)0.0097 (3)
V80.36930 (11)0.48243 (11)0.31023 (5)0.0107 (3)
V90.63138 (10)0.64442 (11)0.31612 (5)0.0092 (3)
O1D0.5982 (4)0.7545 (4)0.37248 (18)0.0073 (10)
O2D0.3762 (4)0.6130 (4)0.36978 (19)0.0097 (11)
O3C0.4450 (4)0.8409 (4)0.39323 (18)0.0077 (10)
O4C0.4671 (4)0.6306 (4)0.28785 (18)0.0090 (11)
O5C0.5095 (4)0.7303 (4)0.45092 (18)0.0079 (10)
O6C0.5283 (4)0.5341 (4)0.35301 (18)0.0085 (11)
O7B0.5441 (4)0.8818 (4)0.30612 (19)0.0097 (11)*
H70.539 (7)0.871 (7)0.2760 (12)0.015*
O8B0.2886 (4)0.7184 (5)0.30061 (19)0.0099 (11)
H80.300 (7)0.719 (7)0.2716 (15)0.015*
O9B0.1471 (4)0.4637 (4)0.36745 (19)0.0120 (11)
O10B0.4427 (4)0.5006 (4)0.43593 (19)0.0107 (11)
O11B0.6689 (4)0.6432 (4)0.43874 (19)0.0108 (11)
O12B0.8313 (4)0.8977 (4)0.37779 (19)0.0113 (11)
O13B0.6724 (4)0.9768 (4)0.39029 (19)0.0110 (11)
O14B0.2173 (4)0.6896 (5)0.38265 (19)0.0126 (12)
O15B0.2350 (4)0.4964 (5)0.2887 (2)0.0133 (12)
O16B0.6928 (4)0.7852 (4)0.29471 (19)0.0119 (11)
O17B0.7368 (4)0.8638 (4)0.45617 (18)0.0104 (11)
O18B0.2870 (4)0.5785 (5)0.4484 (2)0.0138 (12)
O19B0.3080 (4)0.3884 (4)0.35454 (19)0.0125 (11)
O20B0.7577 (4)0.6737 (4)0.36218 (19)0.0114 (11)
O21T0.7782 (4)1.0172 (5)0.3111 (2)0.0138 (12)
O22T0.0600 (5)0.5678 (5)0.3020 (2)0.0159 (12)
O23T0.2087 (5)0.3473 (5)0.4344 (2)0.0182 (13)
O24T0.9056 (5)0.7901 (5)0.4468 (2)0.0197 (13)
O25T0.5988 (5)0.9681 (5)0.47535 (19)0.0147 (12)
O26T0.3380 (5)0.7994 (5)0.4727 (2)0.0155 (12)
O27T0.3765 (5)0.3963 (5)0.2688 (2)0.0173 (12)
O28T0.6421 (5)0.5584 (5)0.2754 (2)0.0153 (12)
Pt20.53911 (2)0.75266 (2)0.16508 (2)0.00586 (7)
V100.80443 (11)0.91131 (12)0.17061 (5)0.0122 (3)
V110.27684 (11)0.58186 (11)0.16058 (5)0.0115 (3)
V120.20221 (11)0.71474 (11)0.08364 (5)0.0114 (3)
V130.46057 (11)0.88413 (11)0.08640 (5)0.0086 (3)
V140.72497 (11)1.04265 (11)0.09456 (5)0.0119 (3)
V150.64396 (11)0.77619 (11)0.07139 (5)0.0097 (3)
V160.38604 (11)0.61354 (11)0.06679 (5)0.0098 (3)
V170.35747 (11)0.84849 (11)0.18413 (5)0.0102 (3)
V180.61454 (11)1.01700 (11)0.18801 (5)0.0102 (3)
O29D0.6175 (4)0.8848 (4)0.13261 (18)0.0088 (11)
O30D0.3927 (4)0.7441 (4)0.12588 (19)0.0087 (11)
O31C0.5470 (4)0.6575 (4)0.10733 (18)0.0086 (11)
O32C0.5210 (4)0.8660 (4)0.21187 (18)0.0095 (11)
O33C0.4847 (4)0.7683 (4)0.04911 (19)0.0109 (11)
O34C0.4619 (4)0.9637 (4)0.14678 (18)0.0096 (11)
O35B0.6982 (4)0.7753 (5)0.20013 (19)0.0102 (11)
H350.708 (7)0.790 (7)0.2306 (11)0.015*
O36B0.4423 (4)0.6146 (4)0.19353 (18)0.0095 (11)
H360.456 (7)0.622 (7)0.2239 (11)0.014*
O37B0.1590 (4)0.5998 (5)0.12020 (19)0.0126 (11)
O38B0.3245 (4)0.8564 (5)0.05981 (18)0.0113 (11)
O39B0.5532 (4)0.9973 (5)0.06518 (19)0.0121 (11)
O40B0.8440 (4)1.0311 (5)0.13493 (19)0.0132 (12)
O41B0.7744 (4)0.8063 (4)0.11859 (18)0.0107 (11)
O42B0.3181 (4)0.5186 (4)0.10828 (18)0.0108 (11)
O43B0.2940 (4)0.7090 (5)0.20421 (19)0.0129 (11)
O44B0.7532 (4)0.9993 (5)0.21330 (19)0.0119 (11)
H440.792 (7)1.017 (7)0.2416 (15)0.018*
O45B0.7080 (4)0.9175 (4)0.05283 (19)0.0116 (11)
O46B0.2550 (4)0.6353 (5)0.04306 (19)0.0125 (11)
O47B0.2332 (4)0.8236 (5)0.13672 (19)0.0132 (12)
O48B0.6835 (4)1.1086 (4)0.14703 (19)0.0121 (11)
O49T0.9260 (5)0.9248 (5)0.2009 (2)0.0199 (13)
O50T0.2067 (5)0.4744 (5)0.1849 (2)0.0183 (13)
O51T0.0834 (5)0.7074 (5)0.0525 (2)0.0178 (13)
O52T0.7884 (5)1.1476 (5)0.0677 (2)0.0180 (13)
O53T0.6564 (5)0.6969 (5)0.0290 (2)0.0153 (12)
O54T0.3952 (5)0.5322 (5)0.02373 (19)0.0143 (12)
O55T0.6068 (5)1.0995 (5)0.2310 (2)0.0179 (12)
O56T0.3456 (5)0.9345 (5)0.2243 (2)0.0169 (12)
Na10.1461 (3)0.1283 (3)0.07263 (15)0.0339 (9)
Na20.5008 (3)0.3083 (3)0.11131 (12)0.0174 (7)
Na30.7943 (3)0.4930 (3)0.11847 (12)0.0194 (7)
Na40.2007 (3)1.0129 (3)0.38164 (12)0.0167 (7)
Na50.4888 (3)1.1888 (3)0.38675 (11)0.0155 (7)
Na60.7798 (3)1.3553 (3)0.38754 (14)0.0265 (8)
Na70.9239 (3)0.5954 (3)0.23834 (12)0.0199 (7)
Na80.0689 (3)0.9108 (3)0.26382 (12)0.0197 (7)
Na90.1092 (4)0.4763 (4)0.48275 (18)0.0510 (12)
O1W0.0600 (6)0.2091 (6)0.1273 (3)0.0383 (17)
H1A0.033 (8)0.165 (9)0.098 (2)0.057*
H1B0.008 (5)0.194 (10)0.137 (3)0.057*
O2W0.1628 (7)0.0001 (6)0.1445 (3)0.0374 (18)
H2A0.093 (5)0.031 (8)0.125 (4)0.056*
H2B0.184 (8)0.057 (6)0.143 (4)0.056*
O3W0.5461 (8)0.2114 (6)0.0491 (2)0.044 (2)
H3A0.540 (11)0.142 (4)0.050 (4)0.065*
H3B0.519 (10)0.215 (9)0.0197 (18)0.065*
O4W0.9156 (5)0.6885 (6)0.1140 (2)0.0226 (14)
H4A0.954 (7)0.696 (8)0.092 (3)0.034*
H4B0.866 (7)0.717 (8)0.110 (3)0.034*
O5W0.8156 (6)0.3811 (6)0.0545 (2)0.0289 (15)
H5A0.879 (6)0.441 (6)0.052 (3)0.043*
H5B0.779 (7)0.355 (8)0.0253 (16)0.043*
O6W0.6875 (5)0.3288 (5)0.1561 (2)0.0205 (13)
H6A0.711 (8)0.349 (7)0.1864 (12)0.031*
H6B0.698 (8)0.270 (5)0.148 (3)0.031*
O7W0.7774 (6)0.4251 (6)0.2556 (2)0.0247 (14)
H7A0.734 (7)0.440 (8)0.271 (3)0.037*
H7B0.803 (8)0.378 (7)0.266 (3)0.037*
O8W0.1747 (6)1.1174 (6)0.4471 (2)0.0305 (16)
H8A0.187 (9)1.110 (8)0.4771 (15)0.046*
H8B0.212 (9)1.186 (4)0.443 (3)0.046*
O9W0.4860 (6)1.0706 (6)0.3198 (2)0.0271 (15)
H9A0.495 (9)1.009 (5)0.321 (3)0.041*
H9B0.478 (9)1.085 (8)0.2913 (16)0.041*
O10W0.4923 (8)1.3096 (7)0.4538 (3)0.046 (2)
H10A0.503 (9)1.295 (11)0.4835 (19)0.069*
H10B0.418 (4)1.294 (12)0.447 (4)0.069*
O11W0.8894 (6)1.5425 (5)0.3708 (2)0.0250 (14)
H11A0.938 (6)1.568 (8)0.351 (3)0.037*
H11B0.823 (4)1.497 (7)0.351 (3)0.037*
O12W0.3096 (5)0.3022 (5)0.0720 (2)0.0181 (12)
H12A0.29710.36550.08840.027*
H12B0.31310.31560.03820.027*
O13W0.6077 (5)0.4766 (5)0.0792 (2)0.0170 (12)
H13A0.59050.54210.08980.025*
H13B0.59720.46460.04370.025*
O14W0.7541 (5)0.5871 (5)0.1854 (2)0.0174 (12)
H14A0.75690.66330.18020.026*
H14B0.68020.53980.19540.026*
O15W1.0571 (5)0.7556 (5)0.2066 (2)0.0243 (14)
H15A1.02460.76080.17330.036*
H15B1.13390.75240.20750.036*
O16W0.9349 (5)0.7502 (5)0.2956 (2)0.0228 (14)
H16A0.85800.75340.29460.027*
H16B0.96710.74490.32890.027*
O17W0.9596 (5)0.4918 (6)0.1720 (2)0.0279 (15)
H17A1.03500.53460.16220.042*
H17B0.95140.41420.17780.042*
O18W0.0315 (5)1.0158 (5)0.3297 (2)0.0209 (13)
H18A0.03961.09340.32380.031*
H18B0.04340.97300.33990.031*
O19W0.2389 (5)0.9159 (5)0.3135 (2)0.0183 (13)
H19A0.31210.96250.30290.027*
H19B0.23540.83930.31850.027*
O20W0.3058 (5)1.1735 (5)0.3436 (2)0.0173 (12)
H20A0.29591.15500.30830.026*
H20B0.28931.24090.35150.026*
O21W0.5954 (5)1.3463 (5)0.3459 (2)0.0210 (13)
H21A0.58221.32580.31060.032*
H21B0.58281.41600.35390.032*
O22W0.3846 (5)1.0217 (5)0.4204 (2)0.0161 (12)
H22A0.39651.03420.45600.024*
H22B0.39960.95510.40940.024*
O23W0.6749 (5)1.1915 (5)0.4225 (2)0.0183 (13)
H23A0.69061.20490.45820.027*
H23B0.68601.12300.41090.027*
O24W0.7492 (8)1.4650 (6)0.4535 (3)0.050 (2)
H24A0.74061.53240.44170.075*
H24B0.67531.41740.46330.075*
O25W0.9619 (6)1.3470 (7)0.4175 (3)0.0397 (18)
H25A1.00101.35060.38950.059*
H25B0.94221.26950.42660.059*
O26W0.0268 (7)0.6045 (7)0.4655 (3)0.055 (2)
H26A0.01030.59430.43120.082*
H26B0.08080.68520.47670.082*
O27W0.0246 (7)0.1633 (7)0.0101 (3)0.047 (2)
H27A0.04330.24520.01320.070*
H27B0.05720.12110.01260.070*
O28W0.0237 (6)0.0493 (7)0.0732 (3)0.0438 (19)
H28A0.02590.10860.04900.066*
H28B0.09490.03640.06550.066*
O29W0.2076 (5)0.0083 (5)0.0286 (2)0.0237 (14)
H29A0.23980.03170.05080.036*
H29B0.26780.05440.01150.036*
O30W0.4040 (5)0.1487 (5)0.1495 (2)0.0260 (15)
H30A0.31960.12620.14140.039*
H30B0.43020.16900.18450.039*
O31W0.5088 (5)0.4329 (5)0.1786 (2)0.0239 (14)
H31A0.49890.39200.20670.036*
H31B0.44610.45890.17150.036*
O32W0.1998 (6)1.0926 (6)0.2446 (2)0.0375 (18)
H32A0.16301.14660.24580.056*
H32B0.21521.08200.21210.056*
O33W0.0827 (5)0.8155 (5)0.3844 (2)0.0197 (13)
H33A0.04980.80840.41390.030*
H33B0.13100.77210.38440.030*
O34W0.7955 (7)1.2617 (6)0.3126 (3)0.0394 (18)
H34A0.72851.18780.30330.059*
H34B0.86771.24990.31750.059*
O35W0.9524 (6)1.1264 (6)0.4358 (3)0.0367 (17)
O36W0.0339 (7)0.3635 (6)0.0656 (3)0.044 (2)
O37W0.4813 (7)1.2430 (8)0.2503 (3)0.047 (2)
O38W0.1417 (7)0.8435 (8)0.4863 (3)0.057 (2)
O39W0.0156 (8)0.2317 (7)0.3108 (3)0.059 (2)
O40W0.1094 (9)0.2640 (8)0.2269 (3)0.073 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.00654 (13)0.00628 (15)0.00492 (15)0.00380 (11)0.00147 (10)0.00062 (11)
V10.0093 (6)0.0106 (7)0.0091 (7)0.0024 (5)0.0014 (5)0.0012 (5)
V20.0090 (6)0.0123 (7)0.0117 (7)0.0048 (5)0.0006 (5)0.0015 (5)
V30.0111 (6)0.0116 (7)0.0145 (7)0.0044 (5)0.0044 (5)0.0046 (6)
V40.0099 (6)0.0100 (6)0.0075 (6)0.0062 (5)0.0014 (5)0.0020 (5)
V50.0102 (6)0.0138 (7)0.0108 (7)0.0063 (5)0.0004 (5)0.0010 (6)
V60.0111 (6)0.0097 (6)0.0072 (6)0.0049 (5)0.0017 (5)0.0013 (5)
V70.0105 (6)0.0112 (7)0.0088 (7)0.0055 (5)0.0042 (5)0.0001 (5)
V80.0115 (6)0.0079 (6)0.0125 (7)0.0034 (5)0.0038 (5)0.0004 (5)
V90.0098 (6)0.0098 (6)0.0089 (7)0.0053 (5)0.0021 (5)0.0013 (5)
O1D0.008 (2)0.008 (3)0.004 (3)0.003 (2)0.0004 (18)0.001 (2)
O2D0.010 (2)0.011 (3)0.011 (3)0.005 (2)0.004 (2)0.003 (2)
O3C0.009 (2)0.005 (3)0.008 (3)0.003 (2)0.0015 (19)0.004 (2)
O4C0.010 (2)0.009 (3)0.009 (3)0.005 (2)0.003 (2)0.002 (2)
O5C0.011 (2)0.010 (3)0.006 (3)0.007 (2)0.0017 (19)0.002 (2)
O6C0.009 (2)0.009 (3)0.008 (3)0.003 (2)0.0025 (19)0.005 (2)
O8B0.008 (2)0.016 (3)0.008 (3)0.007 (2)0.003 (2)0.002 (2)
O9B0.011 (2)0.010 (3)0.015 (3)0.004 (2)0.003 (2)0.000 (2)
O10B0.013 (2)0.009 (3)0.012 (3)0.006 (2)0.003 (2)0.004 (2)
O11B0.009 (2)0.014 (3)0.012 (3)0.008 (2)0.000 (2)0.001 (2)
O12B0.010 (2)0.012 (3)0.009 (3)0.002 (2)0.001 (2)0.002 (2)
O13B0.012 (2)0.010 (3)0.008 (3)0.001 (2)0.000 (2)0.001 (2)
O14B0.010 (2)0.017 (3)0.015 (3)0.010 (2)0.003 (2)0.003 (2)
O15B0.011 (2)0.016 (3)0.015 (3)0.007 (2)0.003 (2)0.003 (2)
O16B0.014 (3)0.012 (3)0.011 (3)0.005 (2)0.008 (2)0.002 (2)
O17B0.014 (3)0.008 (3)0.007 (3)0.005 (2)0.001 (2)0.002 (2)
O18B0.012 (3)0.014 (3)0.018 (3)0.006 (2)0.008 (2)0.008 (2)
O19B0.013 (3)0.011 (3)0.015 (3)0.006 (2)0.003 (2)0.005 (2)
O20B0.009 (2)0.013 (3)0.015 (3)0.007 (2)0.002 (2)0.001 (2)
O21T0.012 (3)0.009 (3)0.017 (3)0.001 (2)0.004 (2)0.003 (2)
O22T0.015 (3)0.019 (3)0.016 (3)0.010 (2)0.002 (2)0.003 (2)
O23T0.018 (3)0.014 (3)0.023 (3)0.004 (2)0.007 (2)0.008 (3)
O24T0.016 (3)0.028 (4)0.016 (3)0.011 (3)0.000 (2)0.003 (3)
O25T0.019 (3)0.014 (3)0.010 (3)0.006 (2)0.004 (2)0.004 (2)
O26T0.015 (3)0.019 (3)0.017 (3)0.011 (2)0.006 (2)0.002 (2)
O27T0.018 (3)0.017 (3)0.019 (3)0.009 (2)0.005 (2)0.002 (2)
O28T0.016 (3)0.015 (3)0.018 (3)0.009 (2)0.007 (2)0.002 (2)
Pt20.00667 (13)0.00671 (15)0.00512 (15)0.00362 (11)0.00141 (10)0.00057 (11)
V100.0097 (6)0.0157 (7)0.0116 (7)0.0056 (5)0.0016 (5)0.0026 (6)
V110.0106 (6)0.0118 (7)0.0104 (7)0.0026 (5)0.0024 (5)0.0020 (5)
V120.0096 (6)0.0140 (7)0.0109 (7)0.0058 (5)0.0006 (5)0.0008 (6)
V130.0105 (6)0.0097 (6)0.0079 (6)0.0063 (5)0.0022 (5)0.0022 (5)
V140.0127 (6)0.0102 (7)0.0148 (7)0.0057 (5)0.0052 (5)0.0036 (6)
V150.0124 (6)0.0105 (7)0.0088 (7)0.0067 (5)0.0044 (5)0.0010 (5)
V160.0111 (6)0.0102 (7)0.0080 (6)0.0048 (5)0.0012 (5)0.0009 (5)
V170.0101 (6)0.0124 (7)0.0092 (7)0.0051 (5)0.0041 (5)0.0001 (5)
V180.0125 (6)0.0076 (6)0.0102 (7)0.0039 (5)0.0027 (5)0.0010 (5)
O29D0.008 (2)0.009 (3)0.009 (3)0.003 (2)0.003 (2)0.001 (2)
O30D0.007 (2)0.008 (3)0.012 (3)0.004 (2)0.0003 (19)0.000 (2)
O31C0.011 (2)0.007 (3)0.011 (3)0.006 (2)0.004 (2)0.003 (2)
O32C0.013 (2)0.011 (3)0.005 (3)0.006 (2)0.000 (2)0.002 (2)
O33C0.011 (2)0.013 (3)0.010 (3)0.006 (2)0.003 (2)0.003 (2)
O34C0.010 (2)0.009 (3)0.008 (3)0.004 (2)0.001 (2)0.001 (2)
O35B0.009 (2)0.012 (3)0.009 (3)0.004 (2)0.001 (2)0.001 (2)
O36B0.015 (3)0.009 (3)0.006 (2)0.004 (2)0.004 (2)0.003 (2)
O37B0.009 (2)0.013 (3)0.010 (3)0.001 (2)0.002 (2)0.001 (2)
O38B0.011 (2)0.014 (3)0.009 (3)0.005 (2)0.002 (2)0.002 (2)
O39B0.013 (3)0.016 (3)0.009 (3)0.008 (2)0.002 (2)0.003 (2)
O40B0.010 (2)0.015 (3)0.013 (3)0.003 (2)0.004 (2)0.000 (2)
O41B0.011 (2)0.013 (3)0.010 (3)0.006 (2)0.004 (2)0.002 (2)
O42B0.016 (3)0.011 (3)0.004 (3)0.005 (2)0.002 (2)0.001 (2)
O43B0.012 (2)0.014 (3)0.011 (3)0.003 (2)0.001 (2)0.002 (2)
O44B0.015 (3)0.012 (3)0.008 (3)0.006 (2)0.004 (2)0.001 (2)
O45B0.011 (2)0.012 (3)0.012 (3)0.005 (2)0.005 (2)0.001 (2)
O46B0.010 (2)0.017 (3)0.012 (3)0.007 (2)0.000 (2)0.003 (2)
O47B0.013 (3)0.020 (3)0.011 (3)0.011 (2)0.002 (2)0.003 (2)
O48B0.015 (3)0.009 (3)0.013 (3)0.005 (2)0.005 (2)0.001 (2)
O49T0.014 (3)0.022 (3)0.022 (3)0.006 (2)0.002 (2)0.008 (3)
O50T0.021 (3)0.020 (3)0.012 (3)0.007 (2)0.003 (2)0.007 (2)
O51T0.012 (3)0.024 (3)0.017 (3)0.010 (2)0.001 (2)0.001 (3)
O52T0.021 (3)0.015 (3)0.020 (3)0.008 (2)0.008 (2)0.007 (3)
O53T0.024 (3)0.016 (3)0.011 (3)0.012 (2)0.008 (2)0.005 (2)
O54T0.020 (3)0.013 (3)0.011 (3)0.008 (2)0.003 (2)0.001 (2)
O55T0.023 (3)0.016 (3)0.014 (3)0.007 (2)0.004 (2)0.000 (2)
O56T0.020 (3)0.019 (3)0.013 (3)0.011 (2)0.003 (2)0.003 (2)
Na10.035 (2)0.027 (2)0.040 (2)0.0101 (17)0.0161 (18)0.0027 (18)
Na20.0203 (16)0.0149 (17)0.0182 (18)0.0082 (14)0.0041 (13)0.0035 (14)
Na30.0195 (16)0.0193 (18)0.0210 (19)0.0094 (14)0.0050 (14)0.0011 (15)
Na40.0174 (15)0.0157 (17)0.0167 (18)0.0082 (13)0.0003 (13)0.0009 (14)
Na50.0170 (15)0.0152 (17)0.0138 (17)0.0063 (13)0.0024 (12)0.0009 (13)
Na60.0232 (18)0.0217 (18)0.039 (2)0.0115 (15)0.0097 (16)0.0091 (16)
Na70.0176 (16)0.0214 (18)0.0189 (18)0.0072 (14)0.0011 (13)0.0009 (14)
Na80.0191 (16)0.0192 (18)0.0192 (18)0.0078 (14)0.0001 (13)0.0018 (14)
Na90.047 (3)0.060 (3)0.051 (3)0.023 (2)0.017 (2)0.009 (2)
O1W0.031 (4)0.031 (4)0.050 (5)0.010 (3)0.009 (3)0.001 (3)
O2W0.060 (5)0.021 (4)0.047 (5)0.028 (4)0.024 (4)0.007 (3)
O3W0.111 (7)0.028 (4)0.006 (3)0.044 (5)0.007 (4)0.004 (3)
O4W0.023 (3)0.032 (4)0.025 (4)0.019 (3)0.012 (3)0.011 (3)
O5W0.047 (4)0.024 (4)0.011 (3)0.013 (3)0.002 (3)0.003 (3)
O6W0.025 (3)0.015 (3)0.022 (3)0.011 (3)0.001 (3)0.002 (3)
O7W0.028 (3)0.027 (4)0.024 (4)0.014 (3)0.010 (3)0.003 (3)
O8W0.046 (4)0.029 (4)0.022 (4)0.021 (3)0.005 (3)0.007 (3)
O9W0.049 (4)0.026 (4)0.015 (3)0.026 (3)0.007 (3)0.000 (3)
O10W0.093 (7)0.046 (5)0.026 (4)0.052 (5)0.017 (4)0.015 (4)
O11W0.033 (4)0.020 (3)0.024 (3)0.011 (3)0.010 (3)0.005 (3)
O12W0.024 (3)0.013 (3)0.018 (3)0.008 (2)0.005 (2)0.001 (2)
O13W0.021 (3)0.018 (3)0.016 (3)0.012 (2)0.005 (2)0.003 (2)
O14W0.018 (3)0.019 (3)0.018 (3)0.011 (2)0.005 (2)0.004 (3)
O15W0.018 (3)0.027 (4)0.026 (4)0.006 (3)0.009 (3)0.000 (3)
O16W0.017 (3)0.026 (3)0.025 (4)0.007 (3)0.010 (3)0.003 (3)
O17W0.021 (3)0.028 (4)0.033 (4)0.010 (3)0.003 (3)0.001 (3)
O18W0.017 (3)0.023 (3)0.026 (3)0.012 (3)0.003 (2)0.003 (3)
O19W0.018 (3)0.017 (3)0.022 (3)0.008 (2)0.007 (2)0.004 (3)
O20W0.020 (3)0.013 (3)0.022 (3)0.011 (2)0.003 (2)0.001 (2)
O21W0.024 (3)0.018 (3)0.025 (3)0.012 (3)0.006 (3)0.007 (3)
O22W0.019 (3)0.019 (3)0.014 (3)0.013 (2)0.001 (2)0.004 (2)
O23W0.018 (3)0.016 (3)0.022 (3)0.008 (2)0.002 (2)0.001 (3)
O24W0.089 (6)0.039 (4)0.060 (5)0.046 (5)0.061 (5)0.037 (4)
O25W0.031 (4)0.051 (5)0.051 (5)0.025 (4)0.016 (3)0.031 (4)
O26W0.044 (5)0.048 (5)0.069 (6)0.018 (4)0.000 (4)0.019 (5)
O27W0.050 (5)0.035 (4)0.053 (5)0.019 (4)0.002 (4)0.002 (4)
O28W0.031 (4)0.049 (5)0.057 (5)0.020 (4)0.016 (4)0.012 (4)
O29W0.030 (3)0.032 (4)0.020 (3)0.019 (3)0.014 (3)0.014 (3)
O30W0.026 (3)0.022 (3)0.033 (4)0.013 (3)0.008 (3)0.005 (3)
O31W0.033 (3)0.023 (3)0.021 (4)0.018 (3)0.004 (3)0.003 (3)
O32W0.043 (4)0.035 (4)0.023 (4)0.005 (3)0.004 (3)0.001 (3)
O33W0.023 (3)0.019 (3)0.022 (3)0.011 (3)0.010 (2)0.005 (3)
O34W0.052 (5)0.025 (4)0.041 (4)0.018 (3)0.001 (4)0.001 (3)
O35W0.033 (4)0.029 (4)0.038 (4)0.007 (3)0.005 (3)0.001 (3)
O36W0.052 (5)0.026 (4)0.044 (5)0.016 (4)0.014 (4)0.009 (4)
O37W0.061 (5)0.069 (5)0.031 (4)0.054 (5)0.002 (4)0.009 (4)
O38W0.044 (5)0.065 (6)0.059 (6)0.023 (4)0.003 (4)0.003 (5)
O39W0.058 (6)0.034 (5)0.081 (7)0.013 (4)0.013 (5)0.013 (5)
O40W0.075 (7)0.045 (5)0.064 (7)0.002 (5)0.015 (5)0.015 (5)
Geometric parameters (Å, º) top
Pt1—O1D1.970 (5)V17—O34C2.035 (5)
Pt1—O2D1.982 (5)V17—O30D2.265 (5)
Pt1—O4C2.012 (5)V17—V183.1050 (18)
Pt1—O7B2.012 (5)V18—O55T1.603 (6)
Pt1—O3C2.025 (5)V18—O48B1.779 (5)
Pt1—O8B2.025 (5)V18—O44B1.907 (5)
Pt1—V83.1038 (14)V18—O34C1.942 (5)
Pt1—V63.1065 (13)V18—O32C2.057 (5)
Pt1—V73.1239 (13)V18—O29D2.253 (5)
Pt1—V93.1393 (13)O35B—H350.85 (3)
Pt1—V13.1495 (13)O36B—H360.84 (3)
Pt1—V43.1627 (13)O44B—H440.84 (3)
V1—O21T1.603 (5)O49T—Na8ii2.420 (7)
V1—O12B1.830 (5)Na1—O29W2.353 (7)
V1—O16B1.882 (5)Na1—O27W2.360 (9)
V1—O13B1.882 (5)Na1—O12W2.379 (7)
V1—O7B2.058 (5)Na1—O1W2.421 (8)
V1—O1D2.340 (5)Na1—O28W2.448 (8)
V1—V53.1109 (19)Na1—O2W2.742 (9)
V2—O22T1.604 (5)Na2—O3W2.361 (7)
V2—O9B1.832 (6)Na2—O30W2.364 (7)
V2—O14B1.841 (6)Na2—O31W2.372 (7)
V2—O15B1.904 (5)Na2—O13W2.378 (6)
V2—O8B2.076 (5)Na2—O6W2.425 (7)
V2—O2D2.387 (5)Na2—O12W2.488 (7)
V2—V33.1190 (19)Na2—Na33.506 (4)
V3—O23T1.595 (6)Na3—O5W2.355 (7)
V3—O9B1.837 (5)Na3—O13W2.387 (6)
V3—O19B1.840 (5)Na3—O4W2.399 (7)
V3—O18B1.883 (6)Na3—O14W2.407 (6)
V3—O10B2.054 (5)Na3—O17W2.409 (7)
V3—O2D2.382 (5)Na3—O6W2.429 (7)
V3—V43.1027 (18)Na4—O8W2.358 (8)
V4—O10B1.674 (5)Na4—O22W2.387 (6)
V4—O11B1.675 (5)Na4—O20W2.397 (7)
V4—O6C1.916 (5)Na4—O33W2.400 (7)
V4—O5C1.922 (5)Na4—O18W2.436 (6)
V4—O2D2.159 (5)Na4—O19W2.441 (6)
V4—O1D2.174 (5)Na5—O9W2.339 (7)
V5—O24T1.578 (6)Na5—O10W2.357 (8)
V5—O17B1.838 (5)Na5—O22W2.382 (6)
V5—O12B1.842 (6)Na5—O20W2.389 (6)
V5—O20B1.896 (5)Na5—O23W2.418 (6)
V5—O11B2.059 (5)Na5—O21W2.425 (7)
V5—O1D2.419 (5)Na5—H10B2.59 (12)
V6—O25T1.602 (5)Na6—O23W2.375 (7)
V6—O13B1.805 (5)Na6—O11W2.380 (7)
V6—O17B1.843 (5)Na6—O25W2.390 (7)
V6—O3C2.001 (5)Na6—O21W2.417 (7)
V6—O5C2.023 (5)Na6—O24W2.436 (8)
V6—O1D2.271 (5)Na6—O34W2.444 (8)
V6—V73.1090 (18)Na7—O7W2.385 (7)
V7—O26T1.610 (5)Na7—O14W2.399 (6)
V7—O18B1.802 (5)Na7—O15W2.419 (7)
V7—O14B1.847 (5)Na7—O16W2.432 (7)
V7—O5C2.007 (5)Na7—O17W2.432 (7)
V7—O3C2.036 (5)Na7—O22Tii2.454 (6)
V7—O2D2.255 (5)Na8—O19W2.373 (6)
V8—O27T1.599 (6)Na8—O49Ti2.420 (7)
V8—O15B1.808 (5)Na8—O16Wi2.428 (7)
V8—O19B1.840 (5)Na8—O32W2.428 (8)
V8—O4C2.024 (5)Na8—O15Wi2.431 (7)
V8—O6C2.026 (5)Na8—O18W2.444 (7)
V8—O2D2.268 (5)Na9—O24Wiii2.204 (11)
V9—O28T1.603 (5)Na9—O26W2.319 (9)
V9—O20B1.805 (5)Na9—O26Wiv2.395 (10)
V9—O16B1.851 (5)Na9—O25Wv2.410 (9)
V9—O6C1.987 (5)O1W—H1A0.92 (3)
V9—O4C2.056 (5)O1W—H1B0.90 (3)
V9—O1D2.260 (5)O2W—H2A0.90 (3)
O7B—H70.85 (3)O2W—H2B0.88 (3)
O8B—H80.86 (3)O3W—H3A0.86 (3)
O15B—O50T2.889 (8)O3W—H3B0.87 (3)
O18B—Na92.498 (7)O4W—H4A0.84 (3)
O22T—Na7i2.454 (6)O4W—H4B0.84 (3)
O23T—Na92.847 (7)O5W—H5A0.87 (3)
Pt2—O29D1.966 (5)O5W—H5B0.86 (3)
Pt2—O30D1.980 (5)O6W—H6A0.85 (3)
Pt2—O32C2.010 (5)O6W—H6B0.84 (3)
Pt2—O35B2.015 (5)O7W—H7A0.83 (3)
Pt2—O31C2.017 (5)O7W—H7B0.84 (3)
Pt2—O36B2.017 (5)O8W—H8A0.86 (3)
Pt2—V173.1101 (13)O8W—H8B0.85 (3)
Pt2—V153.1193 (13)O9W—H9A0.85 (3)
Pt2—V163.1202 (13)O9W—H9B0.84 (3)
Pt2—V183.1413 (14)O10W—H10A0.88 (3)
Pt2—V103.1485 (13)O10W—H10B0.87 (3)
Pt2—V113.1613 (13)O11W—H11A0.87 (3)
V10—O49T1.590 (6)O11W—H11B0.89 (3)
V10—O41B1.820 (5)O12W—H12A0.9900
V10—O40B1.841 (6)O12W—H12B0.9900
V10—O44B1.950 (6)O13W—H13A0.9900
V10—O35B2.059 (5)O13W—H13B0.9900
V10—O29D2.340 (5)O14W—H14A0.9900
V10—V143.1158 (19)O14W—H14B0.9900
V11—O50T1.585 (6)O15W—H15A0.9900
V11—O37B1.846 (5)O15W—H15B0.9900
V11—O42B1.882 (5)O16W—H16A0.9900
V11—O43B1.905 (6)O16W—H16B0.9900
V11—O36B2.035 (5)O17W—H17A0.9900
V11—O30D2.399 (5)O17W—H17B0.9900
V12—O51T1.596 (5)O18W—H18A0.9900
V12—O37B1.813 (6)O18W—H18B0.9900
V12—O46B1.853 (5)O19W—H19A0.9900
V12—O47B1.869 (6)O19W—H19B0.9900
V12—O38B2.103 (5)O20W—H20A0.9900
V12—O30D2.408 (5)O20W—H20B0.9900
V13—O38B1.666 (5)O21W—H21A0.9900
V13—O39B1.683 (5)O21W—H21B0.9900
V13—O33C1.919 (5)O22W—H22A0.9900
V13—O34C1.929 (5)O22W—H22B0.9900
V13—O30D2.136 (5)O23W—H23A0.9900
V13—O29D2.215 (5)O23W—H23B0.9900
V14—O52T1.583 (6)O24W—H24A0.9900
V14—O40B1.819 (5)O24W—H24B0.9900
V14—O45B1.854 (5)O25W—H25A0.9900
V14—O48B1.904 (5)O25W—H25B0.9900
V14—O39B2.048 (5)O26W—H26A0.9900
V14—O29D2.383 (5)O26W—H26B0.9900
V15—O53T1.591 (5)O27W—H27A0.9800
V15—O45B1.824 (5)O27W—H27B0.9800
V15—O41B1.859 (5)O28W—H28A0.9800
V15—O33C1.989 (5)O28W—H28B0.9800
V15—O31C1.992 (5)O29W—H29A0.9800
V15—O29D2.302 (5)O29W—H29B0.9800
V15—V163.0899 (18)O30W—H30A0.9800
V16—O54T1.603 (5)O30W—H30B0.9800
V16—O42B1.808 (5)O31W—H31A0.9800
V16—O46B1.834 (5)O31W—H31B0.9800
V16—O31C2.032 (5)O32W—H32A0.9800
V16—O33C2.033 (5)O32W—H32B0.9800
V16—O30D2.260 (5)O33W—H33A0.9800
V17—O56T1.601 (5)O33W—H33B0.9800
V17—O47B1.821 (5)O34W—H34A0.9801
V17—O43B1.822 (6)O34W—H34B0.9801
V17—O32C2.027 (5)
O1D—Pt1—O2D85.0 (2)O40B—V10—O35B157.9 (2)
O1D—Pt1—O4C85.4 (2)O44B—V10—O35B83.5 (2)
O2D—Pt1—O4C86.0 (2)O49T—V10—O29D174.4 (3)
O1D—Pt1—O7B87.7 (2)O41B—V10—O29D77.4 (2)
O2D—Pt1—O7B172.5 (2)O40B—V10—O29D80.7 (2)
O4C—Pt1—O7B95.1 (2)O44B—V10—O29D73.9 (2)
O1D—Pt1—O3C85.4 (2)O35B—V10—O29D77.41 (19)
O2D—Pt1—O3C85.2 (2)O49T—V10—V14135.4 (2)
O4C—Pt1—O3C167.8 (2)O41B—V10—V1483.73 (17)
O7B—Pt1—O3C92.5 (2)O40B—V10—V1431.43 (16)
O1D—Pt1—O8B173.5 (2)O44B—V10—V1481.89 (17)
O2D—Pt1—O8B88.5 (2)O35B—V10—V14126.73 (15)
O4C—Pt1—O8B94.3 (2)O29D—V10—V1449.32 (13)
O7B—Pt1—O8B98.8 (2)O49T—V10—Pt2136.6 (2)
O3C—Pt1—O8B93.9 (2)O41B—V10—Pt277.74 (16)
O1D—Pt1—V889.71 (15)O40B—V10—Pt2119.20 (17)
O2D—Pt1—V846.83 (15)O44B—V10—Pt276.50 (16)
O4C—Pt1—V839.88 (15)O35B—V10—Pt238.88 (14)
O7B—Pt1—V8134.92 (15)O29D—V10—Pt238.55 (13)
O3C—Pt1—V8132.08 (15)V14—V10—Pt287.86 (4)
O8B—Pt1—V885.95 (16)O50T—V11—O37B102.3 (3)
O1D—Pt1—V646.84 (14)O50T—V11—O42B103.7 (3)
O2D—Pt1—V689.20 (15)O37B—V11—O42B91.4 (2)
O4C—Pt1—V6132.19 (14)O50T—V11—O43B104.1 (3)
O7B—Pt1—V684.60 (15)O37B—V11—O43B90.0 (2)
O3C—Pt1—V639.23 (14)O42B—V11—O43B151.2 (2)
O8B—Pt1—V6133.10 (15)O50T—V11—O36B99.6 (3)
V8—Pt1—V6123.87 (4)O37B—V11—O36B158.1 (2)
O1D—Pt1—V789.07 (14)O42B—V11—O36B83.3 (2)
O2D—Pt1—V746.00 (15)O43B—V11—O36B84.7 (2)
O4C—Pt1—V7131.97 (15)O50T—V11—O30D176.9 (3)
O7B—Pt1—V7132.36 (15)O37B—V11—O30D80.8 (2)
O3C—Pt1—V739.83 (15)O42B—V11—O30D75.7 (2)
O8B—Pt1—V786.34 (15)O43B—V11—O30D76.2 (2)
V8—Pt1—V792.55 (3)O36B—V11—O30D77.27 (19)
V6—Pt1—V759.87 (3)O50T—V11—Pt2138.2 (2)
O1D—Pt1—V945.75 (14)O37B—V11—Pt2119.53 (17)
O2D—Pt1—V988.58 (14)O42B—V11—Pt277.15 (16)
O4C—Pt1—V940.01 (14)O43B—V11—Pt277.21 (16)
O7B—Pt1—V987.51 (15)O36B—V11—Pt238.53 (15)
O3C—Pt1—V9131.16 (14)O30D—V11—Pt238.74 (12)
O8B—Pt1—V9134.34 (15)O51T—V12—O37B105.4 (3)
V8—Pt1—V960.05 (3)O51T—V12—O46B104.2 (3)
V6—Pt1—V992.40 (3)O37B—V12—O46B91.9 (2)
V7—Pt1—V9121.82 (3)O51T—V12—O47B104.1 (3)
O1D—Pt1—V147.87 (15)O37B—V12—O47B91.5 (2)
O2D—Pt1—V1132.90 (15)O46B—V12—O47B149.5 (2)
O4C—Pt1—V189.57 (14)O51T—V12—O38B100.7 (3)
O7B—Pt1—V139.84 (15)O37B—V12—O38B153.9 (2)
O3C—Pt1—V190.19 (14)O46B—V12—O38B82.4 (2)
O8B—Pt1—V1138.59 (15)O47B—V12—O38B81.4 (2)
V8—Pt1—V1120.36 (3)O51T—V12—O30D173.4 (3)
V6—Pt1—V160.49 (3)O37B—V12—O30D81.2 (2)
V7—Pt1—V1120.36 (3)O46B—V12—O30D75.2 (2)
V9—Pt1—V160.34 (3)O47B—V12—O30D75.5 (2)
O1D—Pt1—V442.71 (15)O38B—V12—O30D72.73 (19)
O2D—Pt1—V442.31 (14)O38B—V13—O39B108.8 (3)
O4C—Pt1—V484.03 (15)O38B—V13—O33C99.2 (2)
O7B—Pt1—V4130.38 (15)O39B—V13—O33C97.2 (2)
O3C—Pt1—V483.75 (15)O38B—V13—O34C98.1 (2)
O8B—Pt1—V4130.82 (15)O39B—V13—O34C97.4 (2)
V8—Pt1—V461.95 (3)O33C—V13—O34C152.3 (2)
V6—Pt1—V461.92 (3)O38B—V13—O30D89.0 (2)
V7—Pt1—V461.13 (3)O39B—V13—O30D162.2 (2)
V9—Pt1—V460.69 (3)O33C—V13—O30D79.4 (2)
V1—Pt1—V490.58 (3)O34C—V13—O30D79.5 (2)
O21T—V1—O12B102.9 (3)O38B—V13—O29D164.9 (2)
O21T—V1—O16B102.5 (3)O39B—V13—O29D86.3 (2)
O12B—V1—O16B91.3 (2)O33C—V13—O29D79.6 (2)
O21T—V1—O13B104.3 (3)O34C—V13—O29D78.1 (2)
O12B—V1—O13B91.2 (2)O30D—V13—O29D75.97 (19)
O16B—V1—O13B151.8 (2)O38B—V13—Pt2126.97 (19)
O21T—V1—O7B97.3 (2)O39B—V13—Pt2124.23 (18)
O12B—V1—O7B159.8 (2)O33C—V13—Pt276.42 (16)
O16B—V1—O7B85.8 (2)O34C—V13—Pt275.92 (16)
O13B—V1—O7B82.2 (2)O30D—V13—Pt238.00 (13)
O21T—V1—O1D174.6 (2)O29D—V13—Pt237.97 (13)
O12B—V1—O1D82.5 (2)O52T—V14—O40B103.9 (3)
O16B—V1—O1D76.5 (2)O52T—V14—O45B103.4 (3)
O13B—V1—O1D75.9 (2)O40B—V14—O45B91.3 (2)
O7B—V1—O1D77.38 (19)O52T—V14—O48B103.8 (3)
O21T—V1—V5135.1 (2)O40B—V14—O48B90.9 (2)
O12B—V1—V532.21 (17)O45B—V14—O48B151.2 (2)
O16B—V1—V584.60 (17)O52T—V14—O39B101.8 (3)
O13B—V1—V582.68 (17)O40B—V14—O39B154.3 (2)
O7B—V1—V5127.61 (16)O45B—V14—O39B83.7 (2)
O1D—V1—V550.29 (12)O48B—V14—O39B82.0 (2)
O21T—V1—Pt1136.0 (2)O52T—V14—O29D176.2 (3)
O12B—V1—Pt1121.12 (17)O40B—V14—O29D79.9 (2)
O16B—V1—Pt177.65 (16)O45B—V14—O29D76.9 (2)
O13B—V1—Pt177.00 (16)O48B—V14—O29D75.3 (2)
O7B—V1—Pt138.78 (15)O39B—V14—O29D74.43 (19)
O1D—V1—Pt138.63 (12)O52T—V14—V10135.7 (2)
V5—V1—Pt188.92 (4)O40B—V14—V1031.87 (17)
O22T—V2—O9B104.1 (3)O45B—V14—V1082.04 (17)
O22T—V2—O14B103.9 (3)O48B—V14—V1084.85 (17)
O9B—V2—O14B93.1 (2)O39B—V14—V10122.54 (16)
O22T—V2—O15B104.7 (3)O29D—V14—V1048.14 (12)
O9B—V2—O15B89.2 (2)O53T—V15—O45B102.3 (3)
O14B—V2—O15B149.8 (2)O53T—V15—O41B103.9 (3)
O22T—V2—O8B97.8 (3)O45B—V15—O41B92.5 (2)
O9B—V2—O8B158.1 (2)O53T—V15—O33C102.1 (3)
O14B—V2—O8B83.4 (2)O45B—V15—O33C90.3 (2)
O15B—V2—O8B83.3 (2)O41B—V15—O33C152.6 (2)
O22T—V2—O2D175.0 (3)O53T—V15—O31C100.0 (3)
O9B—V2—O2D80.9 (2)O45B—V15—O31C156.3 (2)
O14B—V2—O2D75.8 (2)O41B—V15—O31C89.7 (2)
O15B—V2—O2D74.9 (2)O33C—V15—O31C77.4 (2)
O8B—V2—O2D77.25 (19)O53T—V15—O29D177.4 (2)
O22T—V2—V3135.9 (2)O45B—V15—O29D79.6 (2)
O9B—V2—V331.83 (16)O41B—V15—O29D77.7 (2)
O14B—V2—V384.70 (17)O33C—V15—O29D76.0 (2)
O15B—V2—V381.58 (17)O31C—V15—O29D77.85 (19)
O8B—V2—V3126.31 (15)O53T—V15—V1691.9 (2)
O2D—V2—V349.08 (13)O45B—V15—V16130.58 (17)
O22T—V2—Pt1136.4 (2)O41B—V15—V16129.82 (17)
O9B—V2—Pt1119.47 (17)O33C—V15—V1640.32 (15)
O14B—V2—Pt176.32 (16)O31C—V15—V1640.33 (15)
O15B—V2—Pt176.36 (16)O29D—V15—V1685.47 (13)
O8B—V2—Pt138.68 (14)O53T—V15—Pt2139.1 (2)
O2D—V2—Pt138.58 (12)O45B—V15—Pt2118.55 (17)
V3—V2—Pt187.65 (4)O41B—V15—Pt278.08 (16)
O23T—V3—O9B103.8 (3)O33C—V15—Pt276.71 (15)
O23T—V3—O19B105.1 (3)O31C—V15—Pt239.20 (15)
O9B—V3—O19B92.0 (2)O29D—V15—Pt238.98 (13)
O23T—V3—O18B102.5 (3)V16—V15—Pt260.33 (3)
O9B—V3—O18B89.7 (2)O54T—V16—O42B104.9 (3)
O19B—V3—O18B151.1 (2)O54T—V16—O46B103.4 (3)
O23T—V3—O10B101.3 (3)O42B—V16—O46B94.8 (2)
O9B—V3—O10B154.8 (2)O54T—V16—O31C98.2 (2)
O19B—V3—O10B83.7 (2)O42B—V16—O31C91.3 (2)
O18B—V3—O10B82.6 (2)O46B—V16—O31C155.2 (2)
O23T—V3—O2D174.7 (3)O54T—V16—O33C99.6 (3)
O9B—V3—O2D81.0 (2)O42B—V16—O33C153.6 (2)
O19B—V3—O2D76.7 (2)O46B—V16—O33C88.8 (2)
O18B—V3—O2D75.1 (2)O31C—V16—O33C75.5 (2)
O10B—V3—O2D73.89 (19)O54T—V16—O30D173.3 (2)
O23T—V3—V4131.2 (2)O42B—V16—O30D80.8 (2)
O9B—V3—V4124.91 (17)O46B—V16—O30D79.4 (2)
O19B—V3—V477.94 (17)O31C—V16—O30D77.92 (19)
O18B—V3—V477.53 (16)O33C—V16—O30D74.2 (2)
O10B—V3—V429.94 (15)O54T—V16—V1589.4 (2)
O2D—V3—V443.96 (12)O42B—V16—V15130.56 (17)
O23T—V3—V2135.5 (2)O46B—V16—V15128.07 (18)
O9B—V3—V231.72 (17)O31C—V16—V1539.37 (14)
O19B—V3—V284.66 (17)O33C—V16—V1539.29 (14)
O18B—V3—V281.72 (17)O30D—V16—V1584.14 (13)
O10B—V3—V2123.10 (16)O54T—V16—Pt2137.5 (2)
O2D—V3—V249.23 (12)O42B—V16—Pt279.19 (17)
V4—V3—V293.19 (5)O46B—V16—Pt2118.62 (18)
O23T—V3—Na960.4 (2)O31C—V16—Pt239.41 (14)
O9B—V3—Na976.93 (19)O33C—V16—Pt276.17 (15)
O19B—V3—Na9157.87 (19)O30D—V16—Pt239.23 (12)
O18B—V3—Na949.40 (18)V15—V16—Pt260.30 (3)
O10B—V3—Na9114.31 (18)O56T—V17—O47B102.2 (3)
O2D—V3—Na9119.39 (16)O56T—V17—O43B104.6 (3)
V4—V3—Na9124.12 (10)O47B—V17—O43B95.4 (2)
V2—V3—Na994.90 (10)O56T—V17—O32C98.3 (3)
O10B—V4—O11B108.3 (3)O47B—V17—O32C156.0 (2)
O10B—V4—O6C98.3 (2)O43B—V17—O32C91.3 (2)
O11B—V4—O6C97.8 (2)O56T—V17—O34C99.4 (3)
O10B—V4—O5C98.0 (2)O47B—V17—O34C88.9 (2)
O11B—V4—O5C98.3 (2)O43B—V17—O34C154.1 (2)
O6C—V4—O5C152.2 (2)O32C—V17—O34C75.5 (2)
O10B—V4—O2D87.7 (2)O56T—V17—O30D173.4 (3)
O11B—V4—O2D163.9 (2)O47B—V17—O30D80.1 (2)
O6C—V4—O2D79.0 (2)O43B—V17—O30D81.3 (2)
O5C—V4—O2D79.2 (2)O32C—V17—O30D78.16 (19)
O10B—V4—O1D163.8 (2)O34C—V17—O30D74.30 (19)
O11B—V4—O1D87.8 (2)O56T—V17—V1889.8 (2)
O6C—V4—O1D78.9 (2)O47B—V17—V18126.52 (18)
O5C—V4—O1D79.2 (2)O43B—V17—V18131.95 (17)
O2D—V4—O1D76.10 (19)O32C—V17—V1840.86 (15)
O10B—V4—V337.78 (18)O34C—V17—V1837.60 (14)
O11B—V4—V3146.1 (2)O30D—V17—V1883.91 (13)
O6C—V4—V388.88 (15)O56T—V17—Pt2137.7 (2)
O5C—V4—V390.29 (15)O47B—V17—Pt2119.53 (17)
O2D—V4—V349.98 (14)O43B—V17—Pt279.64 (17)
O1D—V4—V3126.07 (14)O32C—V17—Pt239.42 (14)
O10B—V4—Pt1125.93 (18)O34C—V17—Pt276.02 (15)
O11B—V4—Pt1125.73 (19)O30D—V17—Pt239.42 (12)
O6C—V4—Pt175.88 (15)V18—V17—Pt260.72 (3)
O5C—V4—Pt176.31 (15)O55T—V18—O48B105.3 (3)
O2D—V4—Pt138.18 (14)O55T—V18—O44B101.9 (3)
O1D—V4—Pt137.92 (13)O48B—V18—O44B92.8 (2)
V3—V4—Pt188.15 (4)O55T—V18—O34C103.1 (3)
O24T—V5—O17B104.5 (3)O48B—V18—O34C92.5 (2)
O24T—V5—O12B105.9 (3)O44B—V18—O34C152.0 (2)
O17B—V5—O12B92.4 (2)O55T—V18—O32C96.5 (3)
O24T—V5—O20B103.6 (3)O48B—V18—O32C157.5 (2)
O17B—V5—O20B150.0 (2)O44B—V18—O32C88.1 (2)
O12B—V5—O20B89.8 (2)O34C—V18—O32C76.9 (2)
O24T—V5—O11B100.5 (3)O55T—V18—O29D173.5 (3)
O17B—V5—O11B83.9 (2)O48B—V18—O29D81.1 (2)
O12B—V5—O11B153.4 (2)O44B—V18—O29D76.8 (2)
O20B—V5—O11B81.0 (2)O34C—V18—O29D76.9 (2)
O24T—V5—O1D173.9 (3)O32C—V18—O29D77.16 (19)
O17B—V5—O1D76.0 (2)O55T—V18—V1790.8 (2)
O12B—V5—O1D80.0 (2)O48B—V18—V17132.26 (18)
O20B—V5—O1D74.98 (19)O44B—V18—V17128.03 (18)
O11B—V5—O1D73.46 (19)O34C—V18—V1739.74 (15)
O24T—V5—V1137.9 (2)O32C—V18—V1740.16 (14)
O17B—V5—V183.64 (17)O29D—V18—V1785.18 (13)
O12B—V5—V131.96 (16)O55T—V18—Pt2135.1 (2)
O20B—V5—V182.54 (17)O48B—V18—Pt2119.60 (18)
O11B—V5—V1121.53 (15)O44B—V18—Pt277.19 (17)
O1D—V5—V148.09 (12)O34C—V18—Pt276.33 (16)
O25T—V6—O13B104.8 (3)O32C—V18—Pt238.89 (14)
O25T—V6—O17B102.3 (3)O29D—V18—Pt238.49 (13)
O13B—V6—O17B94.0 (2)V17—V18—Pt259.72 (3)
O25T—V6—O3C98.7 (2)Pt2—O29D—V1398.2 (2)
O13B—V6—O3C91.9 (2)Pt2—O29D—V1896.0 (2)
O17B—V6—O3C155.9 (2)V13—O29D—V1890.60 (19)
O25T—V6—O5C100.9 (3)Pt2—O29D—V1593.6 (2)
O13B—V6—O5C153.2 (2)V13—O29D—V1590.63 (19)
O17B—V6—O5C88.0 (2)V18—O29D—V15170.1 (3)
O3C—V6—O5C76.5 (2)Pt2—O29D—V1093.6 (2)
O25T—V6—O1D175.2 (2)V13—O29D—V10167.9 (3)
O13B—V6—O1D79.2 (2)V18—O29D—V1091.21 (18)
O17B—V6—O1D79.8 (2)V15—O29D—V1085.57 (17)
O3C—V6—O1D78.45 (19)Pt2—O29D—V14175.8 (3)
O5C—V6—O1D74.86 (19)V13—O29D—V1485.67 (18)
O25T—V6—Pt1138.3 (2)V18—O29D—V1485.54 (18)
O13B—V6—Pt179.13 (17)V15—O29D—V1484.72 (17)
O17B—V6—Pt1119.03 (16)V10—O29D—V1482.54 (16)
O3C—V6—Pt139.77 (14)Pt2—O30D—V13100.4 (2)
O5C—V6—Pt176.55 (15)Pt2—O30D—V1694.5 (2)
O1D—V6—Pt139.24 (12)V13—O30D—V1693.9 (2)
O25T—V6—V791.0 (2)Pt2—O30D—V1794.0 (2)
O13B—V6—V7131.65 (17)V13—O30D—V1793.8 (2)
O17B—V6—V7127.32 (17)V16—O30D—V17167.3 (2)
O3C—V6—V740.04 (15)Pt2—O30D—V1191.9 (2)
O5C—V6—V739.33 (14)V13—O30D—V11167.7 (2)
O1D—V6—V784.38 (13)V16—O30D—V1185.03 (17)
Pt1—V6—V760.35 (3)V17—O30D—V1185.29 (17)
O26T—V7—O18B102.9 (3)Pt2—O30D—V12172.9 (3)
O26T—V7—O14B104.7 (3)V13—O30D—V1286.73 (18)
O18B—V7—O14B94.4 (2)V16—O30D—V1285.41 (17)
O26T—V7—O5C100.3 (2)V17—O30D—V1284.97 (16)
O18B—V7—O5C90.7 (2)V11—O30D—V1280.97 (15)
O14B—V7—O5C152.6 (2)V15—O31C—Pt2102.2 (2)
O26T—V7—O3C98.2 (3)V15—O31C—V16100.3 (2)
O18B—V7—O3C156.8 (2)Pt2—O31C—V16100.8 (2)
O14B—V7—O3C89.3 (2)Pt2—O32C—V17100.8 (2)
O5C—V7—O3C76.1 (2)Pt2—O32C—V18101.1 (2)
O26T—V7—O2D174.8 (2)V17—O32C—V1899.0 (2)
O18B—V7—O2D80.0 (2)V13—O33C—V15110.5 (3)
O14B—V7—O2D79.2 (2)V13—O33C—V16108.7 (2)
O5C—V7—O2D75.24 (19)V15—O33C—V16100.4 (2)
O3C—V7—O2D78.27 (19)V13—O34C—V18110.3 (2)
O26T—V7—V690.4 (2)V13—O34C—V17108.4 (2)
O18B—V7—V6130.40 (17)V18—O34C—V17102.7 (2)
O14B—V7—V6128.33 (18)Pt2—O35B—V10101.2 (2)
O5C—V7—V639.71 (15)Pt2—O35B—H35114 (6)
O3C—V7—V639.24 (14)V10—O35B—H35112 (6)
O2D—V7—V684.51 (13)Pt2—O36B—V11102.6 (2)
O26T—V7—Pt1137.7 (2)Pt2—O36B—H36115 (6)
O18B—V7—Pt1119.17 (18)V11—O36B—H36117 (6)
O14B—V7—Pt177.68 (16)V12—O37B—V11117.1 (3)
O5C—V7—Pt176.32 (14)V13—O38B—V12111.6 (3)
O3C—V7—Pt139.57 (14)V13—O39B—V14113.6 (3)
O2D—V7—Pt139.22 (13)V14—O40B—V10116.7 (3)
V6—V7—Pt159.79 (3)V10—O41B—V15118.0 (3)
O27T—V8—O15B104.2 (3)V16—O42B—V11117.2 (3)
O27T—V8—O19B102.8 (3)V17—O43B—V11116.0 (3)
O15B—V8—O19B94.1 (2)V18—O44B—V10116.6 (3)
O27T—V8—O4C98.2 (3)V18—O44B—H44129 (6)
O15B—V8—O4C92.4 (2)V10—O44B—H44114 (6)
O19B—V8—O4C155.8 (2)V15—O45B—V14118.3 (3)
O27T—V8—O6C101.4 (3)V16—O46B—V12118.4 (3)
O15B—V8—O6C153.1 (2)V17—O47B—V12117.7 (3)
O19B—V8—O6C88.1 (2)V18—O48B—V14117.5 (3)
O4C—V8—O6C75.9 (2)V11—O50T—O15B118.8 (3)
O27T—V8—O2D175.0 (2)O29W—Na1—O27W100.4 (3)
O15B—V8—O2D79.8 (2)O29W—Na1—O12W96.9 (2)
O19B—V8—O2D79.7 (2)O27W—Na1—O12W93.8 (3)
O4C—V8—O2D78.5 (2)O29W—Na1—O1W165.5 (3)
O6C—V8—O2D74.26 (19)O27W—Na1—O1W86.1 (3)
O27T—V8—Pt1137.5 (2)O12W—Na1—O1W95.6 (3)
O15B—V8—Pt179.50 (18)O29W—Na1—O28W83.7 (3)
O19B—V8—Pt1119.27 (18)O27W—Na1—O28W85.7 (3)
O4C—V8—Pt139.58 (14)O12W—Na1—O28W179.3 (3)
O6C—V8—Pt176.10 (15)O1W—Na1—O28W83.9 (3)
O2D—V8—Pt139.60 (13)O29W—Na1—O2W83.8 (2)
O28T—V9—O20B103.0 (3)O27W—Na1—O2W147.5 (3)
O28T—V9—O16B104.0 (3)O12W—Na1—O2W117.8 (3)
O20B—V9—O16B94.6 (2)O1W—Na1—O2W83.9 (3)
O28T—V9—O6C100.5 (3)O28W—Na1—O2W62.6 (3)
O20B—V9—O6C91.2 (2)O3W—Na2—O30W97.7 (3)
O16B—V9—O6C152.8 (2)O3W—Na2—O31W165.1 (3)
O28T—V9—O4C98.4 (2)O30W—Na2—O31W90.3 (2)
O20B—V9—O4C156.8 (2)O3W—Na2—O13W85.3 (3)
O16B—V9—O4C88.8 (2)O30W—Na2—O13W175.3 (3)
O6C—V9—O4C76.0 (2)O31W—Na2—O13W86.0 (2)
O28T—V9—O1D174.6 (2)O3W—Na2—O6W84.5 (3)
O20B—V9—O1D80.9 (2)O30W—Na2—O6W90.2 (2)
O16B—V9—O1D79.2 (2)O31W—Na2—O6W82.9 (2)
O6C—V9—O1D75.5 (2)O13W—Na2—O6W86.4 (2)
O4C—V9—O1D77.26 (19)O3W—Na2—O12W101.4 (3)
O28T—V9—Pt1137.3 (2)O30W—Na2—O12W90.3 (2)
O20B—V9—Pt1119.51 (17)O31W—Na2—O12W91.2 (2)
O16B—V9—Pt178.31 (16)O13W—Na2—O12W92.8 (2)
O6C—V9—Pt175.68 (15)O6W—Na2—O12W174.0 (2)
O4C—V9—Pt138.97 (14)O5W—Na3—O13W93.8 (3)
O1D—V9—Pt138.65 (12)O5W—Na3—O4W107.2 (3)
Pt1—O1D—V499.4 (2)O13W—Na3—O4W101.7 (2)
Pt1—O1D—V995.6 (2)O5W—Na3—O14W173.2 (3)
V4—O1D—V991.78 (19)O13W—Na3—O14W83.7 (2)
Pt1—O1D—V693.9 (2)O4W—Na3—O14W79.6 (2)
V4—O1D—V693.01 (19)O5W—Na3—O17W93.2 (3)
V9—O1D—V6168.5 (2)O13W—Na3—O17W167.2 (3)
Pt1—O1D—V193.5 (2)O4W—Na3—O17W86.4 (2)
V4—O1D—V1167.1 (2)O14W—Na3—O17W88.2 (2)
V9—O1D—V186.79 (17)O5W—Na3—O6W93.6 (2)
V6—O1D—V186.21 (17)O13W—Na3—O6W86.1 (2)
Pt1—O1D—V5175.0 (3)O4W—Na3—O6W157.1 (3)
V4—O1D—V585.52 (18)O14W—Na3—O6W80.0 (2)
V9—O1D—V585.31 (17)O17W—Na3—O6W82.8 (2)
V6—O1D—V584.66 (17)O8W—Na4—O22W95.2 (2)
V1—O1D—V581.62 (16)O8W—Na4—O20W96.8 (3)
Pt1—O2D—V499.5 (2)O22W—Na4—O20W87.9 (2)
Pt1—O2D—V794.8 (2)O8W—Na4—O33W106.4 (3)
V4—O2D—V792.8 (2)O22W—Na4—O33W98.9 (2)
Pt1—O2D—V893.6 (2)O20W—Na4—O33W155.0 (2)
V4—O2D—V893.51 (19)O8W—Na4—O18W91.8 (2)
V7—O2D—V8168.6 (2)O22W—Na4—O18W169.3 (2)
Pt1—O2D—V3174.3 (3)O20W—Na4—O18W83.3 (2)
V4—O2D—V386.07 (18)O33W—Na4—O18W86.8 (2)
V7—O2D—V385.94 (17)O8W—Na4—O19W176.3 (3)
V8—O2D—V385.00 (18)O22W—Na4—O19W83.1 (2)
Pt1—O2D—V292.8 (2)O20W—Na4—O19W79.8 (2)
V4—O2D—V2167.7 (3)O33W—Na4—O19W77.2 (2)
V7—O2D—V285.56 (17)O18W—Na4—O19W89.4 (2)
V8—O2D—V286.25 (18)O9W—Na5—O10W179.4 (3)
V3—O2D—V281.69 (16)O9W—Na5—O22W88.5 (2)
V6—O3C—Pt1101.0 (2)O10W—Na5—O22W92.2 (3)
V6—O3C—V7100.7 (2)O9W—Na5—O20W84.9 (2)
Pt1—O3C—V7100.6 (2)O10W—Na5—O20W95.0 (3)
Pt1—O4C—V8100.5 (2)O22W—Na5—O20W88.2 (2)
Pt1—O4C—V9101.0 (2)O9W—Na5—O23W88.6 (2)
V8—O4C—V999.9 (2)O10W—Na5—O23W91.5 (3)
V4—O5C—V7108.9 (2)O22W—Na5—O23W92.0 (2)
V4—O5C—V6109.7 (2)O20W—Na5—O23W173.5 (2)
V7—O5C—V6101.0 (2)O9W—Na5—O21W85.8 (3)
V4—O6C—V9109.3 (2)O10W—Na5—O21W93.6 (3)
V4—O6C—V8109.8 (2)O22W—Na5—O21W174.3 (2)
V9—O6C—V8102.2 (2)O20W—Na5—O21W91.7 (2)
Pt1—O7B—V1101.4 (2)O23W—Na5—O21W87.5 (2)
Pt1—O7B—H7115 (6)O23W—Na6—O11W166.4 (3)
V1—O7B—H7108 (6)O23W—Na6—O25W91.9 (2)
Pt1—O8B—V2101.5 (2)O11W—Na6—O25W87.3 (3)
Pt1—O8B—H8100 (6)O23W—Na6—O21W88.7 (2)
V2—O8B—H8128 (6)O11W—Na6—O21W94.2 (2)
V2—O9B—V3116.5 (3)O25W—Na6—O21W171.0 (3)
V4—O10B—V3112.3 (3)O23W—Na6—O24W86.0 (2)
V4—O11B—V5113.2 (3)O11W—Na6—O24W81.0 (3)
V1—O12B—V5115.8 (3)O25W—Na6—O24W104.2 (3)
V6—O13B—V1117.5 (3)O21W—Na6—O24W84.8 (3)
V2—O14B—V7117.6 (3)O23W—Na6—O34W99.5 (3)
V8—O15B—V2118.1 (3)O11W—Na6—O34W93.9 (3)
V8—O15B—O50T106.1 (2)O25W—Na6—O34W83.6 (3)
V2—O15B—O50T129.2 (3)O21W—Na6—O34W87.5 (3)
V9—O16B—V1115.7 (3)O24W—Na6—O34W170.4 (3)
V5—O17B—V6118.3 (3)O7W—Na7—O14W78.9 (2)
V7—O18B—V3118.2 (3)O7W—Na7—O15W170.2 (3)
V3—O19B—V8117.3 (3)O14W—Na7—O15W94.0 (2)
V9—O20B—V5117.9 (3)O7W—Na7—O16W106.5 (2)
O29D—Pt2—O30D85.5 (2)O14W—Na7—O16W94.8 (2)
O29D—Pt2—O32C85.2 (2)O15W—Na7—O16W80.7 (2)
O30D—Pt2—O32C85.7 (2)O7W—Na7—O17W92.0 (2)
O29D—Pt2—O35B87.8 (2)O14W—Na7—O17W87.8 (2)
O30D—Pt2—O35B173.2 (2)O15W—Na7—O17W80.9 (2)
O32C—Pt2—O35B94.9 (2)O16W—Na7—O17W161.5 (3)
O29D—Pt2—O31C85.7 (2)O7W—Na7—O22Tii86.9 (2)
O30D—Pt2—O31C85.2 (2)O14W—Na7—O22Tii165.3 (2)
O32C—Pt2—O31C167.6 (2)O15W—Na7—O22Tii100.5 (2)
O35B—Pt2—O31C93.2 (2)O16W—Na7—O22Tii85.5 (2)
O29D—Pt2—O36B173.7 (2)O17W—Na7—O22Tii96.5 (2)
O30D—Pt2—O36B88.2 (2)O19W—Na8—O49Ti166.9 (2)
O32C—Pt2—O36B95.0 (2)O19W—Na8—O16Wi94.8 (2)
O35B—Pt2—O36B98.5 (2)O49Ti—Na8—O16Wi96.9 (2)
O31C—Pt2—O36B93.1 (2)O19W—Na8—O32W84.5 (2)
O29D—Pt2—V1790.02 (14)O49Ti—Na8—O32W85.0 (2)
O30D—Pt2—V1746.60 (15)O16Wi—Na8—O32W169.4 (3)
O32C—Pt2—V1739.82 (14)O19W—Na8—O15Wi92.8 (2)
O35B—Pt2—V17134.64 (15)O49Ti—Na8—O15Wi83.3 (2)
O31C—Pt2—V17131.80 (14)O16Wi—Na8—O15Wi80.5 (2)
O36B—Pt2—V1786.12 (15)O32W—Na8—O15Wi110.1 (3)
O29D—Pt2—V1547.45 (15)O19W—Na8—O18W90.8 (2)
O30D—Pt2—V1588.06 (15)O49Ti—Na8—O18W96.8 (2)
O32C—Pt2—V15132.61 (15)O16Wi—Na8—O18W81.1 (2)
O35B—Pt2—V1586.57 (15)O32W—Na8—O18W88.3 (3)
O31C—Pt2—V1538.63 (14)O15Wi—Na8—O18W161.5 (3)
O36B—Pt2—V15131.77 (15)O24Wiii—Na9—O26W114.8 (4)
V17—Pt2—V15123.17 (3)O24Wiii—Na9—O26Wiv88.6 (3)
O29D—Pt2—V1690.58 (15)O26W—Na9—O26Wiv90.2 (3)
O30D—Pt2—V1646.23 (15)O24Wiii—Na9—O25Wv158.6 (3)
O32C—Pt2—V16131.88 (14)O26W—Na9—O25Wv86.1 (3)
O35B—Pt2—V16132.89 (15)O26Wiv—Na9—O25Wv86.9 (3)
O31C—Pt2—V1639.78 (14)O24Wiii—Na9—O18B77.0 (3)
O36B—Pt2—V1684.62 (15)O26W—Na9—O18B94.9 (3)
V17—Pt2—V1692.42 (3)O26Wiv—Na9—O18B165.5 (3)
V15—Pt2—V1659.37 (3)O25Wv—Na9—O18B107.0 (3)
O29D—Pt2—V1845.50 (15)O24Wiii—Na9—O23T93.2 (3)
O30D—Pt2—V1887.66 (15)O26W—Na9—O23T138.4 (3)
O32C—Pt2—V1839.97 (15)O26Wiv—Na9—O23T122.2 (3)
O35B—Pt2—V1888.41 (15)O25Wv—Na9—O23T71.8 (2)
O31C—Pt2—V18131.12 (14)O18B—Na9—O23T60.72 (19)
O36B—Pt2—V18134.92 (15)H1A—O1W—H1B100 (4)
V17—Pt2—V1859.56 (3)H2A—O2W—H2B101 (4)
V15—Pt2—V1892.92 (3)H3A—O3W—H3B107 (5)
V16—Pt2—V18121.99 (4)H4A—O4W—H4B114 (5)
O29D—Pt2—V1047.89 (14)H5A—O5W—H5B106 (5)
O30D—Pt2—V10133.33 (15)H6A—O6W—H6B110 (5)
O32C—Pt2—V1091.75 (15)H7A—O7W—H7B116 (5)
O35B—Pt2—V1039.90 (15)H8A—O8W—H8B110 (5)
O31C—Pt2—V1088.43 (14)H9A—O9W—H9B111 (5)
O36B—Pt2—V10138.32 (15)H10A—O10W—H10B103 (5)
V17—Pt2—V10122.46 (4)H11A—O11W—H11B104 (4)
V15—Pt2—V1060.42 (3)H12A—O12W—H12B107.5
V16—Pt2—V10119.75 (4)H13A—O13W—H13B110.2
V18—Pt2—V1062.92 (3)H14A—O14W—H14B110.6
O29D—Pt2—V11134.82 (15)H15A—O15W—H15B109.6
O30D—Pt2—V1149.32 (15)H16A—O16W—H16B109.6
O32C—Pt2—V1190.33 (15)H17A—O17W—H17B110.7
O35B—Pt2—V11137.40 (15)H18A—O18W—H18B111.0
O31C—Pt2—V1190.06 (14)H19A—O19W—H19B110.8
O36B—Pt2—V1138.92 (15)H20A—O20W—H20B110.7
V17—Pt2—V1160.53 (4)H21A—O21W—H21B110.7
V15—Pt2—V11119.55 (4)H22A—O22W—H22B110.6
V16—Pt2—V1160.19 (3)H23A—O23W—H23B110.6
V18—Pt2—V11120.09 (3)H24A—O24W—H24B107.6
V10—Pt2—V11176.76 (4)H25A—O25W—H25B106.3
O49T—V10—O41B105.2 (3)H26A—O26W—H26B110.9
O49T—V10—O40B104.0 (3)H28A—O28W—H28B109.5
O41B—V10—O40B93.0 (2)H29A—O29W—H29B109.5
O49T—V10—O44B102.9 (3)H30A—O30W—H30B109.5
O41B—V10—O44B150.8 (2)H31A—O31W—H31B109.5
O40B—V10—O44B87.8 (2)H32A—O32W—H32B109.5
O49T—V10—O35B97.7 (3)H33A—O33W—H33B109.5
O41B—V10—O35B85.0 (2)H34A—O34W—H34B109.5
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z; (iii) x+1, y+2, z+1; (iv) x, y+1, z+1; (v) x1, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7B—H7···O32C0.85 (3)1.79 (3)2.627 (7)171 (8)
O8B—H8···O43B0.86 (3)1.89 (3)2.737 (7)169 (8)
O35B—H35···O16B0.85 (3)1.86 (4)2.685 (7)164 (9)
O36B—H36···O4C0.84 (3)1.79 (3)2.628 (7)174 (8)
O44B—H44···O21T0.84 (3)2.00 (6)2.724 (8)144 (8)
O1W—H1B···O40Bv0.90 (3)2.18 (9)2.845 (9)130 (9)
O2W—H2B···O47Bvi0.88 (3)1.88 (3)2.757 (8)178 (12)
O3W—H3A···O39Bvi0.86 (3)2.01 (4)2.856 (9)168 (10)
O3W—H3B···O33Cvii0.87 (3)1.97 (6)2.795 (8)159 (12)
O4W—H4A···O51Tii0.84 (3)2.08 (3)2.893 (8)163 (8)
O4W—H4B···O41B0.84 (3)1.96 (4)2.780 (8)165 (10)
O5W—H5B···O46Bvii0.86 (3)1.94 (5)2.743 (8)154 (9)
O6W—H6A···O7W0.85 (3)2.03 (3)2.872 (9)170 (9)
O6W—H6B···O48Bvi0.84 (3)2.02 (5)2.810 (8)158 (9)
O7W—H7A···O28T0.83 (3)2.26 (5)2.951 (8)141 (8)
O7W—H7B···O34Wvi0.84 (3)2.05 (6)2.794 (10)148 (8)
O8W—H8A···O17Biii0.86 (3)1.93 (5)2.760 (8)161 (9)
O8W—H8B···O23Tviii0.85 (3)2.12 (7)2.872 (9)148 (10)
O9W—H9A···O7B0.85 (3)2.01 (5)2.826 (8)161 (9)
O9W—H9B···O37W0.84 (3)2.39 (6)3.073 (11)138 (8)
O10W—H10A···O5Ciii0.88 (3)1.92 (4)2.782 (9)165 (11)
O11W—H11A···O22Tix0.87 (3)2.23 (5)3.061 (8)158 (9)
O12W—H12A···O42B0.991.922.861 (8)159
O12W—H12B···O53Tvii0.992.002.956 (8)160
O13W—H13A···O31C0.991.842.831 (7)176
O13W—H13B···O54Tvii0.991.932.905 (8)169
O14W—H14A···O35B0.991.962.806 (8)142
O14W—H14B···O31W0.992.032.928 (8)151
O15W—H15A···O4W0.991.922.819 (9)149
O16W—H16A···O20B0.992.513.054 (7)115
O16W—H16B···O33Wii0.991.882.764 (9)147
O17W—H17A···O37Bii0.992.063.013 (8)162
O17W—H17A···O50Tii0.992.603.205 (8)119
O18W—H18A···O39Wviii0.991.972.942 (10)167
O18W—H18B···O12Bi0.992.012.977 (8)165
O19W—H19A···O9W0.992.052.949 (9)149
O19W—H19B···O8B0.991.992.867 (8)146
O20W—H20A···O32W0.991.942.857 (9)152
O20W—H20B···O19Bviii0.991.812.753 (8)157
O21W—H21A···O37W0.991.932.836 (10)151
O21W—H21B···O6Cviii0.991.902.869 (8)164
O22W—H22A···O25Tiii0.991.942.920 (8)170
O22W—H22B···O3C0.991.832.819 (7)173
O23W—H23A···O26Tiii0.992.042.993 (8)160
O23W—H23B···O13B0.991.872.840 (8)167
O24W—H24A···O11Bviii0.991.972.887 (9)152
O24W—H24B···O10W0.992.153.082 (13)157
O25W—H25A···O9Bix0.992.072.874 (9)137
O25W—H25B···O35W0.991.932.880 (10)160
O26W—H26A···O11Wv0.991.882.848 (11)165
O26W—H26B···O38W0.991.862.811 (12)161
O27W—H27A···O36W0.982.112.881 (10)135
O27W—H27B···O29Wx0.982.092.891 (10)138
O28W—H28A···O27Wx0.981.782.692 (11)153
O28W—H28B···O40Bv0.982.452.994 (9)115
O29W—H29A···O38Bvi0.982.122.992 (8)147
O29W—H29B···O45Bvii0.981.932.755 (8)141
O30W—H30A···O2W0.982.032.877 (10)143
O30W—H30B···O37Wvi0.981.932.893 (10)167
O31W—H31B···O36B0.982.082.812 (8)130
O32W—H32A···O40Wviii0.981.962.901 (13)160
O32W—H32B···O2Wviii0.982.012.896 (10)150
O33W—H33A···O38W0.982.132.833 (11)128
O33W—H33B···O14B0.981.812.786 (8)178
O34W—H34A···O55T0.982.293.038 (9)132
O34W—H34B···O39Wix0.982.022.979 (12)166
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z; (iii) x+1, y+2, z+1; (v) x1, y1, z; (vi) x, y1, z; (vii) x+1, y+1, z; (viii) x, y+1, z; (ix) x+1, y+1, z; (x) x, y, z.
Selected geometric parameters (Å, º) top
Pt1—O7B2.012 (5)Pt2—O35B2.015 (5)
Pt1—O8B2.025 (5)Pt2—O36B2.017 (5)
V1—O12B1.830 (5)V10—O41B1.820 (5)
V1—O16B1.882 (5)V10—O44B1.950 (6)
V1—O13B1.882 (5)V10—O35B2.059 (5)
V1—O7B2.058 (5)V11—O42B1.882 (5)
V2—O14B1.841 (6)V11—O43B1.905 (6)
V2—O15B1.904 (5)V11—O36B2.035 (5)
V2—O8B2.076 (5)V12—O46B1.853 (5)
V3—O19B1.840 (5)V12—O47B1.869 (6)
V3—O18B1.883 (6)V12—O38B2.103 (5)
V3—O10B2.054 (5)V13—O38B1.666 (5)
V4—O11B1.675 (5)V13—O39B1.683 (5)
V5—O17B1.838 (5)V14—O45B1.854 (5)
V5—O12B1.842 (6)V14—O48B1.904 (5)
V5—O20B1.896 (5)V14—O39B2.048 (5)
V5—O11B2.059 (5)V15—O45B1.824 (5)
V6—O13B1.805 (5)V15—O41B1.859 (5)
V6—O17B1.843 (5)V16—O42B1.808 (5)
V7—O18B1.802 (5)V16—O46B1.834 (5)
V7—O14B1.847 (5)V17—O47B1.821 (5)
V8—O15B1.808 (5)V17—O43B1.822 (6)
V8—O19B1.840 (5)V18—O48B1.779 (5)
V9—O20B1.805 (5)V18—O44B1.907 (5)
V9—O16B1.851 (5)
V6—O13B—V1117.5 (3)V10—O41B—V15118.0 (3)
V2—O14B—V7117.6 (3)V16—O42B—V11117.2 (3)
V8—O15B—V2118.1 (3)V17—O43B—V11116.0 (3)
V9—O16B—V1115.7 (3)V18—O44B—V10116.6 (3)
V5—O17B—V6118.3 (3)V15—O45B—V14118.3 (3)
V7—O18B—V3118.2 (3)V16—O46B—V12118.4 (3)
V3—O19B—V8117.3 (3)V17—O47B—V12117.7 (3)
V9—O20B—V5117.9 (3)V18—O48B—V14117.5 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7B—H7···O32C0.85 (3)1.79 (3)2.627 (7)171 (8)
O8B—H8···O43B0.86 (3)1.89 (3)2.737 (7)169 (8)
O35B—H35···O16B0.85 (3)1.86 (4)2.685 (7)164 (9)
O36B—H36···O4C0.84 (3)1.79 (3)2.628 (7)174 (8)
O44B—H44···O21T0.84 (3)2.00 (6)2.724 (8)144 (8)
O1W—H1B···O40Bi0.90 (3)2.18 (9)2.845 (9)130 (9)
O2W—H2B···O47Bii0.88 (3)1.88 (3)2.757 (8)178 (12)
O3W—H3A···O39Bii0.86 (3)2.01 (4)2.856 (9)168 (10)
O3W—H3B···O33Ciii0.87 (3)1.97 (6)2.795 (8)159 (12)
O4W—H4A···O51Tiv0.84 (3)2.08 (3)2.893 (8)163 (8)
O4W—H4B···O41B0.84 (3)1.96 (4)2.780 (8)165 (10)
O5W—H5B···O46Biii0.86 (3)1.94 (5)2.743 (8)154 (9)
O6W—H6A···O7W0.85 (3)2.03 (3)2.872 (9)170 (9)
O6W—H6B···O48Bii0.84 (3)2.02 (5)2.810 (8)158 (9)
O7W—H7A···O28T0.83 (3)2.26 (5)2.951 (8)141 (8)
O7W—H7B···O34Wii0.84 (3)2.05 (6)2.794 (10)148 (8)
O8W—H8A···O17Bv0.86 (3)1.93 (5)2.760 (8)161 (9)
O8W—H8B···O23Tvi0.85 (3)2.12 (7)2.872 (9)148 (10)
O9W—H9A···O7B0.85 (3)2.01 (5)2.826 (8)161 (9)
O9W—H9B···O37W0.84 (3)2.39 (6)3.073 (11)138 (8)
O10W—H10A···O5Cv0.88 (3)1.92 (4)2.782 (9)165 (11)
O11W—H11A···O22Tvii0.87 (3)2.23 (5)3.061 (8)158 (9)
O12W—H12A···O42B0.991.922.861 (8)158.9
O12W—H12B···O53Tiii0.992.002.956 (8)160.3
O13W—H13A···O31C0.991.842.831 (7)175.7
O13W—H13B···O54Tiii0.991.932.905 (8)168.7
O14W—H14A···O35B0.991.962.806 (8)142.4
O14W—H14B···O31W0.992.032.928 (8)150.5
O15W—H15A···O4W0.991.922.819 (9)149.1
O16W—H16A···O20B0.992.513.054 (7)114.6
O16W—H16B···O33Wiv0.991.882.764 (9)147.4
O17W—H17A···O37Biv0.992.063.013 (8)161.5
O17W—H17A···O50Tiv0.992.603.205 (8)119.4
O18W—H18A···O39Wvi0.991.972.942 (10)166.5
O18W—H18B···O12Bviii0.992.012.977 (8)165.1
O19W—H19A···O9W0.992.052.949 (9)149.4
O19W—H19B···O8B0.991.992.867 (8)145.9
O20W—H20A···O32W0.991.942.857 (9)152.1
O20W—H20B···O19Bvi0.991.812.753 (8)157.4
O21W—H21A···O37W0.991.932.836 (10)150.8
O21W—H21B···O6Cvi0.991.902.869 (8)164.3
O22W—H22A···O25Tv0.991.942.920 (8)170.2
O22W—H22B···O3C0.991.832.819 (7)173.2
O23W—H23A···O26Tv0.992.042.993 (8)160.1
O23W—H23B···O13B0.991.872.840 (8)167.3
O24W—H24A···O11Bvi0.991.972.887 (9)152.3
O24W—H24B···O10W0.992.153.082 (13)156.6
O25W—H25A···O9Bvii0.992.072.874 (9)137.2
O25W—H25B···O35W0.991.932.880 (10)160.1
O26W—H26A···O11Wi0.991.882.848 (11)165.3
O26W—H26B···O38W0.991.862.811 (12)161.2
O27W—H27A···O36W0.982.112.881 (10)134.7
O27W—H27B···O29Wix0.982.092.891 (10)138.0
O28W—H28A···O27Wix0.981.782.692 (11)153.4
O28W—H28B···O40Bi0.982.452.994 (9)115.0
O29W—H29A···O38Bii0.982.122.992 (8)147.2
O29W—H29B···O45Biii0.981.932.755 (8)140.8
O30W—H30A···O2W0.982.032.877 (10)143.1
O30W—H30B···O37Wii0.981.932.893 (10)166.5
O31W—H31B···O36B0.982.082.812 (8)129.9
O32W—H32A···O40Wvi0.981.962.901 (13)159.8
O32W—H32B···O2Wvi0.982.012.896 (10)150.0
O33W—H33A···O38W0.982.132.833 (11)127.5
O33W—H33B···O14B0.981.812.786 (8)178.2
O34W—H34A···O55T0.982.293.038 (9)132.3
O34W—H34B···O39Wvii0.982.022.979 (12)166.1
Symmetry codes: (i) x1, y1, z; (ii) x, y1, z; (iii) x+1, y+1, z; (iv) x+1, y, z; (v) x+1, y+2, z+1; (vi) x, y+1, z; (vii) x+1, y+1, z; (viii) x1, y, z; (ix) x, y, z.

Experimental details

Crystal data
Chemical formulaNa9[H2PtV9O28][H3PtV9O28]·40H2O
Mr1567.84
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)12.706 (1), 12.875 (1), 28.319 (2)
α, β, γ (°)93.760 (1), 98.449 (1), 113.318 (1)
V3)4168.9 (5)
Z4
Radiation typeMo Kα
µ (mm1)5.44
Crystal size (mm)0.40 × 0.20 × 0.20
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1997)
Tmin, Tmax0.515, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
37312, 19046, 13416
Rint0.039
(sin θ/λ)max1)0.666
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.053, 0.115, 1.05
No. of reflections19046
No. of parameters1203
No. of restraints38
H-atom treatmentOnly H-atom coordinates refined
w = 1/[σ2(Fo2) + (0.0047P)2 + 66.1402P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.99, 2.15

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXL2014 (Sheldrick, 2015), ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 1998).

 

References

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ISSN: 2056-9890
Volume 71| Part 7| July 2015| Pages 786-790
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