Tetradeca­aqua­tetrasodium hexa­aqua­nickel(II) decavanadate(V) trihydrate

Sun, Z.-G.; Long, L.-S.; Ren, Y.-P.; Huang, R.-B.; Zheng, L.-S.; Ng, S.W.

doi:10.1107/S1600536802005421

Tetradecaaquatetrasodium hexaaquanickel(II) decavanadate(V) trihydrate

Z.-G. Sun, L.-S. Long, Y.-P. Ren, R.-B. Huang, L.-S. Zheng and S. W. Ng

Three crystallographically independent Na atoms and four pairs of water molecules occupying general positions form the link between the other two independent Na atoms occupying special positions on the inversion centres in the crystal of tetradecaaquatetrasodium hexaaquanickel(II) decavanadate(V) trihydrate, Na₄Ni(V₁₀O₂₈)·23H₂O. In this way, the infinite chains made up of the Na atoms and water molecules, and stretching along the (0 $\overline 1$ 1) direction, are formed. Each of the two independent Na atoms, which occupy centrosymmetric sites, are coordinated by one of the vanadyl atoms of one of the two independent centrosymmetric [V₁₀O₂₈]^6- hexaanions, thus effectively linking the chains into infinite layered structure. The layers are further integrated into a three-dimensional network through numerous hydrogen bonds involving water molecules, including those which are part of the sodium chains, as well as those which belong to [Ni(H₂O)₆]²⁺ coordination octahedra and those which are not coordinated by any metal (lattice hydrate molecules).

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802005421/ya6097sup1.cif Contains datablocks I, voni
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802005421/ya6097Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (Ni-O) = 0.004 Å
Disorder in solvent or counterion
R factor = 0.040
wR factor = 0.100
Data-to-parameter ratio = 11.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

PLATON alerts of the form PLAT_7?? have been detected for an inorganic
structure. These tests are under development  for inorganics and
comments are welcomed. It is not necessary to supply a data
validation response form for these alerts at this time.


 Alert Level B:



PLAT_420  Alert B D-H Without Acceptor       O(11W) -   H(111)            ?

PLAT_735  Alert B D-H     Calc     0.85(5), Rep   0.847(10) ....       5.00 s.u-Ratio
                     O1W  -H11     1.555   1.555

PLAT_735  Alert B D-H     Calc     0.84(5), Rep   0.849(10) ....       5.00 s.u-Ratio
                     O11W -H111    1.555   1.555


 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.245     0.290
          Tmin and Tmax expected:      0.466     0.750
          RR =      1.359
          Please check that your absorption correction is appropriate.

PLAT_302  Alert C Anion/Solvent Disorder .......................       3.00 Perc.

PLAT_735  Alert C D-H     Calc     0.86(4), Rep   0.852(10) ....       4.00 s.u-Ratio
                     O2W  -H21     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(4), Rep   0.853(10) ....       4.00 s.u-Ratio
                     O2W  -H22     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O3W  -H31     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O3W  -H32     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.848(10) ....       4.00 s.u-Ratio
                     O4W  -H41     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.845(10) ....       4.00 s.u-Ratio
                     O4W  -H42     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.847(10) ....       4.00 s.u-Ratio
                     O5W  -H51     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(4), Rep   0.847(10) ....       4.00 s.u-Ratio
                     O5W  -H52     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.847(10) ....       4.00 s.u-Ratio
                     O6W  -H61     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.846(10) ....       3.00 s.u-Ratio
                     O6W  -H62     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.847(10) ....       4.00 s.u-Ratio
                     O7W  -H71     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(4), Rep   0.846(10) ....       4.00 s.u-Ratio
                     O7W  -H72     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.848(10) ....       4.00 s.u-Ratio
                     O8W  -H81     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.852(10) ....       4.00 s.u-Ratio
                     O8W  -H82     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O9W  -H91     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.850(10) ....       4.00 s.u-Ratio
                     O9W  -H92     1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O10W -H101    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.847(10) ....       4.00 s.u-Ratio
                     O10W -H102    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.846(10) ....       4.00 s.u-Ratio
                     O11W -H112    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(3), Rep   0.844(10) ....       3.00 s.u-Ratio
                     O12W -H121    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(3), Rep   0.843(10) ....       3.00 s.u-Ratio
                     O12W -H122    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.848(10) ....       3.00 s.u-Ratio
                     O13W -H131    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O13W -H132    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.847(10) ....       3.00 s.u-Ratio
                     O14W -H141    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.849(10) ....       4.00 s.u-Ratio
                     O14W -H142    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.846(10) ....       4.00 s.u-Ratio
                     O15W -H152    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.846(10) ....       4.00 s.u-Ratio
                     O16W -H161    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(3), Rep   0.845(10) ....       3.00 s.u-Ratio
                     O16W -H162    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.848(10) ....       4.00 s.u-Ratio
                     O17W -H172    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(3), Rep   0.843(10) ....       3.00 s.u-Ratio
                     O18W -H181    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.84(4), Rep   0.848(10) ....       4.00 s.u-Ratio
                     O18W -H182    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.845(10) ....       3.00 s.u-Ratio
                     O19W -H191    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.846(10) ....       3.00 s.u-Ratio
                     O19W -H192    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.843(10) ....       4.00 s.u-Ratio
                     O20W -H201    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.847(10) ....       3.00 s.u-Ratio
                     O20W -H202    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(4), Rep   0.846(10) ....       4.00 s.u-Ratio
                     O21W -H211    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.847(10) ....       3.00 s.u-Ratio
                     O21W -H212    1.555   1.555

PLAT_735  Alert C D-H     Calc     0.85(3), Rep   0.845(10) ....       3.00 s.u-Ratio
                     O22W -H221    1.555   1.555

PLAT_736  Alert C H...A   Calc     2.11(4), Rep   2.112(19) ....       2.11 s.u-Ratio
                     H21  -O7W     1.555   1.555

PLAT_736  Alert C H...A   Calc     1.95(5), Rep   1.953(15) ....       3.33 s.u-Ratio
                     H42  -O16W    1.555   1.555

PLAT_736  Alert C H...A   Calc     2.05(4), Rep   2.052(17) ....       2.35 s.u-Ratio
                     H52  -O21W    1.555   1.555

PLAT_736  Alert C H...A   Calc     2.20(4), Rep   2.201(15) ....       2.67 s.u-Ratio
                     H61  -O11     1.555   1.445

PLAT_736  Alert C H...A   Calc     2.06(4), Rep   2.063(12) ....       3.33 s.u-Ratio
                     H62  -O4      1.555   2.765

PLAT_736  Alert C H...A   Calc     1.91(4), Rep   1.910(13) ....       3.08 s.u-Ratio
                     H71  -O3      1.555   2.665

PLAT_736  Alert C H...A   Calc     2.09(4), Rep   2.088(18) ....       2.22 s.u-Ratio
                     H72  -O20     1.555   1.455

PLAT_736  Alert C H...A   Calc     1.87(4), Rep   1.873(14) ....       2.86 s.u-Ratio
                     H81  -O18     1.555   1.555

PLAT_736  Alert C H...A   Calc     2.12(4), Rep   2.119(18) ....       2.22 s.u-Ratio
                     H82  -O2      1.555   2.765

PLAT_736  Alert C H...A   Calc     1.96(4), Rep   1.953(14) ....       2.86 s.u-Ratio
                     H91  -O9      1.555   1.445

PLAT_736  Alert C H...A   Calc     2.00(4), Rep   1.996(14) ....       2.86 s.u-Ratio
                     H101 -O19     1.555   1.455

PLAT_736  Alert C H...A   Calc     2.39(4), Rep   2.397(15) ....       2.67 s.u-Ratio
                     H102 -O17     1.555   1.555

PLAT_736  Alert C H...A   Calc     2.32(3), Rep   2.315(12) ....       2.50 s.u-Ratio
                     H121 -O25     1.555   1.445

PLAT_736  Alert C H...A   Calc     1.98(4), Rep   1.973(17) ....       2.35 s.u-Ratio
                     H122 -O5      1.555   1.445

PLAT_736  Alert C H...A   Calc     2.05(3), Rep   2.047(13) ....       2.31 s.u-Ratio
                     H142 -O8W     1.555   1.555

PLAT_736  Alert C H...A   Calc     1.86(4), Rep   1.862(14) ....       2.86 s.u-Ratio
                     H152 -O21W    1.555   1.555

PLAT_736  Alert C H...A   Calc     1.88(4), Rep   1.876(12) ....       3.33 s.u-Ratio
                     H172 -O22W    1.555   1.555

PLAT_736  Alert C H...A   Calc     1.95(4), Rep   1.946(15) ....       2.67 s.u-Ratio
                     H182 -O12W    1.555   1.565

PLAT_736  Alert C H...A   Calc     1.97(3), Rep   1.974(11) ....       2.73 s.u-Ratio
                     H191 -O26     1.555   1.555

PLAT_736  Alert C H...A   Calc     1.81(3), Rep   1.814(12) ....       2.50 s.u-Ratio
                     H192 -O24     1.555   1.455

PLAT_736  Alert C H...A   Calc     1.92(3), Rep   1.923(12) ....       2.50 s.u-Ratio
                     H201 -O12     1.555   1.455

PLAT_736  Alert C H...A   Calc     1.85(3), Rep   1.849(11) ....       2.73 s.u-Ratio
                     H202 -O7      1.555   1.555

PLAT_743  Alert C Torsion Calc    0.03(13), Rep        0.00 ....    Missing s.u.
                     O1  -V5  -O1  -V5     2.775   1.555   1.555   2.775

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      2.586
          Tmax scaled      0.750 Tmin scaled      0.634


 0 Alert Level A = Potentially serious problem

 3 Alert Level B = Potential problem

 63 Alert Level C = Please check

Comment top

The title compound, which has the empirical formulation of Na₄Ni(V₁₀O₂₈).23H₂O, is related to the water-soluble mineral huemulite, Na₄Mg(V₁₀O₂₈).24H₂O (Gordillo et al., 1966). Both compounds feature the polyhedral [V₁₀O₂₈]^6- hexaanion, whose structure has been well documented: it contains eight terminal, 14 µ₂-bridging, four µ₃-bridging and two µ₆-bridging O atoms linking ten V atoms into a D_{2 h} point-symmetry hexa-anionic species (Capparelli et al., 1986).

In the title compound, the Ni atom is coordinated by six water molecules in the [Ni(H₂O)₆]²⁺ dication (Fig. 1). Three Na atoms (which are in general positions) and four pairs of bridging water molecules comprise a link between the two other independent Na atoms (which are located at the crystallographic inversion centers), and this unit then continues on to form infinite chains in the (011) direction (Fig. 2). Each of the Na atoms in general positions along with the four contacts with bridging water molecules has two terminal water ligands; however, the Na atoms in the inversion centers along with four bridging coordinations are additionally coordinated to the vanadyl atoms (O14 and O16) of each of the two independent [V₁₀O₂₈]^6- anions (Figs. 3 and 4), these interaction linking the chains into layers. The numerous hydrogen bonds connect these negatively charged layers, as well as the otherwise isolated [Ni(H₂O)₆]²⁺ dications and lattice water molecules, into three-dimensional network.

Decavanadates having an aklylammonium cation as the counter-ion are also known; these are synthesized by the reaction of the amine and vanadium pentoxide (Averbuch-Pouchot, 1995; Averbuch-Pouchot & Durif, 1995).

Experimental top

The title compound was the unexpected product of the reaction of equimolar amounts of ammonium metavanadate (0.12 g, 1 mmol), nickel nitrate hexahydrate (0.29 g, 1 mmol) and 1,2,4-benzenetricarboxylic acid anhydride (0.19 g, 1 mmol) in several ml of 50% aqueous ethanol. The pH of the solution was adjusted to approximately 8 by the addition of sodium hydroxide solution. Pink polyhedral crystals separated from the solution after one week.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1988); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top

	Fig. 1. ORTEPII (Johnson, 1976) plot of the hexaaquanickel cation at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.
	Fig. 2. ORTEPII (Johnson, 1976) plot showing the fragment of the infinite chain of coordinated Na atoms in the crystal of the title compound. Displacement ellipsoids are drawn illustrating the octahedral geometry at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.
	Fig. 3. ORTEPII (Johnson, 1976) plot of one of the centrosymmetric decavanadate anions at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.
	Fig. 4. ORTEPII (Johnson, 1976) plot of one of the centrosymmetric decavanadate anions at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.

Tetradecaaquatetrasodium hexaaquanickel(II) decavanadate(V) trihydrate top

Crystal data top

Na₄Ni(V₁₀O₂₈)·23H₂O	Z = 2
M_r = 1522.44	F(000) = 1512
Triclinic, P1	D_x = 2.303 Mg m⁻³
a = 8.925 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.862 (3) Å	Cell parameters from 25 reflections
c = 18.341 (4) Å	θ = 12.8–13.9°
α = 91.81 (3)°	µ = 2.62 mm⁻¹
β = 91.85 (3)°	T = 298 K
γ = 104.32 (3)°	Block, pink
V = 2195.5 (8) Å³	0.50 × 0.25 × 0.11 mm

Data collection top

Enraf-Nonius CAD-4 diffractometer	6270 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.027
Graphite monochromator	θ_max = 26.0°, θ_min = 1.1°
ω scans	h = 0→11
Absorption correction: ψ scan (North et al., 1968)	k = −17→16
T_min = 0.245, T_max = 0.290	l = −22→22
9182 measured reflections	3 standard reflections every 60 min
8594 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.100	Only H-atom coordinates refined
S = 1.02	w = 1/[σ²(F_o²) + (0.0427P)² + 1.0711P] where P = (F_o² + 2F_c²)/3
8594 reflections	(Δ/σ)_max < 0.001
748 parameters	Δρ_max = 0.53 e Å⁻³
71 restraints	Δρ_min = −0.56 e Å⁻³

Crystal data top

Na₄Ni(V₁₀O₂₈)·23H₂O	γ = 104.32 (3)°
M_r = 1522.44	V = 2195.5 (8) Å³
Triclinic, P1	Z = 2
a = 8.925 (2) Å	Mo Kα radiation
b = 13.862 (3) Å	µ = 2.62 mm⁻¹
c = 18.341 (4) Å	T = 298 K
α = 91.81 (3)°	0.50 × 0.25 × 0.11 mm
β = 91.85 (3)°

Data collection top

Enraf-Nonius CAD-4 diffractometer	6270 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.027
T_min = 0.245, T_max = 0.290	3 standard reflections every 60 min
9182 measured reflections	intensity decay: none
8594 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	71 restraints
wR(F²) = 0.100	Only H-atom coordinates refined
S = 1.02	Δρ_max = 0.53 e Å⁻³
8594 reflections	Δρ_min = −0.56 e Å⁻³
748 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.51980 (6)	0.75713 (4)	0.24874 (3)	0.02339 (14)
V1	1.04483 (8)	0.88632 (5)	−0.11579 (4)	0.01989 (17)
V2	0.98071 (8)	0.89853 (5)	0.12389 (4)	0.01966 (16)
V3	1.19773 (9)	0.82060 (6)	0.02127 (4)	0.02303 (18)
V4	0.84823 (9)	0.74714 (5)	−0.00557 (4)	0.02337 (18)
V5	1.18889 (8)	1.04061 (5)	0.01413 (4)	0.01687 (16)
V6	0.79087 (8)	0.25867 (5)	0.49586 (4)	0.02219 (17)
V7	1.02179 (8)	0.37485 (5)	0.38700 (4)	0.01882 (16)
V8	0.81267 (8)	0.48000 (5)	0.48244 (4)	0.01634 (16)
V9	0.86214 (9)	0.70758 (6)	0.47248 (4)	0.02267 (17)
V10	1.05245 (8)	0.59845 (5)	0.37444 (4)	0.01836 (16)
Na1	0.5000	0.5000	0.0000	0.0481 (8)
Na2	0.7076 (2)	0.44162 (16)	0.15135 (11)	0.0418 (5)
Na3	0.4850 (2)	0.24783 (15)	0.25365 (11)	0.0342 (4)
Na4	0.2635 (2)	0.04865 (16)	0.35560 (12)	0.0411 (5)
Na5	0.5000	0.0000	0.5000	0.0363 (7)
O1	1.0104 (3)	0.9053 (2)	0.00392 (15)	0.0163 (6)
O2	1.0745 (4)	0.8835 (2)	−0.20194 (16)	0.0285 (7)
O3	0.8974 (3)	0.7729 (2)	−0.10323 (16)	0.0232 (7)
O4	1.2035 (3)	0.8379 (2)	−0.07840 (16)	0.0241 (7)
O5	0.9530 (4)	0.9039 (2)	0.21043 (16)	0.0273 (7)
O6	1.1456 (3)	0.8473 (2)	0.11791 (16)	0.0234 (7)
O7	0.8395 (3)	0.7826 (2)	0.09280 (16)	0.0238 (7)
O8	0.8303 (3)	0.9750 (2)	0.08851 (15)	0.0185 (6)
O9	1.1116 (3)	1.0350 (2)	0.11259 (15)	0.0170 (6)
O10	1.3121 (3)	0.9681 (2)	0.02871 (16)	0.0226 (7)
O11	1.2938 (3)	1.1598 (2)	0.02227 (16)	0.0224 (7)
O12	1.3420 (4)	0.7730 (2)	0.03757 (18)	0.0329 (8)
O13	1.0314 (4)	0.7133 (2)	0.01179 (17)	0.0261 (7)
O14	0.7209 (4)	0.6436 (2)	−0.01234 (19)	0.0373 (8)
O15	0.9834 (3)	0.4014 (2)	0.50532 (15)	0.0173 (6)
O16	0.6402 (4)	0.1671 (2)	0.48808 (19)	0.0325 (8)
O17	0.6819 (3)	0.3695 (2)	0.47561 (16)	0.0203 (6)
O18	0.8495 (3)	0.2756 (2)	0.39899 (16)	0.0219 (6)
O19	1.1530 (3)	0.3067 (2)	0.42804 (16)	0.0226 (7)
O20	1.0511 (4)	0.3652 (2)	0.30110 (17)	0.0286 (7)
O21	0.8930 (3)	0.4734 (2)	0.38613 (15)	0.0171 (6)
O22	0.9109 (3)	0.6713 (2)	0.37750 (16)	0.0220 (6)
O23	1.0810 (3)	0.5882 (2)	0.28846 (16)	0.0261 (7)
O24	1.2155 (3)	0.7013 (2)	0.40643 (16)	0.0223 (7)
O25	1.0497 (3)	0.7990 (2)	0.48396 (16)	0.0242 (7)
O26	0.7419 (4)	0.7732 (2)	0.45361 (18)	0.0323 (8)
O27	0.7163 (3)	0.5680 (2)	0.46581 (16)	0.0213 (6)
O28	0.8270 (3)	0.4966 (2)	0.58633 (15)	0.0174 (6)
O1w	0.7000 (6)	0.4267 (3)	0.0219 (2)	0.0608 (12)
H11	0.783 (5)	0.459 (3)	0.004 (4)	0.073*
H12	0.682 (6)	0.3656 (13)	0.009 (3)	0.073*
O2w	0.4840 (5)	0.5001 (3)	0.1301 (2)	0.0467 (10)
H21	0.422 (6)	0.449 (2)	0.147 (3)	0.056*
H22	0.481 (6)	0.551 (2)	0.156 (3)	0.056*
O3w	0.9320 (6)	0.3839 (3)	0.1567 (2)	0.0566 (12)
H31	0.945 (7)	0.333 (3)	0.133 (2)	0.068*
H32	0.979 (7)	0.388 (4)	0.1981 (16)	0.068*
O4w	0.8688 (5)	0.6117 (3)	0.1725 (2)	0.0432 (9)
H41	0.900 (6)	0.654 (3)	0.140 (2)	0.052*
H42	0.826 (6)	0.637 (3)	0.206 (2)	0.052*
O5w	0.6518 (4)	0.4140 (3)	0.27762 (19)	0.0358 (8)
H51	0.724 (4)	0.415 (4)	0.3090 (19)	0.043*
H52	0.586 (4)	0.441 (4)	0.296 (2)	0.043*
O6w	0.5611 (4)	0.2584 (3)	0.1279 (2)	0.0374 (8)
H61	0.479 (3)	0.234 (4)	0.102 (2)	0.045*
H62	0.633 (3)	0.232 (3)	0.115 (3)	0.045*
O7w	0.2999 (4)	0.3351 (3)	0.2117 (2)	0.0414 (9)
H71	0.245 (4)	0.303 (4)	0.1761 (18)	0.050*
H72	0.243 (4)	0.352 (4)	0.243 (2)	0.050*
O8w	0.6774 (4)	0.1614 (3)	0.2886 (2)	0.0367 (8)
H81	0.734 (4)	0.191 (4)	0.3246 (17)	0.044*
H82	0.734 (4)	0.145 (4)	0.2561 (18)	0.044*
O9w	0.3255 (4)	0.0814 (3)	0.23084 (19)	0.0366 (8)
H91	0.254 (4)	0.071 (4)	0.1980 (19)	0.044*
H92	0.400 (4)	0.059 (4)	0.216 (2)	0.044*
O10w	0.3988 (4)	0.2292 (3)	0.3776 (2)	0.0397 (9)
H101	0.321 (3)	0.251 (4)	0.388 (3)	0.048*
H102	0.476 (3)	0.259 (3)	0.405 (2)	0.048*
O11w	0.0305 (6)	0.0964 (4)	0.3530 (3)	0.0678 (14)
H111	−0.019 (6)	0.117 (5)	0.386 (2)	0.081*
H112	−0.019 (6)	0.092 (5)	0.3124 (15)	0.081*
O12w	0.1409 (4)	−0.1247 (3)	0.3277 (2)	0.0366 (8)
H121	0.104 (5)	−0.149 (4)	0.3668 (14)	0.044*
H122	0.070 (4)	−0.129 (4)	0.2954 (17)	0.044*
O13w	0.2364 (5)	0.0206 (3)	0.4854 (2)	0.0487 (10)
H131	0.172 (5)	−0.0341 (18)	0.493 (3)	0.058*
H132	0.214 (6)	0.068 (2)	0.510 (3)	0.058*
O14w	0.5033 (4)	0.0001 (3)	0.3708 (2)	0.0395 (9)
H141	0.497 (6)	−0.0583 (13)	0.354 (3)	0.047*
H142	0.562 (5)	0.042 (2)	0.345 (2)	0.047*
O15w	0.3900 (4)	0.6133 (3)	0.25155 (18)	0.0298 (7)
H151	0.2921 (13)	0.602 (4)	0.252 (2)	0.036*
H152	0.423 (4)	0.586 (3)	0.2873 (18)	0.036*
O16w	0.7136 (4)	0.7075 (3)	0.2697 (2)	0.0372 (9)
H161	0.763 (6)	0.704 (3)	0.3094 (15)	0.045*
H162	0.700 (6)	0.654 (2)	0.245 (2)	0.045*
O17w	0.6469 (4)	0.9018 (3)	0.24623 (19)	0.0325 (8)
H171	0.7435 (16)	0.910 (4)	0.242 (3)	0.039*
H172	0.611 (4)	0.935 (3)	0.215 (2)	0.039*
O18w	0.3229 (4)	0.8034 (3)	0.22962 (19)	0.0372 (9)
H181	0.275 (5)	0.801 (4)	0.1890 (12)	0.045*
H182	0.279 (5)	0.829 (4)	0.2625 (16)	0.045*
O19w	0.4932 (4)	0.7834 (3)	0.35793 (16)	0.0265 (7)
H191	0.568 (3)	0.782 (3)	0.3872 (19)	0.032*
H192	0.408 (2)	0.752 (3)	0.375 (2)	0.032*
O20w	0.5485 (4)	0.7312 (3)	0.13999 (17)	0.0295 (8)
H201	0.486 (3)	0.748 (4)	0.110 (2)	0.035*
H202	0.6403 (19)	0.749 (4)	0.126 (2)	0.035*
O21w	0.4617 (4)	0.5095 (3)	0.36387 (19)	0.0371 (9)
H211	0.532 (3)	0.535 (4)	0.3960 (19)	0.044*
H212	0.373 (2)	0.506 (4)	0.381 (2)	0.044*
O22w	0.5382 (4)	1.0058 (3)	0.14203 (19)	0.0378 (9)
H221	0.482 (4)	0.984 (4)	0.1041 (16)	0.045*
H222	0.6317 (18)	1.008 (4)	0.134 (2)	0.045*
O23w	0.868 (2)	0.4466 (15)	−0.0974 (11)	0.141 (7)	0.50
H231	0.90 (3)	0.499 (9)	−0.122 (10)	0.169*	0.50
H232	0.90 (3)	0.400 (10)	−0.115 (11)	0.169*	0.50
O23'	0.968 (3)	0.480 (2)	−0.0420 (12)	0.225 (12)	0.50
H233	1.0000	0.5000	0.0000	0.271*
H234	0.873 (15)	0.45 (3)	−0.043 (5)	0.271*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0214 (3)	0.0301 (3)	0.0203 (3)	0.0092 (2)	0.0011 (2)	0.0027 (2)
V1	0.0215 (4)	0.0228 (4)	0.0162 (4)	0.0075 (3)	−0.0002 (3)	−0.0019 (3)
V2	0.0216 (4)	0.0215 (4)	0.0154 (4)	0.0045 (3)	−0.0005 (3)	0.0026 (3)
V3	0.0233 (4)	0.0243 (4)	0.0242 (4)	0.0120 (3)	−0.0041 (3)	−0.0005 (3)
V4	0.0251 (4)	0.0183 (4)	0.0243 (4)	0.0010 (3)	−0.0020 (3)	0.0008 (3)
V5	0.0127 (3)	0.0215 (4)	0.0160 (4)	0.0037 (3)	−0.0008 (3)	−0.0008 (3)
V6	0.0228 (4)	0.0181 (4)	0.0225 (4)	−0.0005 (3)	−0.0021 (3)	0.0013 (3)
V7	0.0217 (4)	0.0203 (4)	0.0149 (4)	0.0065 (3)	0.0000 (3)	−0.0017 (3)
V8	0.0129 (3)	0.0204 (4)	0.0155 (4)	0.0040 (3)	−0.0012 (3)	0.0000 (3)
V9	0.0242 (4)	0.0227 (4)	0.0233 (4)	0.0108 (3)	−0.0033 (3)	−0.0002 (3)
V10	0.0195 (4)	0.0199 (4)	0.0151 (4)	0.0036 (3)	0.0005 (3)	0.0022 (3)
Na1	0.0464 (18)	0.0416 (18)	0.047 (2)	−0.0059 (14)	−0.0150 (15)	0.0167 (15)
Na2	0.0487 (13)	0.0462 (13)	0.0348 (12)	0.0204 (10)	−0.0023 (10)	0.0026 (10)
Na3	0.0314 (10)	0.0393 (11)	0.0311 (11)	0.0074 (9)	0.0012 (8)	0.0030 (9)
Na4	0.0481 (13)	0.0412 (12)	0.0375 (12)	0.0176 (10)	−0.0003 (10)	0.0048 (10)
Na5	0.0368 (15)	0.0285 (14)	0.0376 (17)	−0.0031 (12)	−0.0055 (13)	0.0086 (12)
O1	0.0155 (14)	0.0172 (14)	0.0163 (15)	0.0048 (11)	−0.0004 (11)	−0.0010 (12)
O2	0.0349 (18)	0.0330 (18)	0.0186 (17)	0.0112 (15)	0.0003 (14)	−0.0053 (14)
O3	0.0272 (16)	0.0213 (16)	0.0198 (17)	0.0049 (13)	−0.0052 (13)	−0.0047 (13)
O4	0.0246 (16)	0.0294 (17)	0.0215 (17)	0.0142 (13)	−0.0028 (13)	−0.0049 (13)
O5	0.0301 (17)	0.0347 (18)	0.0168 (17)	0.0073 (14)	−0.0008 (13)	0.0028 (14)
O6	0.0264 (16)	0.0290 (17)	0.0170 (16)	0.0113 (14)	−0.0045 (13)	0.0026 (13)
O7	0.0259 (16)	0.0211 (16)	0.0222 (17)	0.0009 (13)	0.0016 (13)	0.0056 (13)
O8	0.0158 (14)	0.0232 (15)	0.0166 (15)	0.0048 (12)	0.0024 (11)	0.0006 (12)
O9	0.0162 (14)	0.0213 (15)	0.0137 (15)	0.0055 (12)	−0.0011 (11)	−0.0002 (12)
O10	0.0168 (15)	0.0298 (17)	0.0215 (17)	0.0069 (13)	−0.0016 (12)	−0.0013 (13)
O11	0.0170 (14)	0.0271 (16)	0.0209 (16)	0.0013 (12)	0.0009 (12)	0.0010 (13)
O12	0.0334 (18)	0.0361 (19)	0.034 (2)	0.0194 (15)	−0.0098 (15)	−0.0031 (15)
O13	0.0333 (18)	0.0178 (15)	0.0284 (18)	0.0091 (13)	−0.0052 (14)	0.0022 (13)
O14	0.042 (2)	0.0238 (18)	0.039 (2)	−0.0051 (15)	−0.0050 (16)	0.0005 (15)
O15	0.0168 (14)	0.0190 (15)	0.0163 (15)	0.0054 (12)	−0.0020 (11)	−0.0003 (12)
O16	0.0297 (18)	0.0250 (17)	0.036 (2)	−0.0059 (14)	−0.0031 (15)	0.0010 (15)
O17	0.0144 (14)	0.0259 (16)	0.0185 (16)	0.0014 (12)	−0.0026 (12)	0.0002 (12)
O18	0.0239 (16)	0.0191 (15)	0.0211 (17)	0.0037 (12)	−0.0035 (12)	−0.0036 (12)
O19	0.0256 (16)	0.0264 (16)	0.0182 (16)	0.0116 (13)	−0.0004 (13)	−0.0034 (13)
O20	0.0354 (18)	0.0334 (18)	0.0183 (17)	0.0115 (15)	0.0016 (14)	−0.0042 (14)
O21	0.0165 (14)	0.0207 (15)	0.0149 (15)	0.0064 (12)	−0.0004 (11)	−0.0011 (12)
O22	0.0244 (16)	0.0238 (16)	0.0182 (16)	0.0071 (13)	−0.0040 (12)	0.0025 (12)
O23	0.0282 (17)	0.0303 (18)	0.0183 (17)	0.0041 (14)	0.0010 (13)	0.0028 (13)
O24	0.0209 (15)	0.0228 (16)	0.0209 (16)	0.0007 (12)	0.0007 (12)	0.0032 (13)
O25	0.0293 (17)	0.0208 (16)	0.0213 (17)	0.0043 (13)	−0.0021 (13)	0.0022 (13)
O26	0.0358 (19)	0.0306 (18)	0.036 (2)	0.0186 (15)	−0.0057 (15)	0.0022 (15)
O27	0.0165 (14)	0.0271 (16)	0.0219 (16)	0.0087 (12)	−0.0022 (12)	0.0017 (13)
O28	0.0142 (14)	0.0241 (15)	0.0148 (15)	0.0066 (12)	0.0019 (11)	0.0010 (12)
O1w	0.099 (4)	0.042 (2)	0.048 (3)	0.030 (2)	0.001 (3)	0.003 (2)
O2w	0.052 (3)	0.041 (2)	0.046 (3)	0.014 (2)	−0.0086 (19)	−0.0107 (19)
O3w	0.076 (3)	0.069 (3)	0.038 (3)	0.048 (3)	−0.017 (2)	−0.014 (2)
O4w	0.059 (3)	0.039 (2)	0.035 (2)	0.0166 (19)	0.0054 (19)	0.0076 (17)
O5w	0.0301 (19)	0.052 (2)	0.028 (2)	0.0161 (17)	−0.0096 (15)	−0.0072 (17)
O6w	0.034 (2)	0.043 (2)	0.037 (2)	0.0143 (17)	0.0023 (17)	−0.0035 (17)
O7w	0.0315 (19)	0.060 (3)	0.034 (2)	0.0161 (18)	−0.0037 (16)	−0.0163 (19)
O8w	0.0284 (18)	0.047 (2)	0.032 (2)	0.0079 (16)	−0.0047 (15)	−0.0134 (17)
O9w	0.0319 (19)	0.050 (2)	0.026 (2)	0.0086 (17)	−0.0082 (15)	−0.0051 (16)
O10w	0.0295 (19)	0.060 (3)	0.032 (2)	0.0158 (18)	0.0004 (16)	−0.0091 (18)
O11w	0.079 (3)	0.087 (3)	0.053 (3)	0.055 (3)	−0.026 (3)	−0.023 (3)
O12w	0.042 (2)	0.041 (2)	0.028 (2)	0.0135 (17)	−0.0045 (16)	0.0096 (17)
O13w	0.057 (3)	0.048 (2)	0.046 (3)	0.024 (2)	0.003 (2)	0.001 (2)
O14w	0.047 (2)	0.035 (2)	0.036 (2)	0.0111 (18)	−0.0021 (17)	−0.0037 (17)
O15w	0.0243 (17)	0.0333 (19)	0.032 (2)	0.0069 (15)	0.0037 (14)	0.0061 (15)
O16w	0.034 (2)	0.055 (2)	0.029 (2)	0.0240 (18)	−0.0063 (16)	0.0008 (17)
O17w	0.0268 (17)	0.0334 (19)	0.038 (2)	0.0080 (15)	0.0021 (15)	0.0063 (16)
O18w	0.035 (2)	0.059 (2)	0.0251 (19)	0.0276 (18)	−0.0003 (16)	0.0046 (18)
O19w	0.0223 (16)	0.041 (2)	0.0164 (17)	0.0075 (15)	0.0042 (13)	0.0037 (14)
O20w	0.0196 (16)	0.049 (2)	0.0219 (18)	0.0123 (16)	0.0010 (13)	0.0062 (15)
O21w	0.0228 (17)	0.058 (2)	0.031 (2)	0.0108 (17)	0.0019 (15)	0.0021 (18)
O22w	0.0264 (18)	0.055 (2)	0.031 (2)	0.0086 (18)	−0.0022 (15)	0.0054 (18)
O23w	0.175 (17)	0.142 (15)	0.147 (16)	0.101 (14)	0.089 (13)	0.072 (13)
O23'	0.24 (3)	0.26 (3)	0.15 (2)	0.00 (2)	−0.03 (2)	0.05 (2)

Geometric parameters (Å, º) top

Ni1—O18w	2.038 (3)	V9—O25	1.834 (3)
Ni1—O16w	2.043 (3)	V9—O19ⁱⁱ	1.847 (3)
Ni1—O15w	2.046 (3)	V9—O22	1.892 (3)
Ni1—O17w	2.048 (3)	V9—O27	2.045 (3)
Ni1—O20w	2.051 (3)	V9—O15ⁱⁱ	2.320 (3)
Ni1—O19w	2.056 (3)	V10—O23	1.613 (3)
V1—O2	1.612 (3)	V10—O22	1.803 (3)
V1—O3	1.810 (3)	V10—O24	1.833 (3)
V1—O4	1.834 (3)	V10—O21	1.975 (3)
V1—O9ⁱ	1.974 (3)	V10—O28ⁱⁱ	2.030 (3)
V1—O8ⁱ	2.007 (3)	V10—O15ⁱⁱ	2.238 (3)
V1—O1	2.243 (3)	Na1—O1w	2.292 (5)
V2—O5	1.616 (3)	Na1—O1wⁱⁱⁱ	2.292 (5)
V2—O6	1.791 (3)	Na1—O2wⁱⁱⁱ	2.396 (4)
V2—O7	1.841 (3)	Na1—O2w	2.396 (4)
V2—O9	1.983 (3)	Na1—O14	2.453 (3)
V2—O8	2.009 (3)	Na1—O14ⁱⁱⁱ	2.453 (3)
V2—O1	2.227 (3)	Na2—O3w	2.334 (4)
V3—O12	1.609 (3)	Na2—O2w	2.358 (5)
V3—O13	1.822 (3)	Na2—O1w	2.373 (5)
V3—O4	1.852 (3)	Na2—O5w	2.407 (4)
V3—O6	1.895 (3)	Na2—O4w	2.451 (5)
V3—O10	2.045 (3)	Na2—O6w	2.569 (4)
V3—O1	2.288 (3)	Na3—O7w	2.398 (4)
V4—O14	1.594 (3)	Na3—O8w	2.406 (4)
V4—O13	1.830 (3)	Na3—O9w	2.408 (4)
V4—O7	1.864 (3)	Na3—O6w	2.424 (4)
V4—O3	1.882 (3)	Na3—O10w	2.424 (4)
V4—O11ⁱ	2.043 (3)	Na3—O5w	2.432 (4)
V4—O1	2.307 (3)	Na4—O11w	2.333 (5)
V5—O10	1.684 (3)	Na4—O9w	2.402 (4)
V5—O11	1.685 (3)	Na4—O14w	2.407 (4)
V5—O8ⁱ	1.886 (3)	Na4—O12w	2.412 (4)
V5—O9	1.951 (3)	Na4—O13w	2.434 (5)
V5—O1ⁱ	2.115 (3)	Na4—O10w	2.509 (5)
V5—O1	2.138 (3)	Na5—O16^iv	2.365 (3)
V6—O16	1.604 (3)	Na5—O16	2.365 (3)
V6—O25ⁱⁱ	1.830 (3)	Na5—O14w	2.370 (4)
V6—O24ⁱⁱ	1.866 (3)	Na5—O14w^iv	2.370 (4)
V6—O18	1.874 (3)	Na5—O13w^iv	2.447 (4)
V6—O17	2.049 (3)	Na5—O13w	2.447 (4)
V6—O15	2.274 (3)	O1—V5ⁱ	2.115 (3)
V7—O20	1.612 (3)	O8—V5ⁱ	1.886 (3)
V7—O18	1.817 (3)	O8—V1ⁱ	2.007 (3)
V7—O19	1.834 (3)	O9—V1ⁱ	1.974 (3)
V7—O28ⁱⁱ	1.987 (3)	O11—V4ⁱ	2.043 (3)
V7—O21	1.991 (3)	O15—V8ⁱⁱ	2.130 (3)
V7—O15	2.241 (3)	O15—V10ⁱⁱ	2.238 (3)
V8—O17	1.679 (3)	O15—V9ⁱⁱ	2.320 (3)
V8—O27	1.688 (3)	O19—V9ⁱⁱ	1.847 (3)
V8—O28	1.908 (3)	O24—V6ⁱⁱ	1.866 (3)
V8—O21	1.936 (3)	O25—V6ⁱⁱ	1.830 (3)
V8—O15	2.120 (3)	O28—V7ⁱⁱ	1.987 (3)
V8—O15ⁱⁱ	2.130 (3)	O28—V10ⁱⁱ	2.030 (3)
V9—O26	1.606 (3)	O23'—O23'^v	1.66 (4)

O18w—Ni1—O16w	178.33 (16)	O23—V10—O21	100.04 (14)
O18w—Ni1—O15w	89.71 (15)	O22—V10—O21	91.94 (13)
O16w—Ni1—O15w	88.89 (15)	O24—V10—O21	153.93 (13)
O18w—Ni1—O17w	89.52 (15)	O23—V10—O28ⁱⁱ	99.97 (14)
O16w—Ni1—O17w	91.88 (15)	O22—V10—O28ⁱⁱ	155.19 (13)
O15w—Ni1—O17w	179.18 (14)	O24—V10—O28ⁱⁱ	87.82 (13)
O18w—Ni1—O20w	93.46 (14)	O21—V10—O28ⁱⁱ	75.86 (11)
O16w—Ni1—O20w	87.38 (14)	O23—V10—O15ⁱⁱ	174.72 (14)
O15w—Ni1—O20w	88.08 (14)	O22—V10—O15ⁱⁱ	81.01 (12)
O17w—Ni1—O20w	92.25 (14)	O24—V10—O15ⁱⁱ	79.50 (12)
O18w—Ni1—O19w	87.02 (14)	O21—V10—O15ⁱⁱ	76.78 (11)
O16w—Ni1—O19w	92.14 (14)	O28ⁱⁱ—V10—O15ⁱⁱ	75.24 (11)
O15w—Ni1—O19w	92.18 (14)	O1w—Na1—O1wⁱⁱⁱ	180.0
O17w—Ni1—O19w	87.50 (14)	O1w—Na1—O2wⁱⁱⁱ	96.36 (15)
O20w—Ni1—O19w	179.45 (12)	O1wⁱⁱⁱ—Na1—O2wⁱⁱⁱ	83.64 (15)
O2—V1—O3	104.04 (16)	O1w—Na1—O2w	83.64 (15)
O2—V1—O4	101.52 (15)	O1wⁱⁱⁱ—Na1—O2w	96.36 (15)
O3—V1—O4	94.47 (14)	O2wⁱⁱⁱ—Na1—O2w	180.0 (2)
O2—V1—O9ⁱ	101.02 (14)	O1w—Na1—O14	79.99 (15)
O3—V1—O9ⁱ	90.72 (13)	O1wⁱⁱⁱ—Na1—O14	100.01 (15)
O4—V1—O9ⁱ	154.87 (13)	O2wⁱⁱⁱ—Na1—O14	79.68 (13)
O2—V1—O8ⁱ	99.55 (15)	O2w—Na1—O14	100.32 (13)
O3—V1—O8ⁱ	154.91 (13)	O1w—Na1—O14ⁱⁱⁱ	100.01 (15)
O4—V1—O8ⁱ	89.02 (13)	O1wⁱⁱⁱ—Na1—O14ⁱⁱⁱ	79.99 (15)
O9ⁱ—V1—O8ⁱ	76.39 (11)	O2wⁱⁱⁱ—Na1—O14ⁱⁱⁱ	100.32 (13)
O2—V1—O1	174.82 (14)	O2w—Na1—O14ⁱⁱⁱ	79.68 (13)
O3—V1—O1	80.58 (12)	O14—Na1—O14ⁱⁱⁱ	180.0
O4—V1—O1	80.24 (12)	O3w—Na2—O2w	172.91 (18)
O9ⁱ—V1—O1	76.39 (11)	O3w—Na2—O1w	90.23 (17)
O8ⁱ—V1—O1	75.54 (11)	O2w—Na2—O1w	82.73 (16)
O5—V2—O6	104.03 (15)	O3w—Na2—O5w	94.70 (16)
O5—V2—O7	102.53 (15)	O2w—Na2—O5w	92.29 (15)
O6—V2—O7	94.91 (14)	O1w—Na2—O5w	162.99 (18)
O5—V2—O9	99.68 (14)	O3w—Na2—O4w	88.77 (17)
O6—V2—O9	91.11 (13)	O2w—Na2—O4w	91.74 (15)
O7—V2—O9	154.79 (13)	O1w—Na2—O4w	100.92 (17)
O5—V2—O8	99.17 (14)	O5w—Na2—O4w	95.47 (15)
O6—V2—O8	155.13 (13)	O3w—Na2—O6w	86.18 (16)
O7—V2—O8	88.63 (13)	O2w—Na2—O6w	93.18 (15)
O9—V2—O8	76.14 (11)	O1w—Na2—O6w	78.36 (16)
O5—V2—O1	174.14 (14)	O5w—Na2—O6w	85.72 (14)
O6—V2—O1	80.86 (12)	O4w—Na2—O6w	174.89 (15)
O7—V2—O1	80.03 (12)	O7w—Na3—O8w	176.54 (16)
O9—V2—O1	76.80 (11)	O7w—Na3—O9w	97.29 (14)
O8—V2—O1	75.51 (11)	O8w—Na3—O9w	83.12 (14)
O12—V3—O13	104.21 (16)	O7w—Na3—O6w	83.35 (14)
O12—V3—O4	103.02 (16)	O8w—Na3—O6w	93.20 (14)
O13—V3—O4	93.04 (15)	O9w—Na3—O6w	91.60 (14)
O12—V3—O6	100.23 (15)	O7w—Na3—O10w	96.49 (14)
O13—V3—O6	90.59 (14)	O8w—Na3—O10w	86.97 (14)
O4—V3—O6	154.79 (13)	O9w—Na3—O10w	85.42 (14)
O12—V3—O10	98.91 (15)	O6w—Na3—O10w	176.98 (16)
O13—V3—O10	156.73 (13)	O7w—Na3—O5w	84.25 (14)
O4—V3—O10	84.21 (13)	O8w—Na3—O5w	95.34 (13)
O6—V3—O10	82.69 (13)	O9w—Na3—O5w	178.46 (15)
O12—V3—O1	173.30 (14)	O6w—Na3—O5w	88.44 (14)
O13—V3—O1	82.08 (12)	O10w—Na3—O5w	94.54 (15)
O4—V3—O1	78.66 (12)	O11w—Na4—O9w	97.22 (17)
O6—V3—O1	77.15 (11)	O11w—Na4—O14w	174.50 (18)
O10—V3—O1	74.72 (11)	O9w—Na4—O14w	88.09 (14)
O14—V4—O13	104.81 (17)	O11w—Na4—O12w	93.86 (18)
O14—V4—O7	101.27 (16)	O9w—Na4—O12w	93.09 (15)
O13—V4—O7	91.06 (14)	O14w—Na4—O12w	87.26 (14)
O14—V4—O3	103.02 (16)	O11w—Na4—O13w	89.17 (17)
O13—V4—O3	90.90 (14)	O9w—Na4—O13w	172.63 (16)
O7—V4—O3	154.25 (13)	O14w—Na4—O13w	85.45 (15)
O14—V4—O11ⁱ	98.58 (16)	O12w—Na4—O13w	90.15 (15)
O13—V4—O11ⁱ	156.61 (13)	O11w—Na4—O10w	87.62 (17)
O7—V4—O11ⁱ	84.53 (13)	O9w—Na4—O10w	83.70 (14)
O3—V4—O11ⁱ	83.55 (13)	O14w—Na4—O10w	91.55 (14)
O14—V4—O1	173.73 (15)	O12w—Na4—O10w	176.62 (16)
O13—V4—O1	81.40 (12)	O13w—Na4—O10w	92.92 (15)
O7—V4—O1	77.46 (12)	O16^iv—Na5—O16	180.00 (8)
O3—V4—O1	77.46 (12)	O16^iv—Na5—O14w	98.31 (13)
O11ⁱ—V4—O1	75.21 (11)	O16—Na5—O14w	81.69 (13)
O10—V5—O11	107.03 (15)	O16^iv—Na5—O14w^iv	81.69 (13)
O10—V5—O8ⁱ	98.10 (14)	O16—Na5—O14w^iv	98.31 (13)
O11—V5—O8ⁱ	99.47 (14)	O14w—Na5—O14w^iv	180.000 (1)
O10—V5—O9	96.07 (13)	O16^iv—Na5—O13w^iv	99.42 (13)
O11—V5—O9	96.11 (14)	O16—Na5—O13w^iv	80.58 (13)
O8ⁱ—V5—O9	154.82 (12)	O14w—Na5—O13w^iv	94.04 (14)
O10—V5—O1ⁱ	164.61 (13)	O14w^iv—Na5—O13w^iv	85.96 (14)
O11—V5—O1ⁱ	88.24 (13)	O16^iv—Na5—O13w	80.58 (13)
O8ⁱ—V5—O1ⁱ	80.84 (12)	O16—Na5—O13w	99.42 (13)
O9—V5—O1ⁱ	80.00 (11)	O14w—Na5—O13w	85.96 (14)
O10—V5—O1	86.37 (13)	O14w^iv—Na5—O13w	94.04 (14)
O11—V5—O1	166.37 (13)	O13w^iv—Na5—O13w	180.000 (1)
O8ⁱ—V5—O1	80.61 (12)	V5ⁱ—O1—V5	101.71 (11)
O9—V5—O1	79.63 (11)	V5ⁱ—O1—V2	93.04 (11)
O1ⁱ—V5—O1	78.29 (11)	V5—O1—V2	93.22 (11)
O16—V6—O25ⁱⁱ	104.52 (16)	V5ⁱ—O1—V1	93.19 (11)
O16—V6—O24ⁱⁱ	100.89 (16)	V5—O1—V1	92.53 (11)
O25ⁱⁱ—V6—O24ⁱⁱ	91.85 (14)	V2—O1—V1	170.51 (14)
O16—V6—O18	102.49 (16)	V5ⁱ—O1—V3	170.28 (14)
O25ⁱⁱ—V6—O18	90.87 (13)	V5—O1—V3	88.01 (10)
O24ⁱⁱ—V6—O18	154.96 (13)	V2—O1—V3	86.67 (10)
O16—V6—O17	97.21 (15)	V1—O1—V3	85.99 (10)
O25ⁱⁱ—V6—O17	158.26 (13)	V5ⁱ—O1—V4	87.09 (10)
O24ⁱⁱ—V6—O17	84.41 (13)	V5—O1—V4	171.18 (14)
O18—V6—O17	83.90 (13)	V2—O1—V4	86.85 (10)
O16—V6—O15	172.66 (14)	V1—O1—V4	86.31 (10)
O25ⁱⁱ—V6—O15	82.78 (12)	V3—O1—V4	83.19 (9)
O24ⁱⁱ—V6—O15	77.90 (12)	V1—O3—V4	114.91 (16)
O18—V6—O15	77.76 (12)	V1—O4—V3	113.95 (15)
O17—V6—O15	75.49 (11)	V2—O6—V3	114.41 (15)
O20—V7—O18	103.30 (16)	V2—O7—V4	114.54 (15)
O20—V7—O19	102.61 (15)	V5ⁱ—O8—V1ⁱ	108.81 (14)
O18—V7—O19	93.92 (14)	V5ⁱ—O8—V2	107.96 (14)
O20—V7—O28ⁱⁱ	100.28 (15)	V1ⁱ—O8—V2	99.01 (12)
O18—V7—O28ⁱⁱ	154.52 (13)	V5—O9—V1ⁱ	107.58 (13)
O19—V7—O28ⁱⁱ	90.23 (13)	V5—O9—V2	107.49 (13)
O20—V7—O21	100.30 (14)	V1ⁱ—O9—V2	101.04 (12)
O18—V7—O21	89.84 (12)	V5—O10—V3	110.85 (15)
O19—V7—O21	155.25 (13)	V5—O11—V4ⁱ	109.42 (15)
O28ⁱⁱ—V7—O21	76.49 (11)	V3—O13—V4	113.31 (15)
O20—V7—O15	175.39 (14)	V4—O14—Na1	167.3 (2)
O18—V7—O15	79.77 (12)	V8—O15—V8ⁱⁱ	101.45 (12)
O19—V7—O15	80.47 (12)	V8—O15—V10ⁱⁱ	93.87 (11)
O28ⁱⁱ—V7—O15	76.15 (11)	V8ⁱⁱ—O15—V10ⁱⁱ	92.35 (11)
O21—V7—O15	76.14 (11)	V8—O15—V7	93.33 (11)
O17—V8—O27	106.93 (14)	V8ⁱⁱ—O15—V7	92.41 (11)
O17—V8—O28	98.27 (14)	V10ⁱⁱ—O15—V7	170.41 (14)
O27—V8—O28	97.45 (13)	V8—O15—V6	87.63 (10)
O17—V8—O21	96.70 (14)	V8ⁱⁱ—O15—V6	170.92 (14)
O27—V8—O21	97.05 (13)	V10ⁱⁱ—O15—V6	87.03 (10)
O28—V8—O21	155.13 (12)	V7—O15—V6	86.96 (10)
O17—V8—O15	87.77 (12)	V8—O15—V9ⁱⁱ	170.77 (14)
O27—V8—O15	165.29 (13)	V8ⁱⁱ—O15—V9ⁱⁱ	87.76 (10)
O28—V8—O15	80.63 (11)	V10ⁱⁱ—O15—V9ⁱⁱ	86.20 (10)
O21—V8—O15	80.23 (11)	V7—O15—V9ⁱⁱ	85.68 (10)
O17—V8—O15ⁱⁱ	166.29 (12)	V6—O15—V9ⁱⁱ	83.16 (9)
O27—V8—O15ⁱⁱ	86.74 (13)	V6—O16—Na5	154.7 (2)
O28—V8—O15ⁱⁱ	80.51 (12)	V8—O17—V6	109.10 (14)
O21—V8—O15ⁱⁱ	80.25 (12)	V7—O18—V6	114.68 (16)
O15—V8—O15ⁱⁱ	78.55 (12)	V7—O19—V9ⁱⁱ	114.82 (15)
O26—V9—O25	104.20 (16)	V8—O21—V10	107.45 (14)
O26—V9—O19ⁱⁱ	103.30 (16)	V8—O21—V7	107.81 (13)
O25—V9—O19ⁱⁱ	92.33 (14)	V10—O21—V7	101.01 (12)
O26—V9—O22	100.72 (15)	V10—O22—V9	114.92 (15)
O25—V9—O22	90.65 (14)	V10—O24—V6ⁱⁱ	114.28 (15)
O19ⁱⁱ—V9—O22	154.26 (13)	V6ⁱⁱ—O25—V9	112.63 (15)
O26—V9—O27	100.13 (15)	V8—O27—V9	111.28 (14)
O25—V9—O27	155.59 (13)	V8—O28—V7ⁱⁱ	108.24 (14)
O19ⁱⁱ—V9—O27	84.01 (13)	V8—O28—V10ⁱⁱ	107.90 (13)
O22—V9—O27	82.79 (13)	V7ⁱⁱ—O28—V10ⁱⁱ	99.24 (12)
O26—V9—O15ⁱⁱ	174.07 (15)	Na1—O1w—Na2	97.70 (17)
O25—V9—O15ⁱⁱ	81.42 (12)	Na2—O2w—Na1	95.30 (15)
O19ⁱⁱ—V9—O15ⁱⁱ	78.09 (12)	Na2—O5w—Na3	94.37 (14)
O22—V9—O15ⁱⁱ	77.09 (11)	Na3—O6w—Na2	90.60 (14)
O27—V9—O15ⁱⁱ	74.20 (10)	Na4—O9w—Na3	96.56 (14)
O23—V10—O22	103.43 (15)	Na3—O10w—Na4	93.39 (14)
O23—V10—O24	102.75 (15)	Na4—O13w—Na5	92.28 (14)
O22—V10—O24	94.91 (14)	Na5—O14w—Na4	94.86 (14)

O10—V5—O1—V5ⁱ	178.67 (14)	O28—V8—O15—V6	97.93 (12)
O11—V5—O1—V5ⁱ	9.0 (6)	O21—V8—O15—V6	−98.02 (12)
O8ⁱ—V5—O1—V5ⁱ	−82.50 (13)	O15ⁱⁱ—V8—O15—V6	−179.95 (16)
O9—V5—O1—V5ⁱ	81.81 (12)	O18—V7—O15—V8	−81.32 (12)
O1ⁱ—V5—O1—V5ⁱ	0.0	O19—V7—O15—V8	−177.10 (13)
O10—V5—O1—V2	84.89 (13)	O28ⁱⁱ—V7—O15—V8	90.29 (12)
O11—V5—O1—V2	−84.8 (6)	O21—V7—O15—V8	11.06 (10)
O8ⁱ—V5—O1—V2	−176.28 (12)	O18—V7—O15—V8ⁱⁱ	177.06 (13)
O9—V5—O1—V2	−11.96 (10)	O19—V7—O15—V8ⁱⁱ	81.27 (12)
O1ⁱ—V5—O1—V2	−93.78 (12)	O28ⁱⁱ—V7—O15—V8ⁱⁱ	−11.34 (10)
O10—V5—O1—V1	−87.55 (13)	O21—V7—O15—V8ⁱⁱ	−90.56 (11)
O11—V5—O1—V1	102.8 (5)	O18—V7—O15—V6	6.12 (11)
O8ⁱ—V5—O1—V1	11.28 (10)	O19—V7—O15—V6	−89.66 (12)
O9—V5—O1—V1	175.60 (12)	O28ⁱⁱ—V7—O15—V6	177.73 (11)
O1ⁱ—V5—O1—V1	93.78 (12)	O21—V7—O15—V6	98.51 (11)
O10—V5—O1—V3	−1.66 (12)	O18—V7—O15—V9ⁱⁱ	89.48 (12)
O11—V5—O1—V3	−171.3 (5)	O19—V7—O15—V9ⁱⁱ	−6.30 (11)
O8ⁱ—V5—O1—V3	97.17 (11)	O28ⁱⁱ—V7—O15—V9ⁱⁱ	−98.91 (11)
O9—V5—O1—V3	−98.51 (11)	O21—V7—O15—V9ⁱⁱ	−178.13 (11)
O1ⁱ—V5—O1—V3	179.68 (16)	O25ⁱⁱ—V6—O15—V8	179.96 (13)
O6—V2—O1—V5ⁱ	176.65 (13)	O24ⁱⁱ—V6—O15—V8	−86.57 (12)
O7—V2—O1—V5ⁱ	79.97 (12)	O18—V6—O15—V8	87.48 (12)
O9—V2—O1—V5ⁱ	−90.03 (11)	O17—V6—O15—V8	0.70 (10)
O8—V2—O1—V5ⁱ	−11.19 (10)	O25ⁱⁱ—V6—O15—V10ⁱⁱ	−86.04 (12)
O6—V2—O1—V5	−81.43 (13)	O24ⁱⁱ—V6—O15—V10ⁱⁱ	7.43 (11)
O7—V2—O1—V5	−178.11 (13)	O18—V6—O15—V10ⁱⁱ	−178.51 (12)
O9—V2—O1—V5	11.89 (10)	O17—V6—O15—V10ⁱⁱ	94.71 (11)
O8—V2—O1—V5	90.73 (12)	O25ⁱⁱ—V6—O15—V7	86.50 (12)
O6—V2—O1—V3	6.39 (11)	O24ⁱⁱ—V6—O15—V7	179.96 (12)
O7—V2—O1—V3	−90.29 (12)	O18—V6—O15—V7	−5.98 (11)
O9—V2—O1—V3	99.71 (11)	O17—V6—O15—V7	−92.76 (11)
O8—V2—O1—V3	178.55 (12)	O25ⁱⁱ—V6—O15—V9ⁱⁱ	0.49 (11)
O6—V2—O1—V4	89.74 (12)	O24ⁱⁱ—V6—O15—V9ⁱⁱ	93.95 (12)
O7—V2—O1—V4	−6.94 (11)	O18—V6—O15—V9ⁱⁱ	−91.99 (12)
O9—V2—O1—V4	−176.94 (11)	O17—V6—O15—V9ⁱⁱ	−178.77 (12)
O8—V2—O1—V4	−98.10 (11)	O25ⁱⁱ—V6—O16—Na5	13.2 (5)
O3—V1—O1—V5ⁱ	−81.15 (12)	O24ⁱⁱ—V6—O16—Na5	−81.6 (5)
O4—V1—O1—V5ⁱ	−177.40 (13)	O18—V6—O16—Na5	107.4 (5)
O9ⁱ—V1—O1—V5ⁱ	11.90 (10)	O17—V6—O16—Na5	−167.2 (4)
O8ⁱ—V1—O1—V5ⁱ	91.09 (12)	O14w—Na5—O16—V6	−112.2 (5)
O3—V1—O1—V5	176.97 (13)	O14w^iv—Na5—O16—V6	67.8 (5)
O4—V1—O1—V5	80.72 (12)	O13w^iv—Na5—O16—V6	−16.6 (5)
O9ⁱ—V1—O1—V5	−89.98 (11)	O13w—Na5—O16—V6	163.4 (5)
O8ⁱ—V1—O1—V5	−10.79 (10)	O27—V8—O17—V6	−179.65 (14)
O3—V1—O1—V3	89.14 (12)	O28—V8—O17—V6	−79.21 (15)
O4—V1—O1—V3	−7.10 (11)	O21—V8—O17—V6	80.86 (15)
O9ⁱ—V1—O1—V3	−177.81 (12)	O15—V8—O17—V6	0.98 (14)
O8ⁱ—V1—O1—V3	−98.62 (11)	O15ⁱⁱ—V8—O17—V6	4.6 (6)
O3—V1—O1—V4	5.72 (11)	O16—V6—O17—V8	178.29 (18)
O4—V1—O1—V4	−90.52 (12)	O25ⁱⁱ—V6—O17—V8	−2.9 (4)
O9ⁱ—V1—O1—V4	98.77 (11)	O24ⁱⁱ—V6—O17—V8	77.98 (16)
O8ⁱ—V1—O1—V4	177.96 (11)	O18—V6—O17—V8	−79.83 (16)
O13—V3—O1—V5	179.66 (13)	O15—V6—O17—V8	−0.94 (14)
O4—V3—O1—V5	−85.61 (13)	O20—V7—O18—V6	175.34 (17)
O6—V3—O1—V5	87.23 (13)	O19—V7—O18—V6	71.39 (17)
O10—V3—O1—V5	1.41 (10)	O28ⁱⁱ—V7—O18—V6	−27.4 (4)
O13—V3—O1—V2	86.32 (13)	O21—V7—O18—V6	−84.12 (16)
O4—V3—O1—V2	−178.95 (13)	O15—V7—O18—V6	−8.18 (14)
O6—V3—O1—V2	−6.11 (11)	O16—V6—O18—V7	−179.39 (18)
O10—V3—O1—V2	−91.93 (12)	O25ⁱⁱ—V6—O18—V7	−74.31 (17)
O13—V3—O1—V1	−87.66 (13)	O24ⁱⁱ—V6—O18—V7	22.0 (4)
O4—V3—O1—V1	7.07 (11)	O17—V6—O18—V7	84.54 (16)
O6—V3—O1—V1	179.91 (12)	O15—V6—O18—V7	8.12 (14)
O10—V3—O1—V1	94.09 (12)	O20—V7—O19—V9ⁱⁱ	−174.79 (17)
O13—V3—O1—V4	−0.91 (12)	O18—V7—O19—V9ⁱⁱ	−70.22 (18)
O4—V3—O1—V4	93.83 (12)	O28ⁱⁱ—V7—O19—V9ⁱⁱ	84.62 (17)
O6—V3—O1—V4	−93.33 (12)	O21—V7—O19—V9ⁱⁱ	27.9 (4)
O10—V3—O1—V4	−179.15 (12)	O15—V7—O19—V9ⁱⁱ	8.71 (15)
O13—V4—O1—V5ⁱ	−179.32 (13)	O17—V8—O21—V10	178.58 (14)
O7—V4—O1—V5ⁱ	−86.29 (12)	O27—V8—O21—V10	70.52 (15)
O3—V4—O1—V5ⁱ	87.82 (12)	O28—V8—O21—V10	−54.7 (3)
O11ⁱ—V4—O1—V5ⁱ	1.28 (10)	O15—V8—O21—V10	−94.86 (13)
O13—V4—O1—V2	−86.11 (12)	O15ⁱⁱ—V8—O21—V10	−14.93 (12)
O7—V4—O1—V2	6.92 (11)	O17—V8—O21—V7	−73.29 (15)
O3—V4—O1—V2	−178.97 (12)	O27—V8—O21—V7	178.65 (14)
O11ⁱ—V4—O1—V2	94.49 (11)	O28—V8—O21—V7	53.4 (3)
O13—V4—O1—V1	87.30 (12)	O15—V8—O21—V7	13.27 (12)
O7—V4—O1—V1	−179.68 (12)	O15ⁱⁱ—V8—O21—V7	93.20 (13)
O3—V4—O1—V1	−5.56 (11)	O23—V10—O21—V8	−169.93 (15)
O11ⁱ—V4—O1—V1	−92.10 (11)	O22—V10—O21—V8	−65.92 (15)
O13—V4—O1—V3	0.91 (12)	O24—V10—O21—V8	39.4 (3)
O7—V4—O1—V3	93.93 (12)	O28ⁱⁱ—V10—O21—V8	92.22 (14)
O3—V4—O1—V3	−91.95 (12)	O15ⁱⁱ—V10—O21—V8	14.38 (11)
O11ⁱ—V4—O1—V3	−178.50 (12)	O23—V10—O21—V7	77.26 (15)
O2—V1—O3—V4	174.65 (17)	O22—V10—O21—V7	−178.74 (13)
O4—V1—O3—V4	71.59 (18)	O24—V10—O21—V7	−73.4 (3)
O9ⁱ—V1—O3—V4	−83.80 (17)	O28ⁱⁱ—V10—O21—V7	−20.60 (12)
O8ⁱ—V1—O3—V4	−25.7 (4)	O15ⁱⁱ—V10—O21—V7	−98.44 (13)
O1—V1—O3—V4	−7.73 (15)	O20—V7—O21—V8	170.26 (15)
O14—V4—O3—V1	−178.82 (18)	O18—V7—O21—V8	66.76 (15)
O13—V4—O3—V1	−73.40 (18)	O19—V7—O21—V8	−32.3 (4)
O7—V4—O3—V1	20.9 (4)	O28ⁱⁱ—V7—O21—V8	−91.53 (14)
O11ⁱ—V4—O3—V1	83.82 (17)	O15—V7—O21—V8	−12.73 (12)
O1—V4—O3—V1	7.59 (14)	O20—V7—O21—V10	−77.20 (16)
O2—V1—O4—V3	−175.35 (17)	O18—V7—O21—V10	179.31 (14)
O3—V1—O4—V3	−70.03 (18)	O19—V7—O21—V10	80.3 (3)
O9ⁱ—V1—O4—V3	31.3 (4)	O28ⁱⁱ—V7—O21—V10	21.01 (12)
O8ⁱ—V1—O4—V3	85.10 (17)	O15—V7—O21—V10	99.81 (13)
O1—V1—O4—V3	9.60 (15)	O23—V10—O22—V9	−174.95 (16)
O12—V3—O4—V1	177.18 (18)	O24—V10—O22—V9	−70.58 (18)
O13—V3—O4—V1	71.83 (18)	O21—V10—O22—V9	84.25 (17)
O6—V3—O4—V1	−26.0 (4)	O28ⁱⁱ—V10—O22—V9	24.9 (4)
O10—V3—O4—V1	−84.99 (17)	O15ⁱⁱ—V10—O22—V9	7.96 (15)
O1—V3—O4—V1	−9.46 (15)	O26—V9—O22—V10	177.85 (18)
O5—V2—O6—V3	174.82 (17)	O25—V9—O22—V10	73.27 (17)
O7—V2—O6—V3	70.59 (18)	O19ⁱⁱ—V9—O22—V10	−23.5 (4)
O9—V2—O6—V3	−84.91 (17)	O27—V9—O22—V10	−83.15 (17)
O8—V2—O6—V3	−26.8 (4)	O15ⁱⁱ—V9—O22—V10	−7.78 (14)
O1—V2—O6—V3	−8.47 (15)	O23—V10—O24—V6ⁱⁱ	174.81 (17)
O12—V3—O6—V2	−177.95 (18)	O22—V10—O24—V6ⁱⁱ	69.83 (17)
O13—V3—O6—V2	−73.39 (18)	O21—V10—O24—V6ⁱⁱ	−34.8 (4)
O4—V3—O6—V2	25.0 (4)	O28ⁱⁱ—V10—O24—V6ⁱⁱ	−85.46 (16)
O10—V3—O6—V2	84.26 (17)	O15ⁱⁱ—V10—O24—V6ⁱⁱ	−10.07 (15)
O1—V3—O6—V2	8.34 (15)	O26—V9—O25—V6ⁱⁱ	−178.72 (17)
O5—V2—O7—V4	−175.93 (17)	O19ⁱⁱ—V9—O25—V6ⁱⁱ	76.94 (17)
O6—V2—O7—V4	−70.36 (18)	O22—V9—O25—V6ⁱⁱ	−77.49 (17)
O9—V2—O7—V4	32.8 (4)	O27—V9—O25—V6ⁱⁱ	−3.7 (4)
O8—V2—O7—V4	84.98 (17)	O15ⁱⁱ—V9—O25—V6ⁱⁱ	−0.65 (15)
O1—V2—O7—V4	9.45 (15)	O17—V8—O27—V9	179.91 (14)
O14—V4—O7—V2	177.08 (18)	O28—V8—O27—V9	78.87 (16)
O13—V4—O7—V2	71.75 (17)	O21—V8—O27—V9	−80.86 (16)
O3—V4—O7—V2	−22.5 (4)	O15—V8—O27—V9	−2.5 (6)
O11ⁱ—V4—O7—V2	−85.23 (17)	O15ⁱⁱ—V8—O27—V9	−1.10 (15)
O1—V4—O7—V2	−9.20 (14)	O26—V9—O27—V8	179.28 (18)
O5—V2—O8—V5ⁱ	−169.32 (15)	O25—V9—O27—V8	4.2 (4)
O6—V2—O8—V5ⁱ	31.9 (4)	O19ⁱⁱ—V9—O27—V8	−78.24 (17)
O7—V2—O8—V5ⁱ	−66.85 (15)	O22—V9—O27—V8	79.62 (17)
O9—V2—O8—V5ⁱ	92.88 (15)	O15ⁱⁱ—V9—O27—V8	1.05 (14)
O1—V2—O8—V5ⁱ	13.20 (12)	O17—V8—O28—V7ⁱⁱ	−179.99 (14)
O5—V2—O8—V1ⁱ	77.44 (15)	O27—V8—O28—V7ⁱⁱ	−71.58 (15)
O6—V2—O8—V1ⁱ	−81.4 (3)	O21—V8—O28—V7ⁱⁱ	53.6 (3)
O7—V2—O8—V1ⁱ	179.90 (13)	O15—V8—O28—V7ⁱⁱ	93.67 (13)
O9—V2—O8—V1ⁱ	−20.36 (11)	O15ⁱⁱ—V8—O28—V7ⁱⁱ	13.83 (12)
O1—V2—O8—V1ⁱ	−100.04 (12)	O17—V8—O28—V10ⁱⁱ	73.51 (15)
O10—V5—O9—V1ⁱ	−179.15 (14)	O27—V8—O28—V10ⁱⁱ	−178.08 (14)
O11—V5—O9—V1ⁱ	72.93 (15)	O21—V8—O28—V10ⁱⁱ	−52.9 (3)
O8ⁱ—V5—O9—V1ⁱ	−55.2 (3)	O15—V8—O28—V10ⁱⁱ	−12.83 (12)
O1ⁱ—V5—O9—V1ⁱ	−14.19 (12)	O15ⁱⁱ—V8—O28—V10ⁱⁱ	−92.67 (13)
O1—V5—O9—V1ⁱ	−93.98 (13)	O2wⁱⁱⁱ—Na1—O1w—Na2	173.96 (16)
O10—V5—O9—V2	−71.07 (15)	O2w—Na1—O1w—Na2	−6.04 (16)
O11—V5—O9—V2	−178.98 (14)	O14—Na1—O1w—Na2	95.65 (17)
O8ⁱ—V5—O9—V2	52.9 (3)	O14ⁱⁱⁱ—Na1—O1w—Na2	−84.35 (17)
O1ⁱ—V5—O9—V2	93.90 (13)	O3w—Na2—O1w—Na1	−173.01 (19)
O1—V5—O9—V2	14.10 (12)	O2w—Na2—O1w—Na1	6.15 (17)
O5—V2—O9—V5	171.11 (15)	O5w—Na2—O1w—Na1	79.9 (6)
O6—V2—O9—V5	66.67 (15)	O4w—Na2—O1w—Na1	−84.22 (19)
O7—V2—O9—V5	−37.3 (4)	O6w—Na2—O1w—Na1	100.93 (18)
O8—V2—O9—V5	−91.74 (14)	O1w—Na2—O2w—Na1	−5.86 (15)
O1—V2—O9—V5	−13.67 (11)	O5w—Na2—O2w—Na1	−169.52 (14)
O5—V2—O9—V1ⁱ	−76.29 (15)	O4w—Na2—O2w—Na1	94.93 (15)
O6—V2—O9—V1ⁱ	179.27 (13)	O6w—Na2—O2w—Na1	−83.69 (15)
O7—V2—O9—V1ⁱ	75.2 (3)	O1w—Na1—O2w—Na2	6.05 (16)
O8—V2—O9—V1ⁱ	20.85 (12)	O1wⁱⁱⁱ—Na1—O2w—Na2	−173.95 (16)
O1—V2—O9—V1ⁱ	98.92 (13)	O14—Na1—O2w—Na2	−72.52 (15)
O11—V5—O10—V3	179.45 (14)	O14ⁱⁱⁱ—Na1—O2w—Na2	107.48 (15)
O8ⁱ—V5—O10—V3	−77.99 (16)	O3w—Na2—O5w—Na3	−92.75 (17)
O9—V5—O10—V3	81.14 (16)	O2w—Na2—O5w—Na3	86.07 (15)
O1ⁱ—V5—O10—V3	6.9 (6)	O1w—Na2—O5w—Na3	13.6 (6)
O1—V5—O10—V3	1.98 (15)	O4w—Na2—O5w—Na3	178.04 (14)
O12—V3—O10—V5	−179.81 (18)	O6w—Na2—O5w—Na3	−6.95 (13)
O13—V3—O10—V5	−6.3 (4)	O7w—Na3—O5w—Na2	−76.13 (14)
O4—V3—O10—V5	77.88 (17)	O8w—Na3—O5w—Na2	100.42 (14)
O6—V3—O10—V5	−80.54 (17)	O6w—Na3—O5w—Na2	7.35 (14)
O1—V3—O10—V5	−1.92 (14)	O10w—Na3—O5w—Na2	−172.21 (13)
O10—V5—O11—V4ⁱ	−179.82 (14)	O7w—Na3—O6w—Na2	77.53 (14)
O8ⁱ—V5—O11—V4ⁱ	78.61 (16)	O8w—Na3—O6w—Na2	−102.12 (13)
O9—V5—O11—V4ⁱ	−81.54 (15)	O9w—Na3—O6w—Na2	174.68 (13)
O1ⁱ—V5—O11—V4ⁱ	−1.80 (15)	O5w—Na3—O6w—Na2	−6.86 (13)
O1—V5—O11—V4ⁱ	−10.6 (6)	O3w—Na2—O6w—Na3	101.96 (16)
O12—V3—O13—V4	178.89 (18)	O2w—Na2—O6w—Na3	−85.11 (15)
O4—V3—O13—V4	−76.86 (18)	O1w—Na2—O6w—Na3	−167.02 (17)
O6—V3—O13—V4	78.18 (18)	O5w—Na2—O6w—Na3	6.95 (13)
O10—V3—O13—V4	5.5 (5)	O11w—Na4—O9w—Na3	94.06 (18)
O1—V3—O13—V4	1.24 (16)	O14w—Na4—O9w—Na3	−84.50 (15)
O14—V4—O13—V3	179.67 (19)	O12w—Na4—O9w—Na3	−171.66 (14)
O7—V4—O13—V3	−78.38 (18)	O10w—Na4—O9w—Na3	7.27 (13)
O3—V4—O13—V3	75.94 (18)	O7w—Na3—O9w—Na4	−103.47 (15)
O11ⁱ—V4—O13—V3	0.2 (5)	O8w—Na3—O9w—Na4	79.99 (15)
O1—V4—O13—V3	−1.23 (16)	O6w—Na3—O9w—Na4	173.02 (14)
O13—V4—O14—Na1	120.9 (9)	O10w—Na3—O9w—Na4	−7.50 (14)
O7—V4—O14—Na1	26.8 (10)	O7w—Na3—O10w—Na4	103.98 (14)
O3—V4—O14—Na1	−144.6 (9)	O8w—Na3—O10w—Na4	−76.18 (14)
O11ⁱ—V4—O14—Na1	−59.3 (10)	O9w—Na3—O10w—Na4	7.15 (13)
O1w—Na1—O14—V4	−118.9 (10)	O5w—Na3—O10w—Na4	−171.30 (13)
O1wⁱⁱⁱ—Na1—O14—V4	61.1 (10)	O11w—Na4—O10w—Na3	−104.72 (17)
O2wⁱⁱⁱ—Na1—O14—V4	142.7 (10)	O9w—Na4—O10w—Na3	−7.19 (13)
O2w—Na1—O14—V4	−37.3 (10)	O14w—Na4—O10w—Na3	80.72 (14)
O17—V8—O15—V8ⁱⁱ	179.12 (14)	O13w—Na4—O10w—Na3	166.24 (14)
O27—V8—O15—V8ⁱⁱ	1.5 (6)	O11w—Na4—O13w—Na5	−169.93 (18)
O28—V8—O15—V8ⁱⁱ	−82.12 (13)	O14w—Na4—O13w—Na5	8.97 (14)
O21—V8—O15—V8ⁱⁱ	81.93 (13)	O12w—Na4—O13w—Na5	96.22 (14)
O15ⁱⁱ—V8—O15—V8ⁱⁱ	0.0	O10w—Na4—O13w—Na5	−82.35 (14)
O17—V8—O15—V10ⁱⁱ	−87.69 (13)	O16^iv—Na5—O13w—Na4	−108.23 (15)
O27—V8—O15—V10ⁱⁱ	94.7 (5)	O16—Na5—O13w—Na4	71.77 (15)
O28—V8—O15—V10ⁱⁱ	11.07 (11)	O14w—Na5—O13w—Na4	−9.11 (14)
O21—V8—O15—V10ⁱⁱ	175.12 (12)	O14w^iv—Na5—O13w—Na4	170.89 (14)
O15ⁱⁱ—V8—O15—V10ⁱⁱ	93.19 (13)	O16^iv—Na5—O14w—Na4	89.09 (14)
O17—V8—O15—V7	85.98 (13)	O16—Na5—O14w—Na4	−90.91 (14)
O27—V8—O15—V7	−91.7 (5)	O13w^iv—Na5—O14w—Na4	−170.77 (14)
O28—V8—O15—V7	−175.26 (12)	O13w—Na5—O14w—Na4	9.23 (14)
O21—V8—O15—V7	−11.21 (10)	O9w—Na4—O14w—Na5	167.16 (14)
O15ⁱⁱ—V8—O15—V7	−93.14 (13)	O12w—Na4—O14w—Na5	−99.66 (14)
O17—V8—O15—V6	−0.83 (12)	O13w—Na4—O14w—Na5	−9.29 (14)
O27—V8—O15—V6	−178.5 (5)	O10w—Na4—O14w—Na5	83.52 (14)

Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y+1, −z; (iv) −x+1, −y, −z+1; (v) −x+2, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O23w	0.85 (1)	2.05 (5)	2.675 (15)	131 (6)
O1w—H12···O12^v	0.85 (1)	2.04 (2)	2.876 (5)	170 (5)
O2w—H21···O7w	0.85 (1)	2.11 (2)	2.946 (6)	166 (5)
O2w—H22···O15w	0.85 (1)	2.19 (3)	2.945 (5)	148 (4)
O3w—H31···O3^v	0.85 (1)	2.34 (3)	3.098 (5)	149 (5)
O3w—H32···O20	0.85 (1)	2.04 (2)	2.864 (5)	165 (6)
O4w—H41···O7	0.85 (1)	2.19 (3)	2.884 (5)	140 (4)
O4w—H42···O16w	0.85 (1)	1.95 (2)	2.789 (5)	170 (5)
O5w—H51···O21	0.85 (1)	2.03 (2)	2.831 (4)	158 (5)
O5w—H52···O21w	0.85 (1)	2.05 (2)	2.878 (5)	165 (4)
O6w—H61···O11^vi	0.85 (1)	2.20 (2)	3.039 (5)	170 (4)
O6w—H62···O4^v	0.85 (1)	2.06 (1)	2.908 (4)	175 (4)
O7w—H71···O3ⁱⁱⁱ	0.85 (1)	1.91 (1)	2.753 (5)	174 (5)
O7w—H72···O20^vii	0.85 (1)	2.09 (2)	2.906 (5)	163 (4)
O8w—H81···O18	0.85 (1)	1.87 (1)	2.713 (4)	170 (5)
O8w—H82···O2^v	0.85 (1)	2.12 (2)	2.943 (5)	163 (4)
O9w—H91···O9^vi	0.85 (1)	1.95 (1)	2.793 (4)	170 (4)
O9w—H92···O22w^viii	0.85 (1)	2.09 (2)	2.904 (5)	159 (4)
O10w—H101···O19^vii	0.85 (1)	2.00 (1)	2.838 (4)	171 (5)
O10w—H102···O17	0.85 (1)	2.40 (2)	3.233 (5)	169 (5)
O11w—H111···O19^vii	0.85 (1)	2.76 (7)	3.108 (6)	106 (5)
O11w—H112···O2ⁱⁱⁱ	0.85 (1)	2.13 (2)	2.940 (6)	160 (7)
O12w—H121···O25^vi	0.84 (1)	2.32 (1)	3.148 (5)	169 (4)
O12w—H122···O5^vi	0.84 (1)	1.97 (2)	2.783 (5)	161 (4)
O13w—H131···O25^vi	0.85 (1)	2.30 (2)	3.110 (5)	160 (4)
O13w—H132···O26^ix	0.85 (1)	2.22 (2)	2.994 (5)	151 (4)
O14w—H141···O19w^viii	0.85 (1)	2.19 (2)	2.985 (5)	156 (5)
O14w—H142···O8w	0.85 (1)	2.05 (1)	2.886 (6)	169 (5)
O15w—H151···O23^vii	0.85 (1)	1.99 (2)	2.801 (4)	160 (4)
O15w—H152···O21w	0.85 (1)	1.86 (1)	2.699 (5)	170 (4)
O16w—H161···O22	0.85 (1)	1.94 (2)	2.746 (4)	160 (5)
O16w—H162···O4w	0.85 (1)	2.21 (5)	2.789 (5)	126 (5)
O17w—H171···O5	0.85 (1)	1.99 (2)	2.823 (5)	165 (5)
O17w—H172···O22w	0.85 (1)	1.88 (1)	2.723 (5)	177 (5)
O18w—H181···O6^vii	0.84 (1)	1.94 (2)	2.723 (4)	155 (4)
O18w—H182···O12w^x	0.85 (1)	1.95 (2)	2.783 (5)	169 (5)
O19w—H191···O26	0.85 (1)	1.97 (1)	2.818 (4)	177 (5)
O19w—H192···O24^vii	0.85 (1)	1.81 (1)	2.653 (4)	171 (4)
O20w—H201···O12^vii	0.84 (1)	1.92 (1)	2.763 (4)	174 (5)
O20w—H202···O7	0.85 (1)	1.85 (1)	2.696 (4)	178 (5)
O21w—H211···O27	0.85 (1)	2.00 (2)	2.835 (5)	167 (5)
O21w—H212···O28^ix	0.85 (1)	1.90 (1)	2.744 (4)	176 (5)
O22w—H221···O10^vii	0.85 (1)	1.99 (2)	2.794 (5)	160 (5)
O22w—H222···O8	0.85 (1)	2.13 (2)	2.938 (4)	161 (4)

Symmetry codes: (iii) −x+1, −y+1, −z; (v) −x+2, −y+1, −z; (vi) x−1, y−1, z; (vii) x−1, y, z; (viii) x, y−1, z; (ix) −x+1, −y+1, −z+1; (x) x, y+1, z.

Experimental details

Crystal data
Chemical formula	Na₄Ni(V₁₀O₂₈)·23H₂O
M_r	1522.44
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	8.925 (2), 13.862 (3), 18.341 (4)
α, β, γ (°)	91.81 (3), 91.85 (3), 104.32 (3)
V (Å³)	2195.5 (8)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.62
Crystal size (mm)	0.50 × 0.25 × 0.11

Data collection
Diffractometer	Enraf-Nonius CAD-4 diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.245, 0.290
No. of measured, independent and observed [I > 2σ(I)] reflections	9182, 8594, 6270
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.100, 1.02
No. of reflections	8594
No. of parameters	748
No. of restraints	71
H-atom treatment	Only H-atom coordinates refined
Δρ_max, Δρ_min (e Å⁻³)	0.53, −0.56

Computer programs: CAD-4 Software (Enraf-Nonius, 1988), CAD-4 Software, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

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Tetradeca­aqua­tetrasodium hexa­aqua­nickel(II) decavanadate(V) trihydrate

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Tetradecaaquatetrasodium hexaaquanickel(II) decavanadate(V) trihydrate