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Acta Crystallogr Sect E Struct Rep Online. 2010 March 1; 66(Pt 3): i20–i21.
Published online 2010 February 20. doi:  10.1107/S160053681000601X
PMCID: PMC2983582

Penta­ammonium hepta­sodium bis­[penta­kis(μ2-oxido)deca­oxido­bis­(μ5-phosphato)penta­molybdenum(VI)] henicosa­hydrate

Abstract

The title compound, (NH4)5Na7[Mo5P2O23]2·21H2O, was prepared under atmospheric conditions in aqueous solution at room temperature. The structure contains the [Mo5P2O23]6− heteropolyoxometallate anion, which has been previously reported a number of times with a variety of differing counter-cations. Each anion is built up of five MoO6 octa­hedra sharing an edge and forming a ring which is closed by common corners of the terminal octa­hedra. The rings are closed on both sides by two asymmetric PO4 tetra­hedra, sharing three corners with three MoO6 octa­hedra. The anions are chiral and the two independent anions in the asymmetric unit were arbitarily chosen with the same chirality, but the centrosymmetric crystal contains both enanti­omers. The structure can alternatively be described as a succession of layers parallel to (101), formed by the [Mo5P2O23]6− anions and linked by sodium chains. Water mol­ecules and ammonium ions fill the remaining space and ensure the cohesion through extensive N—H(...)O and O—H(...)O hydrogen bonding.

Related literature

For ammonium polyoxomolybophosphates, see: Boeyens et al. (1976 [triangle]); Ferrari & Nanni (1939 [triangle]); Ilhan et al. (2007 [triangle]); Andersen & Villadsen (1993 [triangle]); Xu et al.(1998 [triangle]). For background to the heteropolyoxometallate anion, see: Hedman & Strandberg (1979 [triangle]); Long et al. (2007 [triangle]); Pope (1983 [triangle]); Strandberg (1973 [triangle]). For examples of hybrid compounds see: Ma et al. (2006 [triangle]); Wu et al. (2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-00i20-scheme1.jpg

Experimental

Crystal data

  • (NH4)5Na7[Mo5P2O23]2·21H2O
  • M r = 2448.76
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-00i20-efi1.jpg
  • a = 9.2299 (3) Å
  • b = 18.3516 (6) Å
  • c = 19.7918 (6) Å
  • α = 73.860 (1)°
  • β = 85.323 (3)°
  • γ = 75.772 (2)°
  • V = 3121.17 (17) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.23 mm−1
  • T = 298 K
  • 0.42 × 0.14 × 0.08 mm

Data collection

  • Bruker X8 APEXII Diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2005 [triangle]) T min = 0.695, T max = 0.837
  • 132450 measured reflections
  • 33626 independent reflections
  • 28095 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.022
  • wR(F 2) = 0.057
  • S = 1.09
  • 33626 reflections
  • 839 parameters
  • H-atom parameters constrained
  • Δρmax = 0.99 e Å−3
  • Δρmin = −0.76 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT (Bruker, 2005 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 [triangle]) and PLATON (Spek, 2009 [triangle]); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S160053681000601X/fj2276sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681000601X/fj2276Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for making the present work possible. They also thank H. Zouihri for his helpful technical assistance during the X-ray measurements. The authors are also grateful to the Swedish Research Council and the Swedish Inter­national Development Co-operation Agency (Sida) for the financial grant (MENA) offered in support of this work.

supplementary crystallographic information

Comment

Among the numerous molybdenum phosphates that are actually known, those containing ammonium cations are of particular interest, since they are susceptible to being used as matrices to generate new phases in the Mo–P–O system without foreign cations, by extracting the ammonium ion using soft chemistry methods or electrochemistry. The number of ammonium polyoxomolybophosphates that are actually known is quite limited and some of them are cited here:(NH4)3[Mo12PO40].3(H2O) (Ferrari and Nanni, 1939), (NH4)1.8K1.2[Mo12PO40] (Boeyens et al.,1976), (NH4)3[Mo12PO40].21(H2O) (Xu et al.,1998), (NH4)3[Mo12PO40].x(H2O) (Ilhan et al. 2007) and (NH4)8Ni(HPO4)2[Mo10P2O38].12(H2O), (Andersen and Villadsen, 1993). We have thus revisited the system NH4–Na–P–Mo—O using slow evaporation synthesis. We have obtained a new mixed NH4—Na molybdenum (VI) phosphate hydrate corresponding to the chemical formula (NH4)5Na7[Mo5P2O23]2.21(H2O). Here we report on its structure.

A three-dimensional view of the structure is represented in Fig. 1. It shows that the structure is formed by almost regular PO4 tetrahedra linked to distorted oxygen octahedra around the Movi+ ions. The unit cell contains 4 [Mo5P2O23]6- anions. Each anion is built up of five MoO6 octahedra sharing an edge and forming a ring which is closed by common corners of the terminal octahedra. The rings are closed on both sides by two asymmetric PO4 tetrahedra sharing three corners with three MoO6 octhedra as shown in Fig.2. Thus there are 2 independent anions with the same chirality in the asymmetric unit as shown in Fig. 2. In the crystal, the two enantiomers coexist.

The projection of the structure of the title compound along b direction (Fig.3), showing the layered arrangement of the [Mo5P2O23]6- anions parallel to the plane (1 0 1). The layers are connected by two small chains of five octahedra of oxygen, more or less distorted, surrounding the sodium atoms. Besides, all sodium has an octahedral coordination number except Na6 who is in a bipyramid with a pentagonal basis. Each of the two chains is formed by 4 octahedra linked in pairs by an edge, while the fifth shares two vertices with the last two as shown in Fig. 4. It also shows that the second chain ends with a bipyramid-NaO7. Water molecules and Ammonium ions fill the remaining space and ensure the cohesion of the whole through the ionic and hydrogen bonds.

Heteropolyoxometallates are polyanions of general chemical formula [XnMpOq]z-. Their structures are characterized and distinguished by the form of their anionic blocks. Among them, the structures with the Keggin anions [PMo12O40]3- (12 MoO6 octahedra surrounding PO4 tetrahedron) are the most extensively investigated (Pope, 1983), followed by structures with heteropolyoxoanion [P2 Mo5O23]6- called Strandberg structure (Strandberg, 1973; Hedman and Strandberg, 1979; Long et al. 2007). All these structures are built up by porous layers able to receive different organic ligands thus forming hybrid compounds (Ma et al. 2006; Wu et al.2009).

Experimental

Colourless crystals of (NH4)5Na7[Mo5P2O23]2.21(H2O) were easily grown by slow evaporation at room temperature from aqueous solution of disodium molybdate dihydrate (Na2MoO4.2H2O) and ammonium phosphate (NH4H2PO4) with 1:1 molar ratio. The product was filtered off and washed with a mixture of ethanol/water (80/20).

Refinement

All O-bound and N-bound H atoms were initially located in a difference map and refined with a O–H and N–H distance restraint of 0.84 (1) Å and 0.89 (1) Å respctively. An additional H···H restraint of 1.37 (2) Å and 1.44 (2) Åfor the water molecules and the ammonium respectively. Later they were refined in the ridingmodel with Uiso(H) set to 1.2 Ueq(O) or (N). The not significants bonds and angles were removed from the CIF file.

Figures

Fig. 1.
Polyhedral representation of the crystal packing of (NH4)5Na7[Mo5P2O23]2.21(H2O), viewed along the a direction.
Fig. 2.
: Plot of the asymmetric unit of the title compound, showing the two independent [Mo5P2O23]6- anions with the same chirality and atom labeling scheme. Displacement ellipsoids are drawn at the 50% probability level.
Fig. 3.
Projection of the structure of the title compound along the b axis, showing the layered arrangement of the structure parallel to the (101) plane.
Fig. 4.
Interconnections of sodium octahedra in the crystal structure. Symetrie codes:i(x, -1+y, 1+z); ii(1-x,1-y, 1-z); iii(1+x, 1+y, z) iv(1-x, 2-y, 1-z); v(2-x, 1-y, 1-z)

Crystal data

(NH4)5Na7[Mo5P2O23]2·21H2OZ = 2
Mr = 2448.76F(000) = 2380
Triclinic, P1Dx = 2.606 Mg m3
Hall symbol: -p 1Mo Kα radiation, λ = 0.71073 Å
a = 9.2299 (3) ÅCell parameters from 33624 reflections
b = 18.3516 (6) Åθ = 1.4–38.0°
c = 19.7918 (6) ŵ = 2.23 mm1
α = 73.860 (1)°T = 298 K
β = 85.323 (3)°Paralellipiped, colourless
γ = 75.772 (2)°0.42 × 0.14 × 0.08 mm
V = 3121.17 (17) Å3

Data collection

Bruker X8 APEXII Diffractometer33626 independent reflections
Radiation source: fine-focus sealed tube28095 reflections with I > 2σ(I)
graphiteRint = 0.024
[var phi] and ω scansθmax = 38.0°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −15→15
Tmin = 0.695, Tmax = 0.837k = −31→31
132450 measured reflectionsl = −34→34

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022H-atom parameters constrained
wR(F2) = 0.057w = 1/[σ2(Fo2) + (0.0181P)2 + 2.3233P] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.005
33626 reflectionsΔρmax = 0.99 e Å3
839 parametersΔρmin = −0.76 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00095 (3)

Special details

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.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

xyzUiso*/Ueq
Mo1A0.492310 (12)0.902494 (7)0.343660 (6)0.01467 (2)
Mo2A0.735113 (12)0.814966 (7)0.215956 (6)0.01368 (2)
Mo3A0.873090 (13)0.628793 (7)0.303128 (6)0.01678 (2)
Mo4A0.678462 (13)0.587156 (7)0.453493 (6)0.01620 (2)
Mo5A0.433389 (12)0.748439 (7)0.472935 (6)0.01530 (2)
P1A0.48960 (4)0.71885 (2)0.308740 (17)0.01286 (5)
P2A0.79211 (3)0.75969 (2)0.402960 (17)0.01274 (5)
O1A0.34812 (11)0.69257 (7)0.30366 (6)0.02106 (19)
O2A0.53301 (11)0.76604 (6)0.23641 (5)0.01649 (17)
O3A0.46154 (11)0.77456 (6)0.35793 (5)0.01569 (16)
O4A0.62074 (11)0.64826 (6)0.33780 (5)0.01611 (16)
O5A0.94463 (11)0.74016 (7)0.43521 (6)0.0215 (2)
O6A0.71593 (11)0.84625 (6)0.39166 (5)0.01732 (17)
O7A0.68843 (11)0.71080 (6)0.45080 (5)0.01592 (16)
O8A0.80787 (11)0.74280 (6)0.32905 (5)0.01586 (16)
O9A0.31315 (12)0.93039 (7)0.31154 (6)0.0243 (2)
O10A0.67181 (12)0.85621 (7)0.13130 (5)0.02108 (19)
O11A0.84747 (16)0.55099 (7)0.27801 (7)0.0302 (3)
O12A0.64223 (15)0.50469 (7)0.44157 (7)0.0278 (2)
O13A0.24416 (13)0.75961 (8)0.47347 (7)0.0309 (3)
O14A0.52178 (14)0.98849 (7)0.35016 (7)0.0258 (2)
O15A0.89771 (12)0.84629 (7)0.21162 (6)0.02135 (19)
O16A1.06197 (13)0.62069 (9)0.29542 (7)0.0341 (3)
O17A0.74864 (14)0.55493 (7)0.53758 (6)0.0265 (2)
O18A0.47398 (15)0.73386 (8)0.55946 (6)0.0274 (2)
O19A0.60715 (11)0.88732 (6)0.26208 (5)0.01796 (17)
O20A0.81587 (12)0.70838 (6)0.21550 (5)0.01797 (17)
O21A0.86607 (11)0.58826 (6)0.40407 (5)0.01919 (18)
O22A0.47846 (11)0.64131 (6)0.46786 (6)0.01934 (18)
O23A0.44199 (12)0.85665 (6)0.44104 (5)0.01914 (18)
Mo1B0.215242 (12)0.815178 (6)0.718288 (5)0.01292 (2)
Mo2B−0.025676 (12)0.907008 (6)0.843473 (6)0.01376 (2)
Mo3B−0.081624 (12)0.756868 (7)0.978050 (6)0.01538 (2)
Mo4B0.167731 (12)0.593177 (7)0.963923 (6)0.01502 (2)
Mo5B0.362696 (11)0.634503 (7)0.813014 (6)0.01370 (2)
P1B0.27703 (3)0.76807 (2)0.906219 (17)0.01229 (5)
P2B−0.02535 (3)0.719500 (19)0.817922 (17)0.01141 (5)
O1B0.42849 (11)0.75117 (7)0.93786 (6)0.02107 (19)
O2B0.19706 (11)0.85435 (6)0.89184 (5)0.01634 (16)
O3B0.28897 (11)0.74801 (6)0.83384 (5)0.01464 (16)
O4B0.17722 (11)0.71920 (6)0.95805 (5)0.01549 (16)
O5B−0.16688 (11)0.69176 (6)0.81884 (5)0.01820 (18)
O6B0.01321 (10)0.76426 (6)0.74363 (5)0.01486 (16)
O7B0.10810 (10)0.64902 (6)0.84613 (5)0.01464 (15)
O8B−0.04676 (10)0.77750 (6)0.86459 (5)0.01455 (15)
O9B0.37818 (12)0.84669 (7)0.71131 (6)0.02057 (19)
O10B0.00007 (13)0.99519 (6)0.84546 (6)0.0247 (2)
O11B−0.03688 (16)0.74633 (8)1.06283 (6)0.0306 (3)
O12B0.23471 (14)0.56392 (8)1.04855 (6)0.0270 (2)
O13B0.54923 (12)0.63231 (7)0.80612 (6)0.0250 (2)
O14B0.15290 (12)0.85003 (7)0.63305 (5)0.02072 (19)
O15B−0.20435 (12)0.93135 (7)0.81118 (6)0.0230 (2)
O16B−0.27055 (13)0.76566 (8)0.98036 (7)0.0306 (3)
O17B0.13950 (14)0.50961 (7)0.95064 (6)0.0253 (2)
O18B0.34637 (12)0.55192 (6)0.79159 (6)0.0218 (2)
O19B0.08888 (11)0.88917 (6)0.76195 (5)0.01694 (17)
O20B−0.07788 (12)0.86570 (6)0.94177 (5)0.01857 (18)
O21B−0.03213 (11)0.64729 (6)0.97706 (5)0.01781 (17)
O22B0.35501 (11)0.59687 (6)0.91380 (5)0.01754 (17)
O23B0.29709 (11)0.70706 (6)0.72405 (5)0.01634 (16)
Na10.09393 (8)0.88130 (4)0.12276 (4)0.02741 (13)
Na20.44879 (8)0.90873 (5)0.05715 (4)0.03205 (15)
Na30.32566 (11)0.69247 (6)0.06676 (5)0.0475 (2)
Na40.06704 (8)1.08630 (5)0.44343 (4)0.03092 (15)
Na50.42461 (8)0.11186 (4)0.37681 (4)0.02557 (13)
Na60.89731 (8)0.47633 (4)0.19135 (4)0.02833 (14)
Na70.23473 (7)0.36371 (4)0.26312 (4)0.02572 (13)
O10.13802 (15)0.50097 (8)0.18793 (7)0.0349 (3)
H110.18830.51750.15070.042*
H120.13800.53190.21350.042*
O20.80373 (18)0.61051 (8)0.12368 (7)0.0367 (3)
H210.85520.62190.08560.044*
H220.80290.64640.14400.044*
O30.62913 (13)0.07746 (7)0.45018 (6)0.0247 (2)
H310.60220.10080.48290.030*
H320.70620.09370.43060.030*
O40.07634 (18)0.95082 (9)0.44777 (8)0.0388 (3)
H410.02260.94830.41540.047*
H420.16130.91970.44410.047*
O50.30931 (14)0.89540 (8)0.17057 (7)0.0305 (3)
H510.29350.93240.19100.037*
H520.37270.85770.19670.037*
O60.88411 (14)0.93215 (7)0.04955 (6)0.0255 (2)
H610.80360.92040.06960.031*
H620.90070.91060.01540.031*
O70.29608 (14)1.08048 (8)0.49264 (6)0.0285 (2)
H710.32991.03220.51400.034*
H720.29471.10520.52380.034*
O80.77938 (14)1.08752 (8)−0.00967 (6)0.0284 (2)
H810.81931.03900.00840.034*
H820.77831.10940.02370.034*
O90.02918 (15)1.22207 (8)0.44210 (7)0.0340 (3)
H910.03781.22860.48280.041*
H92−0.06551.23100.43620.041*
O100.89823 (18)0.95851 (9)0.34047 (9)0.0431 (3)
H1010.87091.00150.30830.052*
H1020.82170.93830.34800.052*
O110.97177 (19)0.40736 (11)0.43052 (9)0.0483 (4)
H1111.04920.37420.45080.058*
H1120.97980.45150.43480.058*
O120.29779 (15)0.24836 (8)0.36313 (7)0.0340 (3)
H1210.22040.24340.38970.041*
H1220.35320.26460.38590.041*
O130.60970 (18)0.03813 (9)0.15981 (9)0.0421 (3)
H1310.6343−0.00590.19090.051*
H1320.69070.05440.15040.051*
O140.97224 (15)0.37508 (8)0.30176 (7)0.0306 (3)
H1410.97330.37980.34370.037*
H1420.95750.32930.30720.037*
O150.20367 (14)1.10295 (8)0.32985 (7)0.0295 (2)
H1510.14551.14230.30270.035*
H1520.22191.06720.30790.035*
O160.57481 (17)0.95301 (9)−0.05286 (8)0.0368 (3)
H1610.51890.9503−0.08440.044*
H1620.66040.9235−0.05860.044*
O170.49009 (18)0.76434 (10)0.08862 (9)0.0459 (4)
H1710.43430.77400.05300.055*
H1720.57990.75840.07190.055*
O180.18027 (19)0.73673 (10)0.16301 (10)0.0514 (4)
H1810.23140.70560.19840.062*
H1820.10040.72010.16440.062*
O190.5309 (2)0.58788 (10)0.08724 (11)0.0571 (5)
H1910.47060.59350.12190.069*
H1920.61720.58640.10180.069*
O200.3219 (2)0.43251 (11)0.32741 (9)0.0601 (5)
H2010.33170.47830.30450.072*
H2020.28040.43800.36680.072*
O210.3970 (3)0.56485 (13)0.24794 (15)0.0976 (10)
H2110.37340.60740.26080.117*
H2120.48840.54450.26040.117*
N10.6411 (2)0.40411 (12)0.36141 (10)0.0471 (5)
H11N0.65340.41010.40230.057*
H12N0.54950.40160.35790.057*
H13N0.66000.44340.32880.057*
H14N0.70130.36140.35660.057*
N20.11305 (15)0.81900 (9)0.32080 (8)0.0282 (3)
H21N0.07880.80360.36310.034*
H22N0.15150.85850.31770.034*
H23N0.18120.78120.31120.034*
H24N0.04080.83270.29120.034*
N30.40355 (15)0.17946 (9)0.17830 (8)0.0272 (3)
H31N0.33250.21780.18470.033*
H32N0.47350.16940.20850.033*
H33N0.44000.19210.13600.033*
H34N0.36820.13850.18390.033*
N40.20062 (16)0.61691 (8)0.42575 (8)0.0266 (3)
H41N0.24120.63700.38610.032*
H42N0.12030.64980.43350.032*
H43N0.26310.60640.45950.032*
H44N0.17790.57440.42400.032*
N50.32188 (16)0.37776 (8)0.06106 (7)0.0258 (3)
H51N0.39370.34130.05170.031*
H52N0.27470.35840.09890.031*
H53N0.35870.41450.06740.031*
H54N0.26030.39680.02630.031*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo1A0.01617 (4)0.01225 (5)0.01538 (5)−0.00185 (3)0.00054 (3)−0.00482 (4)
Mo2A0.01413 (4)0.01481 (5)0.01165 (4)−0.00409 (3)0.00129 (3)−0.00259 (3)
Mo3A0.01754 (5)0.01578 (5)0.01542 (5)−0.00018 (4)0.00213 (3)−0.00550 (4)
Mo4A0.02082 (5)0.01240 (5)0.01418 (5)−0.00345 (4)0.00126 (4)−0.00243 (4)
Mo5A0.01518 (4)0.01755 (5)0.01396 (4)−0.00465 (4)0.00283 (3)−0.00563 (4)
P1A0.01306 (12)0.01411 (14)0.01280 (13)−0.00474 (10)0.00051 (10)−0.00464 (11)
P2A0.01218 (12)0.01468 (14)0.01270 (13)−0.00422 (10)0.00020 (9)−0.00498 (11)
O1A0.0167 (4)0.0261 (5)0.0247 (5)−0.0107 (4)0.0004 (3)−0.0089 (4)
O2A0.0171 (4)0.0202 (5)0.0126 (4)−0.0065 (3)−0.0001 (3)−0.0033 (3)
O3A0.0193 (4)0.0145 (4)0.0138 (4)−0.0031 (3)0.0007 (3)−0.0056 (3)
O4A0.0179 (4)0.0138 (4)0.0162 (4)−0.0022 (3)−0.0004 (3)−0.0044 (3)
O5A0.0142 (4)0.0290 (6)0.0231 (5)−0.0043 (4)−0.0033 (3)−0.0095 (4)
O6A0.0192 (4)0.0148 (4)0.0200 (4)−0.0051 (3)−0.0006 (3)−0.0069 (4)
O7A0.0166 (4)0.0164 (4)0.0155 (4)−0.0057 (3)0.0021 (3)−0.0044 (3)
O8A0.0194 (4)0.0160 (4)0.0125 (4)−0.0046 (3)0.0015 (3)−0.0043 (3)
O9A0.0199 (5)0.0229 (5)0.0268 (5)−0.0003 (4)−0.0035 (4)−0.0046 (4)
O10A0.0214 (4)0.0247 (5)0.0150 (4)−0.0054 (4)−0.0010 (3)−0.0018 (4)
O11A0.0471 (7)0.0181 (5)0.0256 (6)−0.0024 (5)0.0010 (5)−0.0110 (4)
O12A0.0383 (6)0.0181 (5)0.0293 (6)−0.0105 (5)0.0022 (5)−0.0070 (4)
O13A0.0174 (5)0.0394 (7)0.0396 (7)−0.0084 (5)0.0059 (4)−0.0166 (6)
O14A0.0314 (6)0.0168 (5)0.0315 (6)−0.0056 (4)−0.0001 (4)−0.0104 (4)
O15A0.0196 (4)0.0250 (5)0.0198 (5)−0.0102 (4)0.0009 (3)−0.0025 (4)
O16A0.0188 (5)0.0474 (8)0.0289 (6)−0.0007 (5)0.0024 (4)−0.0053 (6)
O17A0.0339 (6)0.0248 (6)0.0170 (5)−0.0046 (5)−0.0014 (4)−0.0011 (4)
O18A0.0361 (6)0.0311 (6)0.0155 (5)−0.0091 (5)0.0012 (4)−0.0064 (4)
O19A0.0217 (4)0.0148 (4)0.0157 (4)−0.0028 (3)0.0030 (3)−0.0037 (3)
O20A0.0232 (4)0.0171 (4)0.0133 (4)−0.0023 (3)0.0016 (3)−0.0062 (3)
O21A0.0185 (4)0.0187 (5)0.0167 (4)0.0002 (3)0.0003 (3)−0.0028 (4)
O22A0.0199 (4)0.0170 (4)0.0222 (5)−0.0076 (3)0.0038 (3)−0.0051 (4)
O23A0.0268 (5)0.0158 (4)0.0156 (4)−0.0046 (4)0.0033 (3)−0.0067 (3)
Mo1B0.01374 (4)0.01404 (5)0.01068 (4)−0.00449 (3)0.00104 (3)−0.00208 (3)
Mo2B0.01503 (4)0.01176 (4)0.01424 (4)−0.00222 (3)0.00020 (3)−0.00397 (4)
Mo3B0.01626 (4)0.01601 (5)0.01367 (4)−0.00422 (4)0.00364 (3)−0.00431 (4)
Mo4B0.01617 (4)0.01305 (5)0.01367 (4)−0.00304 (3)0.00121 (3)−0.00079 (4)
Mo5B0.01213 (4)0.01431 (5)0.01421 (4)−0.00206 (3)0.00130 (3)−0.00441 (4)
P1B0.01225 (12)0.01427 (14)0.01123 (12)−0.00434 (10)−0.00025 (9)−0.00368 (10)
P2B0.01083 (11)0.01214 (13)0.01187 (12)−0.00324 (9)−0.00013 (9)−0.00371 (10)
O1B0.0157 (4)0.0263 (5)0.0218 (5)−0.0053 (4)−0.0049 (3)−0.0058 (4)
O2B0.0184 (4)0.0146 (4)0.0176 (4)−0.0045 (3)−0.0015 (3)−0.0058 (3)
O3B0.0181 (4)0.0143 (4)0.0118 (4)−0.0043 (3)0.0009 (3)−0.0037 (3)
O4B0.0166 (4)0.0171 (4)0.0128 (4)−0.0063 (3)0.0018 (3)−0.0025 (3)
O5B0.0145 (4)0.0231 (5)0.0200 (4)−0.0089 (3)0.0009 (3)−0.0069 (4)
O6B0.0154 (4)0.0169 (4)0.0120 (4)−0.0049 (3)−0.0003 (3)−0.0025 (3)
O7B0.0144 (4)0.0127 (4)0.0153 (4)−0.0011 (3)−0.0011 (3)−0.0027 (3)
O8B0.0174 (4)0.0133 (4)0.0135 (4)−0.0031 (3)0.0007 (3)−0.0051 (3)
O9B0.0189 (4)0.0243 (5)0.0195 (4)−0.0103 (4)0.0012 (3)−0.0032 (4)
O10B0.0299 (5)0.0158 (5)0.0304 (6)−0.0066 (4)−0.0001 (4)−0.0085 (4)
O11B0.0443 (7)0.0324 (7)0.0157 (5)−0.0103 (5)0.0027 (5)−0.0068 (5)
O12B0.0278 (5)0.0321 (6)0.0162 (5)−0.0062 (5)−0.0015 (4)0.0013 (4)
O13B0.0148 (4)0.0357 (6)0.0240 (5)−0.0054 (4)0.0019 (4)−0.0083 (5)
O14B0.0220 (4)0.0257 (5)0.0133 (4)−0.0069 (4)−0.0010 (3)−0.0019 (4)
O15B0.0175 (4)0.0224 (5)0.0260 (5)−0.0014 (4)−0.0036 (4)−0.0036 (4)
O16B0.0188 (5)0.0315 (6)0.0421 (7)−0.0072 (4)0.0080 (4)−0.0120 (5)
O17B0.0292 (5)0.0160 (5)0.0300 (6)−0.0068 (4)0.0020 (4)−0.0043 (4)
O18B0.0248 (5)0.0169 (5)0.0245 (5)−0.0038 (4)0.0014 (4)−0.0082 (4)
O19B0.0202 (4)0.0146 (4)0.0146 (4)−0.0028 (3)0.0022 (3)−0.0035 (3)
O20B0.0258 (5)0.0164 (4)0.0146 (4)−0.0052 (4)0.0037 (3)−0.0069 (3)
O21B0.0171 (4)0.0158 (4)0.0201 (4)−0.0059 (3)0.0033 (3)−0.0034 (4)
O22B0.0146 (4)0.0198 (5)0.0145 (4)−0.0013 (3)−0.0003 (3)−0.0009 (3)
O23B0.0193 (4)0.0162 (4)0.0131 (4)−0.0026 (3)0.0011 (3)−0.0050 (3)
Na10.0274 (3)0.0300 (4)0.0237 (3)−0.0067 (3)−0.0013 (2)−0.0051 (3)
Na20.0297 (3)0.0363 (4)0.0286 (4)−0.0107 (3)−0.0032 (3)−0.0027 (3)
Na30.0512 (5)0.0525 (6)0.0403 (5)−0.0036 (4)−0.0161 (4)−0.0176 (4)
Na40.0302 (3)0.0353 (4)0.0289 (3)−0.0120 (3)−0.0027 (3)−0.0066 (3)
Na50.0250 (3)0.0253 (3)0.0259 (3)−0.0044 (2)−0.0026 (2)−0.0068 (3)
Na60.0271 (3)0.0251 (3)0.0338 (4)−0.0079 (3)−0.0004 (3)−0.0079 (3)
Na70.0231 (3)0.0333 (4)0.0241 (3)−0.0099 (3)0.0031 (2)−0.0111 (3)
O10.0336 (6)0.0361 (7)0.0334 (7)−0.0115 (5)0.0041 (5)−0.0048 (6)
O20.0540 (9)0.0301 (7)0.0288 (6)−0.0174 (6)−0.0055 (6)−0.0046 (5)
O30.0302 (5)0.0270 (6)0.0200 (5)−0.0103 (4)0.0042 (4)−0.0096 (4)
O40.0427 (8)0.0394 (8)0.0372 (7)−0.0099 (6)0.0035 (6)−0.0160 (6)
O50.0268 (5)0.0346 (7)0.0283 (6)0.0020 (5)−0.0084 (4)−0.0113 (5)
O60.0317 (6)0.0285 (6)0.0197 (5)−0.0104 (5)0.0033 (4)−0.0098 (4)
O70.0337 (6)0.0274 (6)0.0234 (5)−0.0048 (5)−0.0051 (4)−0.0059 (5)
O80.0343 (6)0.0306 (6)0.0218 (5)−0.0065 (5)−0.0026 (4)−0.0098 (5)
O90.0326 (6)0.0412 (8)0.0309 (6)−0.0082 (5)0.0030 (5)−0.0154 (6)
O100.0417 (8)0.0362 (8)0.0488 (9)−0.0151 (6)−0.0041 (7)−0.0008 (7)
O110.0477 (9)0.0604 (11)0.0420 (9)−0.0108 (8)−0.0022 (7)−0.0234 (8)
O120.0337 (6)0.0326 (7)0.0359 (7)−0.0098 (5)−0.0055 (5)−0.0062 (6)
O130.0420 (8)0.0310 (7)0.0495 (9)−0.0129 (6)−0.0028 (7)0.0000 (6)
O140.0402 (7)0.0270 (6)0.0267 (6)−0.0076 (5)−0.0010 (5)−0.0107 (5)
O150.0270 (5)0.0336 (7)0.0271 (6)0.0000 (5)−0.0088 (4)−0.0106 (5)
O160.0384 (7)0.0374 (8)0.0353 (7)−0.0068 (6)0.0061 (6)−0.0145 (6)
O170.0406 (8)0.0480 (9)0.0589 (10)−0.0150 (7)0.0098 (7)−0.0293 (8)
O180.0423 (9)0.0435 (9)0.0602 (11)−0.0053 (7)0.0079 (7)−0.0070 (8)
O190.0437 (9)0.0396 (9)0.0789 (13)−0.0083 (7)−0.0148 (9)0.0017 (9)
O200.0965 (15)0.0632 (12)0.0327 (8)−0.0292 (11)0.0098 (9)−0.0261 (8)
O210.1028 (19)0.0707 (15)0.151 (2)−0.0483 (14)0.0766 (17)−0.0777 (16)
N10.0635 (13)0.0582 (12)0.0340 (9)−0.0283 (10)0.0111 (8)−0.0266 (9)
N20.0218 (6)0.0331 (8)0.0285 (7)−0.0064 (5)−0.0009 (5)−0.0059 (6)
N30.0203 (5)0.0284 (7)0.0305 (7)−0.0042 (5)−0.0006 (5)−0.0052 (6)
N40.0305 (6)0.0221 (6)0.0258 (6)−0.0087 (5)−0.0044 (5)−0.0006 (5)
N50.0278 (6)0.0243 (6)0.0231 (6)−0.0074 (5)−0.0035 (5)−0.0005 (5)

Geometric parameters (Å, °)

Mo1A—O14A1.7062 (11)Na3—O192.311 (2)
Mo1A—O9A1.7248 (11)Na3—O172.3745 (18)
Mo1A—O19A1.9063 (10)Na3—O182.449 (2)
Mo1A—O23A1.9449 (10)Na3—O4Bix2.5122 (13)
Mo1A—O6A2.2261 (10)Na3—O1Bix2.6738 (15)
Mo1A—O3A2.3703 (10)Na3—O12Bix2.8100 (16)
Mo2A—O10A1.7200 (10)Na4—O72.3657 (15)
Mo2A—O15A1.7222 (10)Na4—O92.4224 (16)
Mo2A—O20A1.9166 (10)Na4—O42.4442 (17)
Mo2A—O19A1.9284 (10)Na4—O4vi2.4527 (17)
Mo2A—O2A2.2243 (9)Na4—O152.4661 (15)
Mo2A—O8A2.3184 (10)Na4—O14Bvi2.4757 (13)
Mo3A—O11A1.7092 (12)Na4—H922.6056
Mo3A—O16A1.7107 (12)Na5—O32.3286 (14)
Mo3A—O21A1.9300 (10)Na5—O15x2.3677 (14)
Mo3A—O20A1.9447 (10)Na5—O14Ax2.4075 (13)
Mo3A—O8A2.2204 (10)Na5—O122.4396 (16)
Mo3A—O4A2.3431 (10)Na5—O7x2.4805 (15)
Mo4A—O12A1.7083 (11)Na5—O9Bv2.5217 (12)
Mo4A—O17A1.7260 (12)Na6—O1ii2.3659 (15)
Mo4A—O22A1.9095 (11)Na6—O18Bv2.4069 (13)
Mo4A—O21A1.9198 (10)Na6—O22.4316 (16)
Mo4A—O7A2.2791 (10)Na6—O142.4624 (15)
Mo4A—O4A2.2939 (10)Na6—O7Bv2.6182 (12)
Mo5A—O13A1.7073 (11)Na6—O17Bv2.7909 (15)
Mo5A—O18A1.7161 (11)Na7—O202.3281 (18)
Mo5A—O23A1.9289 (10)Na7—O13Bv2.3302 (12)
Mo5A—O22A1.9362 (10)Na7—O5Biv2.3360 (12)
Mo5A—O3A2.1992 (9)Na7—O122.4476 (15)
Mo5A—O7A2.3262 (10)Na7—O14vii2.4568 (15)
P1A—O1A1.5185 (10)Na7—O12.5266 (16)
P1A—O2A1.5323 (10)O1—Na6vii2.3659 (15)
P1A—O4A1.5499 (10)O1—H110.8599
P1A—O3A1.5629 (10)O1—H120.8598
P2A—O5A1.5129 (10)O2—H210.8600
P2A—O6A1.5319 (11)O2—H220.8600
P2A—O7A1.5554 (10)O3—H310.8598
P2A—O8A1.5660 (10)O3—H320.8599
O10A—Na22.4599 (13)O4—Na4vi2.4527 (17)
O11A—Na62.4288 (14)O4—H410.8599
O14A—Na5i2.4075 (13)O4—H420.8600
O15A—Na1ii2.4920 (12)O5—H510.8599
Mo1B—O14B1.7214 (10)O5—H520.8599
Mo1B—O9B1.7217 (10)O6—Na1ii2.3534 (14)
Mo1B—O19B1.9132 (10)O6—H610.8600
Mo1B—O23B1.9162 (10)O6—H620.8599
Mo1B—O6B2.2462 (9)O7—Na5i2.4806 (15)
Mo1B—O3B2.3424 (9)O7—H710.8597
Mo2B—O10B1.7038 (11)O7—H720.8599
Mo2B—O15B1.7259 (11)O8—Na2viii2.3534 (15)
Mo2B—O19B1.9168 (10)O8—Na1viii2.4279 (14)
Mo2B—O20B1.9489 (10)O8—H810.8600
Mo2B—O2B2.2150 (10)O8—H820.8600
Mo2B—O8B2.3501 (10)O9—H910.8597
Mo3B—O11B1.7079 (12)O9—H920.8598
Mo3B—O16B1.7092 (12)O10—H1010.8598
Mo3B—O20B1.9335 (10)O10—H1020.8599
Mo3B—O21B1.9550 (10)O11—H1110.8598
Mo3B—O8B2.1815 (9)O11—H1120.8597
Mo3B—O4B2.3512 (10)O12—H1210.8598
Mo4B—O17B1.7090 (11)O12—H1220.8598
Mo4B—O12B1.7268 (11)O13—H1310.8599
Mo4B—O21B1.9030 (10)O13—H1320.8598
Mo4B—O22B1.9280 (10)O14—Na7ii2.4568 (15)
Mo4B—O4B2.3062 (10)O14—H1410.8598
Mo4B—O7B2.3221 (10)O14—H1420.8599
Mo5B—O13B1.7074 (10)O15—Na5i2.3677 (14)
Mo5B—O18B1.7261 (11)O15—H1510.8599
Mo5B—O22B1.9225 (10)O15—H1520.8599
Mo5B—O23B1.9272 (10)O16—Na2viii2.4707 (17)
Mo5B—O3B2.1696 (10)O16—H1610.8599
Mo5B—O7B2.3581 (9)O16—H1620.8598
P1B—O1B1.5047 (10)O17—H1710.8598
P1B—O2B1.5304 (10)O17—H1720.8600
P1B—O4B1.5639 (10)O18—H1810.8599
P1B—O3B1.5643 (10)O18—H1820.8599
P2B—O5B1.5113 (10)O19—H1910.8599
P2B—O6B1.5331 (10)O19—H1920.8600
P2B—O7B1.5586 (10)O20—H2010.8600
P2B—O8B1.5616 (10)O20—H2020.8600
O1B—Na3iii2.6738 (15)O21—H2110.8601
O4B—Na3iii2.5122 (13)O21—H2120.8601
O5B—Na7iv2.3360 (12)N1—H11N0.8669
O7B—Na6v2.6182 (12)N1—H12N0.8668
O9B—Na5v2.5217 (12)N1—H13N0.8669
O10B—Na1vi2.4541 (13)N1—H14N0.8668
O12B—Na3iii2.8100 (16)N2—H21N0.8667
O13B—Na7v2.3302 (12)N2—H22N0.8669
O14B—Na4vi2.4758 (13)N2—H23N0.8668
O17B—Na6v2.7909 (15)N2—H24N0.8669
O18B—Na6v2.4069 (13)N3—H31N0.8670
Na1—O6vii2.3534 (14)N3—H32N0.8670
Na1—O52.3686 (14)N3—H33N0.8668
Na1—O8viii2.4279 (14)N3—H34N0.8667
Na1—O10Bvi2.4541 (13)N4—H41N0.8666
Na1—O182.4895 (19)N4—H42N0.8669
Na1—O15Avii2.4920 (12)N4—H43N0.8669
Na2—O8viii2.3533 (15)N4—H44N0.8670
Na2—O162.4129 (16)N5—H51N0.8667
Na2—O16viii2.4707 (17)N5—H52N0.8672
Na2—O52.4768 (15)N5—H53N0.8669
Na2—O172.4858 (18)N5—H54N0.8666
O14A—Mo1A—O9A102.22 (6)O8viii—Na1—O15Avii159.95 (5)
O14A—Mo1A—O19A102.60 (5)O10Bvi—Na1—O15Avii79.37 (4)
O9A—Mo1A—O19A101.23 (5)O18—Na1—O15Avii78.15 (5)
O14A—Mo1A—O23A100.23 (5)O8viii—Na2—O1697.26 (6)
O9A—Mo1A—O23A97.14 (5)O8viii—Na2—O10A158.25 (6)
O19A—Mo1A—O23A146.77 (4)O16—Na2—O10A97.36 (5)
O14A—Mo1A—O6A86.85 (5)O8viii—Na2—O16viii102.28 (6)
O9A—Mo1A—O6A170.21 (5)O16—Na2—O16viii78.87 (5)
O19A—Mo1A—O6A80.08 (4)O10A—Na2—O16viii96.29 (5)
O23A—Mo1A—O6A77.39 (4)O8viii—Na2—O584.99 (5)
O14A—Mo1A—O3A169.02 (5)O16—Na2—O5166.63 (6)
O9A—Mo1A—O3A83.84 (5)O10A—Na2—O584.51 (4)
O19A—Mo1A—O3A84.95 (4)O16viii—Na2—O587.78 (5)
O23A—Mo1A—O3A69.70 (4)O8viii—Na2—O1786.32 (6)
O6A—Mo1A—O3A86.62 (3)O16—Na2—O17109.59 (6)
O10A—Mo2A—O15A101.45 (5)O10A—Na2—O1773.63 (5)
O10A—Mo2A—O20A101.79 (5)O16viii—Na2—O17167.31 (6)
O15A—Mo2A—O20A100.16 (5)O5—Na2—O1783.66 (5)
O10A—Mo2A—O19A99.60 (5)O19—Na3—O1785.28 (7)
O15A—Mo2A—O19A99.19 (5)O19—Na3—O18121.92 (8)
O20A—Mo2A—O19A147.53 (4)O17—Na3—O1882.98 (6)
O10A—Mo2A—O2A86.21 (4)O19—Na3—O4Bix117.80 (7)
O15A—Mo2A—O2A172.34 (4)O17—Na3—O4Bix127.96 (7)
O20A—Mo2A—O2A77.78 (4)O18—Na3—O4Bix113.98 (6)
O19A—Mo2A—O2A79.58 (4)O19—Na3—O1Bix91.20 (7)
O10A—Mo2A—O8A171.17 (5)O17—Na3—O1Bix77.46 (6)
O15A—Mo2A—O8A85.41 (4)O18—Na3—O1Bix139.83 (6)
O20A—Mo2A—O8A71.26 (4)O4Bix—Na3—O1Bix57.64 (4)
O19A—Mo2A—O8A84.61 (4)O19—Na3—O12Bix72.69 (6)
O2A—Mo2A—O8A86.94 (3)O17—Na3—O12Bix157.94 (6)
O11A—Mo3A—O16A104.13 (7)O18—Na3—O12Bix109.41 (6)
O11A—Mo3A—O21A100.05 (5)O4Bix—Na3—O12Bix64.75 (4)
O16A—Mo3A—O21A96.78 (5)O1Bix—Na3—O12Bix101.35 (4)
O11A—Mo3A—O20A97.90 (5)O19—Na3—P1Bix111.15 (6)
O16A—Mo3A—O20A97.92 (6)O17—Na3—P1Bix99.82 (6)
O21A—Mo3A—O20A153.22 (4)O18—Na3—P1Bix126.87 (6)
O11A—Mo3A—O8A156.81 (5)O4Bix—Na3—P1Bix29.91 (2)
O16A—Mo3A—O8A98.32 (6)O1Bix—Na3—P1Bix28.87 (2)
O21A—Mo3A—O8A82.77 (4)O12Bix—Na3—P1Bix87.39 (3)
O20A—Mo3A—O8A73.05 (4)O19—Na3—Mo4Bix88.18 (6)
O11A—Mo3A—O4A86.34 (5)O17—Na3—Mo4Bix155.44 (6)
O16A—Mo3A—O4A166.47 (5)O18—Na3—Mo4Bix120.22 (6)
O21A—Mo3A—O4A72.64 (4)O4Bix—Na3—Mo4Bix38.41 (3)
O20A—Mo3A—O4A88.92 (4)O1Bix—Na3—Mo4Bix79.04 (3)
O8A—Mo3A—O4A72.44 (3)O12Bix—Na3—Mo4Bix27.02 (2)
O12A—Mo4A—O17A102.25 (6)P1Bix—Na3—Mo4Bix60.775 (16)
O12A—Mo4A—O22A98.92 (5)O19—Na3—Na1146.98 (6)
O17A—Mo4A—O22A102.37 (5)O17—Na3—Na169.69 (5)
O12A—Mo4A—O21A100.92 (5)O18—Na3—Na136.46 (4)
O17A—Mo4A—O21A97.16 (5)O4Bix—Na3—Na194.86 (4)
O22A—Mo4A—O21A148.39 (4)O1Bix—Na3—Na1103.43 (4)
O12A—Mo4A—O7A167.40 (5)O12Bix—Na3—Na1130.91 (4)
O17A—Mo4A—O7A89.35 (5)O19—Na3—H17197.1
O22A—Mo4A—O7A73.47 (4)O17—Na3—H17120.0
O21A—Mo4A—O7A82.23 (4)O18—Na3—H17190.3
O12A—Mo4A—O4A88.68 (5)O4Bix—Na3—H171108.0
O17A—Mo4A—O4A167.20 (5)O1Bix—Na3—H17161.2
O22A—Mo4A—O4A82.18 (4)O12Bix—Na3—H171160.3
O21A—Mo4A—O4A73.97 (4)O19—Na3—H19121.7
O7A—Mo4A—O4A80.42 (3)O17—Na3—H19187.4
O13A—Mo5A—O18A103.91 (6)O18—Na3—H191100.9
O13A—Mo5A—O23A99.20 (6)O4Bix—Na3—H191131.5
O18A—Mo5A—O23A97.31 (5)O1Bix—Na3—H191112.7
O13A—Mo5A—O22A94.56 (5)O12Bix—Na3—H19172.6
O18A—Mo5A—O22A99.91 (5)H171—Na3—H191104.2
O23A—Mo5A—O22A154.66 (4)O7—Na4—O980.79 (5)
O13A—Mo5A—O3A95.75 (5)O7—Na4—O4104.19 (6)
O18A—Mo5A—O3A159.60 (5)O9—Na4—O4173.79 (6)
O23A—Mo5A—O3A73.89 (4)O7—Na4—O4vi99.21 (6)
O22A—Mo5A—O3A83.68 (4)O9—Na4—O4vi95.84 (5)
O13A—Mo5A—O7A163.36 (5)O4—Na4—O4vi79.81 (6)
O18A—Mo5A—O7A88.32 (5)O7—Na4—O1585.76 (5)
O23A—Mo5A—O7A90.22 (4)O9—Na4—O1593.57 (5)
O22A—Mo5A—O7A71.92 (4)O4—Na4—O1590.52 (5)
O3A—Mo5A—O7A73.61 (4)O4vi—Na4—O15169.95 (6)
O1A—P1A—O2A110.26 (6)O7—Na4—O14Bvi154.61 (5)
O1A—P1A—O4A111.26 (6)O9—Na4—O14Bvi77.41 (5)
O2A—P1A—O4A109.65 (6)O4—Na4—O14Bvi98.51 (5)
O1A—P1A—O3A109.98 (6)O4vi—Na4—O14Bvi95.83 (5)
O2A—P1A—O3A106.42 (6)O15—Na4—O14Bvi82.78 (4)
O4A—P1A—O3A109.15 (6)O7—Na4—H9299.3
O5A—P2A—O6A111.48 (6)O9—Na4—H9219.2
O5A—P2A—O7A110.97 (6)O4—Na4—H92154.8
O6A—P2A—O7A108.23 (6)O4vi—Na4—H9287.6
O5A—P2A—O8A109.93 (6)O15—Na4—H92100.2
O6A—P2A—O8A107.03 (6)O14Bvi—Na4—H9260.9
O7A—P2A—O8A109.09 (5)Na5i—Na4—H9299.3
O14B—Mo1B—O9B101.76 (5)Na4vi—Na4—H92124.2
O14B—Mo1B—O19B101.50 (5)O3—Na5—O15x158.87 (6)
O9B—Mo1B—O19B99.54 (5)O3—Na5—O14Ax86.21 (5)
O14B—Mo1B—O23B101.46 (5)O15x—Na5—O14Ax82.36 (5)
O9B—Mo1B—O23B99.65 (5)O3—Na5—O12110.20 (5)
O19B—Mo1B—O23B146.22 (4)O15x—Na5—O1284.84 (5)
O14B—Mo1B—O6B86.61 (4)O14Ax—Na5—O12160.63 (5)
O9B—Mo1B—O6B171.55 (4)O3—Na5—O7x80.56 (5)
O19B—Mo1B—O6B79.67 (4)O15x—Na5—O7x85.39 (5)
O23B—Mo1B—O6B77.31 (4)O14Ax—Na5—O7x105.30 (5)
O14B—Mo1B—O3B170.15 (4)O12—Na5—O7x88.03 (5)
O9B—Mo1B—O3B85.40 (4)O3—Na5—O9Bv79.66 (4)
O19B—Mo1B—O3B83.76 (4)O15x—Na5—O9Bv116.19 (5)
O23B—Mo1B—O3B70.39 (4)O14Ax—Na5—O9Bv82.76 (4)
O6B—Mo1B—O3B86.16 (3)O12—Na5—O9Bv89.96 (5)
O10B—Mo2B—O15B102.25 (6)O7x—Na5—O9Bv158.06 (5)
O10B—Mo2B—O19B102.34 (5)O1ii—Na6—O18Bv173.83 (6)
O15B—Mo2B—O19B100.28 (5)O1ii—Na6—O11A83.19 (5)
O10B—Mo2B—O20B100.37 (5)O18Bv—Na6—O11A92.36 (5)
O15B—Mo2B—O20B96.72 (5)O1ii—Na6—O289.19 (5)
O19B—Mo2B—O20B147.90 (4)O18Bv—Na6—O293.83 (5)
O10B—Mo2B—O2B87.44 (5)O11A—Na6—O275.31 (5)
O15B—Mo2B—O2B169.73 (5)O1ii—Na6—O1486.93 (5)
O19B—Mo2B—O2B80.68 (4)O18Bv—Na6—O1487.94 (5)
O20B—Mo2B—O2B77.97 (4)O11A—Na6—O1477.56 (5)
O10B—Mo2B—O8B168.43 (5)O2—Na6—O14152.86 (5)
O15B—Mo2B—O8B84.88 (5)O1ii—Na6—O7Bv114.27 (5)
O19B—Mo2B—O8B85.09 (4)O18Bv—Na6—O7Bv68.03 (4)
O20B—Mo2B—O8B69.48 (4)O11A—Na6—O7Bv150.16 (5)
O2B—Mo2B—O8B85.02 (3)O2—Na6—O7Bv126.23 (5)
O11B—Mo3B—O16B104.68 (7)O14—Na6—O7Bv79.40 (4)
O11B—Mo3B—O20B97.40 (5)O1ii—Na6—O17Bv100.56 (5)
O16B—Mo3B—O20B99.23 (6)O18Bv—Na6—O17Bv85.58 (4)
O11B—Mo3B—O21B99.59 (6)O11A—Na6—O17Bv142.03 (5)
O16B—Mo3B—O21B94.53 (5)O2—Na6—O17Bv67.03 (4)
O20B—Mo3B—O21B154.64 (4)O14—Na6—O17Bv140.04 (5)
O11B—Mo3B—O8B156.61 (5)O7Bv—Na6—O17Bv61.63 (3)
O16B—Mo3B—O8B98.14 (5)O20—Na7—O13Bv87.38 (6)
O20B—Mo3B—O8B73.56 (4)O20—Na7—O5Biv169.63 (6)
O21B—Mo3B—O8B83.51 (4)O13Bv—Na7—O5Biv84.19 (4)
O11B—Mo3B—O4B85.93 (5)O20—Na7—O1287.87 (6)
O16B—Mo3B—O4B164.14 (5)O13Bv—Na7—O12106.61 (5)
O20B—Mo3B—O4B90.88 (4)O5Biv—Na7—O12100.32 (5)
O21B—Mo3B—O4B71.78 (4)O20—Na7—O14vii102.96 (6)
O8B—Mo3B—O4B72.93 (3)O13Bv—Na7—O14vii162.97 (5)
O17B—Mo4B—O12B103.73 (6)O5Biv—Na7—O14vii83.91 (4)
O17B—Mo4B—O21B101.14 (5)O12—Na7—O14vii87.50 (5)
O12B—Mo4B—O21B101.57 (5)O20—Na7—O180.53 (6)
O17B—Mo4B—O22B99.57 (5)O13Bv—Na7—O184.83 (5)
O12B—Mo4B—O22B98.32 (5)O5Biv—Na7—O192.68 (5)
O21B—Mo4B—O22B146.83 (4)O12—Na7—O1163.38 (6)
O17B—Mo4B—O4B166.92 (5)O14vii—Na7—O183.60 (5)
O12B—Mo4B—O4B89.17 (5)H51—O5—H52105.0
O21B—Mo4B—O4B73.69 (4)H71—O7—H72105.0
O22B—Mo4B—O4B80.36 (4)H81—O8—H82104.9
O17B—Mo4B—O7B85.57 (5)H91—O9—H92105.0
O12B—Mo4B—O7B168.90 (5)H101—O10—H102105.0
O21B—Mo4B—O7B82.23 (4)H111—O11—H112105.0
O22B—Mo4B—O7B73.83 (4)H121—O12—H122105.0
O4B—Mo4B—O7B81.85 (3)H131—O13—H132105.0
O13B—Mo5B—O18B105.26 (6)H141—O14—H142105.0
O13B—Mo5B—O22B96.53 (5)H151—O15—H152105.0
O18B—Mo5B—O22B98.97 (5)H161—O16—H162105.0
O13B—Mo5B—O23B99.76 (5)H171—O17—H172105.0
O18B—Mo5B—O23B96.50 (5)H181—O18—H182104.9
O22B—Mo5B—O23B153.69 (4)H191—O19—H192104.9
O13B—Mo5B—O3B96.85 (5)H201—O20—H202104.9
O18B—Mo5B—O3B157.26 (5)H211—O21—H212104.9
O22B—Mo5B—O3B83.47 (4)H11N—N1—H12N109.5
O23B—Mo5B—O3B74.21 (4)H11N—N1—H13N109.5
O13B—Mo5B—O7B166.16 (5)H12N—N1—H13N109.5
O18B—Mo5B—O7B85.72 (4)H11N—N1—H14N109.5
O22B—Mo5B—O7B73.07 (4)H12N—N1—H14N109.5
O23B—Mo5B—O7B87.07 (4)H13N—N1—H14N109.5
O3B—Mo5B—O7B73.29 (3)H21N—N2—H22N109.5
O1B—P1B—O2B112.22 (6)H21N—N2—H23N109.5
O1B—P1B—O4B109.35 (6)H22N—N2—H23N109.5
O2B—P1B—O4B108.15 (6)H21N—N2—H24N109.5
O1B—P1B—O3B111.48 (6)H22N—N2—H24N109.5
O2B—P1B—O3B106.11 (5)H23N—N2—H24N109.5
O4B—P1B—O3B109.40 (5)H31N—N3—H32N109.4
O5B—P2B—O6B111.49 (6)H31N—N3—H33N109.5
O5B—P2B—O7B110.43 (6)H32N—N3—H33N109.5
O6B—P2B—O7B109.17 (5)H31N—N3—H34N109.5
O5B—P2B—O8B110.02 (6)H32N—N3—H34N109.5
O6B—P2B—O8B106.37 (5)H33N—N3—H34N109.5
O7B—P2B—O8B109.26 (5)H41N—N4—H42N109.5
O6vii—Na1—O5151.31 (6)H41N—N4—H43N109.5
O6vii—Na1—O8viii80.81 (5)H42N—N4—H43N109.5
O5—Na1—O8viii85.76 (5)H41N—N4—H44N109.5
O6vii—Na1—O10Bvi81.44 (5)H42N—N4—H44N109.4
O5—Na1—O10Bvi78.23 (5)H43N—N4—H44N109.4
O8viii—Na1—O10Bvi106.45 (5)H51N—N5—H52N109.5
O6vii—Na1—O18117.14 (6)H51N—N5—H53N109.5
O5—Na1—O1890.43 (6)H52N—N5—H53N109.4
O8viii—Na1—O18102.53 (6)H51N—N5—H54N109.5
O10Bvi—Na1—O18147.83 (6)H52N—N5—H54N109.5
O6vii—Na1—O15Avii81.16 (4)H53N—N5—H54N109.5
O5—Na1—O15Avii114.30 (5)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1—H11···O12Bix0.862.022.8415 (18)160
N1—H11N···O12A0.872.072.750 (2)135
O1—H12···O16Avii0.862.553.383 (2)164
N1—H12N···O200.872.132.963 (3)161
N1—H13N···O18Bv0.872.372.909 (2)121
N1—H14N···O23Bv0.872.292.922 (2)130
O2—H21···O21Bxi0.862.293.1414 (17)172
N2—H21N···O5Avii0.872.102.8892 (19)151
N2—H21N···O13A0.872.593.146 (2)123
O2—H22···O20A0.862.072.9134 (18)165
N2—H22N···O9A0.872.203.036 (2)162
N2—H23N···O1A0.871.982.837 (2)171
N2—H24N···O15Avii0.872.062.9121 (19)167
O3—H31···O23Av0.861.862.7120 (16)174
N3—H31N···O5Biv0.871.952.8066 (19)170
O3—H32···O14Bv0.862.002.8440 (16)165
N3—H32N···O9Bv0.872.092.9533 (19)173
N3—H33N···O1Bv0.872.042.8410 (19)152
N3—H34N···O15Biv0.872.193.017 (2)159
O4—H41···O10vii0.861.892.743 (2)172
N4—H41N···O1A0.872.002.8544 (19)171
O4—H42···O23A0.862.573.403 (2)164
N4—H42N···O5Avii0.872.022.8757 (19)169
N4—H43N···O12Av0.872.443.123 (2)136
N4—H43N···O22A0.872.262.9312 (19)134
N4—H44N···O17Av0.872.232.958 (2)142
O5—H51···O9A0.862.403.0367 (18)132
O5—H51···O15Bvi0.862.423.201 (2)151
N5—H51N···O1Bv0.872.032.8649 (19)162
O5—H52···O2A0.861.972.8118 (18)167
N5—H52N···O5Biv0.871.962.8251 (17)175
N5—H53N···O13Bv0.872.552.9140 (18)106
N5—H54N···O21Biv0.872.453.0098 (18)123
N5—H54N···O17Bix0.872.283.0203 (19)144
O6—H61···O10A0.862.012.8234 (17)159
O6—H62···O20Bxi0.861.842.6971 (16)176
O7—H71···O3v0.861.892.7347 (19)167
O7—H72···O6Axii0.862.092.9430 (16)173
O8—H81···O60.861.872.7221 (19)174
O8—H82···O2Bxii0.862.012.8642 (16)171
O9—H91···O5Axii0.861.902.7476 (18)171
O9—H92···O13Avi0.862.342.9118 (19)124
O9—H92···O14Bvi0.862.583.0630 (18)117
O1—H01···O9Bxii0.862.202.985 (2)152
O10—H102···O6A0.862.102.893 (2)153
O11—H111···O17Axiii0.862.582.987 (2)110
O11—H112···O17Axiii0.862.582.987 (2)110
O11—H112···O21A0.862.393.126 (2)143
O12—H121···O9x0.862.042.891 (2)171
O12—H122···O18Av0.862.012.834 (2)160
O13—H131···O19Ax0.862.132.944 (2)158
O13—H132···O2Bv0.862.122.904 (2)151
O14—H141···O110.861.922.772 (2)171
O14—H142···O6Bv0.862.172.9073 (18)143
O15—H151···O6Bvi0.862.012.8578 (17)169
O15—H152···O15Bvi0.862.373.0264 (18)134
O15—H152···O9A0.862.433.192 (2)148
O16—H161···O13xiv0.861.922.769 (2)171
O16—H162···O20Bxi0.862.393.220 (2)163
O17—H171···O1Bix0.862.443.167 (2)143
O17—H172···O16Bxi0.862.182.949 (2)149
O18—H181···O1A0.862.353.105 (2)147
O18—H182···O11Bix0.862.342.874 (2)121
O19—H191···O210.862.483.270 (4)154
O19—H192···O20.861.992.830 (3)166
O20—H201···O210.861.872.716 (3)166
O20—H202···O17Av0.861.932.757 (2)162
O21—H211···O1A0.861.932.784 (3)169
O21—H212···O18Bv0.862.442.992 (3)123

Symmetry codes: (ix) x, y, z−1; (vii) x−1, y, z; (v) −x+1, −y+1, −z+1; (xi) x+1, y, z−1; (iv) −x, −y+1, −z+1; (vi) −x, −y+2, −z+1; (xii) −x+1, −y+2, −z+1; (xiii) −x+2, −y+1, −z+1; (x) x, y−1, z; (xiv) −x+1, −y+1, −z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FJ2276).

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