Acta Cryst.(2003). E59, i151±i153 DOI: 10.1107/S1600536803024024 Dan BostroÈmet al. NaRb3(VO3)4(H2O)
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inorganic papers
Acta Crystallographica Section E
Structure Reports
Online ISSN 1600-5368
Sodium trirubidium metavanadate
monohydrate
Dan BostroÈm,* Gustaf Bergquist and Lage Pettersson
Department of Chemistry, Inorganic Chemistry, UmeaÊ University, SE-901 87 UmeaÊ, Sweden
Correspondence e-mail: dan.bostrom@chem.umu.se
Key indicators Single-crystal X-ray study T= 150 K
Mean(V±O) = 0.002 AÊ Rfactor = 0.034 wRfactor = 0.077
Data-to-parameter ratio = 21.2
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
#2003 International Union of Crystallography Printed in Great Britain ± all rights reserved
The title compound, sodium trirubidium metavanadate
monohydrate, NaRb3(VO3)4(H2O), crystallizes in the
ortho-rhombic space groupPnma. The structure, which represents a
rare type of catena-vanadate, is built up of strongly folded
chains of corner-sharing [VO4] tetrahedra, running in the [010]
direction with a periodicity of four. A three-dimensional framework is obtained by sodium ions linking adjacent chains in the [001] direction and by rubidium ions linking adjacent chains in the [100] direction. The single water molecule binds to the sodium ion and to two rubidium ions.
Comment
As part of a continuing research project, vanadate±organic ligand systems of biomedical interest are studied. The primary aim is to determine the complete speciation by using
poten-tiometry and multinuclear NMR (with emphasis on51V). In
the ongoing study of the vanadocitrate (V-Cit) system, a series of anionic divanadocitrate species were found to be formed,
having chargesÿ4,ÿ3 andÿ2. Our goal is also to determine
the aqueous and solid structures of species formed. No X-ray structures of these species have been published and therefore extensive crystallization experiments have been performed and are still in progress. So far, we have not been able to obtain single crystals of any divanadocitrate species, but crystals of other compounds have been found. We report here the structure of a mixed cation metavanadate, NaRb3(VO3)4(H2O).
Received 13 October 2003 Accepted 20 October 2003 Online 31 October 2003
Figure 1
inorganic papers
i152
Dan BostroÈmet al. NaRb3(VO3)4(H2O) Acta Cryst.(2003). E59, i151±i153The title compound possesses a rare type of metavanadate
chain structure, built up of corner-sharing [VO4] tetrahedra.
The chains, which are strongly folded with a periodicity of four, run in the [010] direction (Fig. 1). The folding is described by the angles V2ÐO6ÐV2, O6ÐV2ÐO4, V2Ð O4ÐV1, O4ÐV1ÐO2 and V1ÐO2ÐV1 (Fig. 2 and Table 1). A three-dimensional framework is obtained by sodium ions linking adjacent chains in the [001] direction and by rubidium ions linking adjacent chains in the [100] direction (Fig. 3).
The vanadate tetrahedra have angles and VÐO distances common for vanadate chain structures (Table 1). The sodium ion is coordinated by six vanadate O atoms and a water molecule within distances ranging from 2.282 (2) to 2.705 (3) AÊ, and with a mean distance of 2.470 (8) AÊ. There are three crystallographically different rubidium ions. If distances shorter than 3.4 AÊ are considered, Rb1 is coordin-ated by nine O atoms between 2.892 (4) and 3.382 (4) AÊ (including a water molecule), with a mean distance of 3.123 (10) AÊ, Rb2 coordinate ten O atoms within 2.837 (3)± 3.324 (2) AÊ, with a mean distance of 3.127 (9) AÊ, and Rb3 coordinate nine O atoms (including a water molecule), within 2.946 (2)±3.335 (3) AÊ, with a mean distance of 3.126 (8) AÊ (Table 1 and Fig. 2).
An isotypic structure, NaCs3(VO3)4(H2O), was brie¯y
described by Elvingson (1997). The structure of Th(VO3)2O
(Launayet al., 1992), contains similar folded chains arranged
in layers. In addition, however, this structure also contains isolated vanadate tetrahedra. In the large group of silicate chain structures, there are several examples of a periodicity of four tetrahedra. A close resemblance exists between the
present structure and that of Cu3Na2(SiO3)4 (Kawamura &
Kawahara, 1976) with respect to both the features and the packing of the chains.
Experimental
1 ml of methanol was added to 1.2 ml of an aqueous pH 7.6 solution containing [V5+]
tot= 670 mM, [Cit]tot= 420 mM, [Na+]tot= 1580 mM and [Rb+]
tot= 330 mM, and the resulting solution was allowed to evaporate at room temperature. Pale yellow crystals of appropriate dimensions formed within hours.
Crystal data
NaRb3(VO3)4(H2O)
Mr= 693.18 Orthorhombic,Pnma a= 11.1610 (5) AÊ
b= 8.3050 (11) AÊ
c= 15.8180 (8) AÊ
V= 1466.2 (2) AÊ3
Z= 4
Dx= 3.140 Mg mÿ3
MoKradiation Cell parameters from 2407
re¯ections
= 2.9±33.1
= 12.45 mmÿ1
T= 150 K Prism, light yellow 0.140.130.10 mm
Data collection
Nonius KappaCCD diffractometer
'and!scans
Absorption correction: multi-scan
(HKL SCALEPACK;
Otwinowski & Minor, 1997)
Tmin= 0.203,Tmax= 0.288
24175 measured re¯ections
2271 independent re¯ections 2175 re¯ections withI> 2(I)
Rint= 0.083 max= 30.0
h=ÿ15!15
k=ÿ11!11
l=ÿ22!22
Re®nement
Re®nement onF2
R[F2> 2(F2)] = 0.034
wR(F2) = 0.077
S= 1.14 2271 re¯ections 107 parameters
H-atom parameters constrained
w= 1/[2(F
o2) + (0.0136P)2 + 4.7048P]
whereP= (Fo2+ 2Fc2)/3 (/)max= 0.001
max= 1.09 e AÊÿ3 min=ÿ1.87 e AÊÿ3
Extinction correction:SHELXL97 Extinction coef®cient: 0.0036 (5)
Figure 3
Packing diagram showing the metavanadate chains and the positions of the rubidium ions, sodium ions, water O and H atoms (green, yellow, red and blue spheres of arbitrary size, respectively).
Figure 2
Table 1
Selected geometric parameters (AÊ,).
Rb1ÐO6 2.892 (4)
Rb1ÐO1i 3.029 (2)
Rb1ÐO5i 3.046 (3)
Rb1ÐO1ii 3.194 (3)
Rb1ÐOwiii 3.299 (4)
Rb1ÐO2iv 3.382 (4)
Rb2ÐO2v 2.837 (3)
Rb2ÐO4 2.986 (3)
Rb2ÐO5vi 3.132 (3)
Rb2ÐO6 3.140 (4)
Rb2ÐO3vii 3.203 (3)
Rb2ÐO3viii 3.324 (2)
Rb3ÐO5i 2.946 (3)
Rb3ÐO4 3.033 (3)
Rb3ÐOw 3.127 (4)
Rb3ÐO3ix 3.190 (2)
Rb3ÐO7 3.335 (3)
V1ÐO3 1.632 (2)
V1ÐO1 1.648 (2)
V1ÐO2x 1.8025 (10)
V1ÐO4 1.804 (2)
V2ÐO7 1.624 (3)
V2ÐO5 1.641 (2)
V2ÐO6 1.8064 (15)
V2ÐO4 1.815 (2)
NaÐO7 2.282 (3)
NaÐOw 2.349 (4)
NaÐO1xi 2.483 (3)
NaÐO3xi 2.705 (3)
O3ÐV1ÐO1 108.47 (13) O3ÐV1ÐO2x 109.15 (14)
O1ÐV1ÐO2x 110.18 (15)
O3ÐV1ÐO4 109.36 (12) O1ÐV1ÐO4 109.47 (11) O2xÐV1ÐO4 110.19 (14)
O7ÐV2ÐO5 110.13 (15) O7ÐV2ÐO6 107.39 (16)
O5ÐV2ÐO6 110.22 (15) O7ÐV2ÐO4 108.21 (13) O5ÐV2ÐO4 113.59 (12) O6ÐV2ÐO4 107.07 (15) V2viiiÐO6ÐV2 134.5 (2)
V1xiiÐO2ÐV1xiii 150.6 (2)
V1ÐO4ÐV2 135.92 (14)
Symmetry codes: (i)xÿ1
2;y;32ÿz; (ii)32ÿx;12y;12z; (iii) 1ÿx;1ÿy;2ÿz; (iv) 3
2ÿx;ÿy;12z; (v) 1ÿx;ÿy;1ÿz; (vi)xÿ12;32ÿy;32ÿz; (vii) 1ÿx;1ÿy;1ÿz; (viii)
x;3
2ÿy;z; (ix) 1ÿx;yÿ21;1ÿz; (x)x;1y;z; (xi)32ÿx;1ÿy;21z; (xii)x;yÿ1;z;
(xiii)x;ÿ1 2ÿy;z.
The H atoms of the water molecule were located inm a difference Fourier map, ®xed at a distance of 0.97 AÊ and re®ned using a riding
model withU(iso)(H) = 1.2Ueq(O). The highest peak and deepest hole in the difference density map are located at distances of 1.58 and 0.73 AÊ from atoms H8 and Rb3, respectively.
Data collection:COLLECT(Nonius, 1999); cell re®nement:HKL SCALEPACK(Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to re®ne structure:SHELXL97 (Sheldrick, 1997); molecular graphics:ATOMS(Dowty, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and local procedures.
This work was supported by the Swedish Research Council.
References
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999).J. Appl. Cryst.32, 115±119.
Dowty, E. (2000).ATOMS for Windows and Macintosh. Version 5.1. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA.
Elvingson, K. (1997). PhD Thesis, UmeaÊ University, Sweden. Kawamura, K. & Kawahara, A. (1976).Acta Cryst.B32, 2419±2422. Launay, S., Mahe, P., Quarton, M. & Robert, F. (1992).J. Solid State Chem.97,
305±313.
Nonius (1999).COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A, edited by C. W. Carter Jr and
R. M. Sweet, pp. 307±326. New York: Academic Press.
Sheldrick, G. M. (1997).SHELXL97. University of GoÈttingen, Germany.
Acta Cryst.(2003). E59, i151±i153 Dan BostroÈmet al. NaRb3(VO3)4(H2O)
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supporting information
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Acta Cryst. (2003). E59, i151–i153
supporting information
Acta Cryst. (2003). E59, i151–i153 [https://doi.org/10.1107/S1600536803024024]
Sodium trirubidium metavanadate monohydrate
Dan Bostr
ö
m, Gustaf Bergquist and Lage Pettersson
(I)
Crystal data
NaRb3(VO3)4(H2O)
Mr = 693.18
Orthorhombic, Pnma
Hall symbol: -P 2ac 2n
a = 11.1610 (5) Å
b = 8.3050 (11) Å
c = 15.8180 (8) Å
V = 1466.2 (2) Å3
Z = 4
F(000) = 1280
Dx = 3.140 Mg m−3
Mo Kα radiation, λ = 0.71073 Å Cell parameters from 2407 reflections
θ = 2.9–33.1°
µ = 12.45 mm−1
T = 150 K
Prism, light yellow 0.14 × 0.13 × 0.10 mm
Data collection
Nonius KappaCCD diffractometer
Radiation source: fine-focus sealed tube, KappaCCD
Graphite monochromator
φ and ω scans
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski & Minor, 1997)
Tmin = 0.203, Tmax = 0.288
24175 measured reflections 2271 independent reflections 2175 reflections with I > 2σ(I)
Rint = 0.083
θmax = 30.0°, θmin = 3.2°
h = −15→15
k = −11→11
l = −22→22
Refinement
Refinement on F2
Least-squares matrix: full
R[F2 > 2σ(F2)] = 0.034
wR(F2) = 0.077
S = 1.14 2271 reflections 107 parameters 0 restraints
Primary atom site location: structure-invariant direct methods
Secondary atom site location: difference Fourier map
H-atom parameters constrained
w = 1/[σ2(F
o2) + (0.0136P)2 + 4.7048P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.001
Δρmax = 1.09 e Å−3
Δρmin = −1.87 e Å−3
Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Extinction coefficient: 0.0036 (5)
Special details
supporting information
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Acta Cryst. (2003). E59, i151–i153
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)
x y z Uiso*/Ueq
Rb1 0.52769 (4) 0.7500 0.89948 (3) 0.02539 (14) Rb2 0.48559 (4) 0.7500 0.62101 (3) 0.01808 (12) Rb3 0.48232 (5) 0.2500 0.69433 (4) 0.02690 (14) V1 0.71486 (4) 0.45993 (6) 0.52643 (3) 0.01183 (13) V2 0.74207 (5) 0.54938 (7) 0.73235 (3) 0.01450 (14) Na 0.68488 (18) 0.2500 0.91556 (11) 0.0189 (4) O1 0.8537 (2) 0.5234 (3) 0.51424 (14) 0.0216 (5) O2 0.7038 (3) −0.7500 0.4986 (2) 0.0218 (7) O3 0.6281 (2) 0.5647 (3) 0.46424 (15) 0.0218 (5) O4 0.6691 (2) 0.4897 (3) 0.63472 (13) 0.0203 (5) O5 0.8889 (2) 0.5460 (3) 0.72709 (16) 0.0260 (6) O6 0.6904 (3) 0.7500 0.7572 (2) 0.0227 (7) O7 0.6958 (3) 0.4309 (4) 0.80725 (17) 0.0349 (7) Ow 0.4771 (3) 0.2500 0.8920 (2) 0.0251 (8) H8 0.4333 0.3413 0.9146 0.030*
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
Rb1 0.0199 (2) 0.0300 (3) 0.0263 (3) 0.000 0.00265 (17) 0.000 Rb2 0.0153 (2) 0.0185 (2) 0.0205 (2) 0.000 −0.00518 (15) 0.000 Rb3 0.0239 (3) 0.0157 (2) 0.0411 (3) 0.000 0.00626 (19) 0.000 V1 0.0129 (2) 0.0109 (3) 0.0117 (2) −0.00049 (17) 0.00012 (17) 0.00071 (18) V2 0.0165 (3) 0.0146 (3) 0.0124 (2) −0.00063 (19) −0.00209 (18) 0.00365 (19) Na 0.0260 (10) 0.0164 (9) 0.0143 (8) 0.000 0.0009 (7) 0.000 O1 0.0162 (11) 0.0292 (13) 0.0194 (11) −0.0075 (10) 0.0018 (8) −0.0008 (10) O2 0.0298 (18) 0.0129 (16) 0.0226 (17) 0.000 −0.0080 (14) 0.000 O3 0.0254 (12) 0.0211 (12) 0.0190 (11) 0.0049 (10) −0.0029 (9) 0.0041 (9) O4 0.0165 (11) 0.0310 (14) 0.0134 (10) −0.0005 (9) 0.0005 (8) −0.0022 (10) O5 0.0187 (12) 0.0296 (14) 0.0298 (13) 0.0043 (10) −0.0049 (10) 0.0028 (11) O6 0.0213 (17) 0.0166 (16) 0.0302 (18) 0.000 0.0033 (14) 0.000 O7 0.0488 (18) 0.0349 (16) 0.0211 (13) −0.0178 (14) −0.0072 (12) 0.0135 (12) Ow 0.0216 (18) 0.025 (2) 0.0287 (19) 0.000 0.0025 (14) 0.000
Geometric parameters (Å, º)
Rb1—O6 2.892 (4) V1—O3 1.632 (2)
Rb1—O1i 3.029 (2) V1—O1 1.648 (2)
Rb1—O1ii 3.029 (2) V1—O2xiv 1.8025 (10)
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Rb1—O5ii 3.046 (3) V2—O7 1.624 (3)
Rb1—O1iii 3.194 (3) V2—O5 1.641 (2)
Rb1—O1iv 3.194 (3) V2—O6 1.8064 (15)
Rb1—Owv 3.299 (4) V2—O4 1.815 (2)
Rb1—O2vi 3.382 (4) Na—O7 2.282 (3)
Rb1—O7 3.560 (3) Na—O7xii 2.282 (3)
Rb1—O7vii 3.560 (4) Na—Ow 2.349 (4)
Rb2—O2viii 2.837 (3) Na—O1iv 2.483 (3)
Rb2—O4 2.986 (3) Na—O1xv 2.483 (3)
Rb2—O4vii 2.986 (3) Na—O3iv 2.705 (3)
Rb2—O5ii 3.132 (3) Na—O3xv 2.705 (3)
Rb2—O5i 3.132 (3) O6—V2vii 1.8064 (15)
Rb2—O6 3.140 (4) O5—Rb3xvi 2.946 (3)
Rb2—O3ix 3.203 (3) O5—Rb1xvi 3.046 (3)
Rb2—O3x 3.203 (3) O5—Rb2xvi 3.132 (3)
Rb2—O3vii 3.324 (2) O2—V1xvii 1.8025 (10)
Rb2—O3 3.324 (2) O2—V1xviii 1.8025 (10)
Rb3—O5i 2.946 (3) O2—Rb2viii 2.837 (3)
Rb3—O5xi 2.946 (3) O2—Rb1xix 3.382 (4)
Rb3—O4 3.033 (3) O1—Naxx 2.483 (3)
Rb3—O4xii 3.033 (2) O1—Rb1xvi 3.029 (2)
Rb3—Ow 3.127 (4) O1—Rb1xx 3.194 (3)
Rb3—O3xiii 3.190 (2) O3—Naxx 2.705 (3)
Rb3—O3ix 3.190 (2) O3—Rb3ix 3.190 (2)
Rb3—O7 3.335 (3) O3—Rb2ix 3.203 (3)
Rb3—O7xii 3.335 (3) Ow—Rb1v 3.299 (4)
Rb3—O7xi 3.533 (3) Ow—H8 0.9704
Rb3—O7i 3.533 (3) O7—Rb3xvi 3.533 (3)
O6—Rb1—O1i 138.87 (5) O3ix—Rb2—O3 59.85 (8)
O6—Rb1—O1ii 138.87 (5) O3x—Rb2—O3 104.67 (4)
O1i—Rb1—O1ii 76.82 (10) O3vii—Rb2—O3 55.16 (9)
O6—Rb1—O5i 78.90 (8) O5i—Rb3—O5xi 113.16 (10)
O1i—Rb1—O5i 67.96 (7) O5i—Rb3—O4 80.02 (7)
O1ii—Rb1—O5i 108.40 (7) O5xi—Rb3—O4 157.27 (7)
O6—Rb1—O5ii 78.90 (8) O5i—Rb3—O4xii 157.26 (7)
O1i—Rb1—O5ii 108.40 (7) O5xi—Rb3—O4xii 80.02 (7)
O1ii—Rb1—O5ii 67.96 (7) O4—Rb3—O4xii 82.04 (10)
O5i—Rb1—O5ii 67.58 (10) O5i—Rb3—Ow 64.63 (6)
O6—Rb1—O1iii 100.50 (7) O5xi—Rb3—Ow 64.63 (6)
O1i—Rb1—O1iii 116.82 (3) O4—Rb3—Ow 108.89 (6)
O1ii—Rb1—O1iii 64.40 (7) O4xii—Rb3—Ow 108.89 (6)
O5i—Rb1—O1iii 168.42 (7) O5i—Rb3—O3xiii 126.70 (7)
O5ii—Rb1—O1iii 100.89 (7) O5xi—Rb3—O3xiii 78.02 (7)
O6—Rb1—O1iv 100.50 (7) O4—Rb3—O3xiii 109.73 (6)
O1i—Rb1—O1iv 64.40 (7) O4xii—Rb3—O3xiii 72.82 (6)
O1ii—Rb1—O1iv 116.82 (3) Ow—Rb3—O3xiii 141.16 (6)
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O5ii—Rb1—O1iv 168.42 (7) O5xi—Rb3—O3ix 126.70 (7)
O1iii—Rb1—O1iv 90.61 (9) O4—Rb3—O3ix 72.82 (6)
O6—Rb1—Owv 142.04 (10) O4xii—Rb3—O3ix 109.73 (6)
O1i—Rb1—Owv 62.55 (6) Ow—Rb3—O3ix 141.16 (6)
O1ii—Rb1—Owv 62.55 (6) O3xiii—Rb3—O3ix 57.68 (9)
O5i—Rb1—Owv 130.47 (7) O5i—Rb3—O7 69.57 (8)
O5ii—Rb1—Owv 130.47 (7) O5xi—Rb3—O7 113.75 (7)
O1iii—Rb1—Owv 55.84 (5) O4—Rb3—O7 51.67 (6)
O1iv—Rb1—Owv 55.84 (5) O4xii—Rb3—O7 88.34 (8)
O6—Rb1—O2vi 78.73 (9) Ow—Rb3—O7 58.53 (7)
O1i—Rb1—O2vi 111.05 (6) O3xiii—Rb3—O7 156.10 (7)
O1ii—Rb1—O2vi 111.05 (6) O3ix—Rb3—O7 118.67 (7)
O5i—Rb1—O2vi 139.05 (6) O5i—Rb3—O7xii 113.75 (7)
O5ii—Rb1—O2vi 139.05 (6) O5xi—Rb3—O7xii 69.57 (8)
O1iii—Rb1—O2vi 50.91 (5) O4—Rb3—O7xii 88.34 (8)
O1iv—Rb1—O2vi 50.91 (5) O4xii—Rb3—O7xii 51.67 (6)
Owv—Rb1—O2vi 63.31 (8) Ow—Rb3—O7xii 58.53 (7)
O6—Rb1—O7 49.47 (5) O3xiii—Rb3—O7xii 118.67 (7)
O1i—Rb1—O7 93.44 (7) O3ix—Rb3—O7xii 156.10 (7)
O1ii—Rb1—O7 170.09 (7) O7—Rb3—O7xii 53.53 (11)
O5i—Rb1—O7 65.46 (7) O5i—Rb3—O7xi 92.15 (7)
O5ii—Rb1—O7 114.37 (7) O5xi—Rb3—O7xi 47.76 (7)
O1iii—Rb1—O7 122.94 (6) O4—Rb3—O7xi 154.03 (6)
O1iv—Rb1—O7 59.02 (6) O4xii—Rb3—O7xi 109.94 (7)
Owv—Rb1—O7 114.72 (6) Ow—Rb3—O7xi 89.44 (7)
O2vi—Rb1—O7 73.91 (6) O3xiii—Rb3—O7xi 55.93 (6)
O6—Rb1—O7vii 49.47 (5) O3ix—Rb3—O7xi 81.37 (6)
O1i—Rb1—O7vii 170.09 (7) O7—Rb3—O7xi 147.34 (4)
O1ii—Rb1—O7vii 93.44 (7) O7xii—Rb3—O7xi 117.32 (8)
O5i—Rb1—O7vii 114.37 (7) O5i—Rb3—O7i 47.76 (7)
O5ii—Rb1—O7vii 65.46 (7) O5xi—Rb3—O7i 92.15 (7)
O1iii—Rb1—O7vii 59.02 (6) O4—Rb3—O7i 109.94 (7)
O1iv—Rb1—O7vii 122.94 (7) O4xii—Rb3—O7i 154.03 (6)
Owv—Rb1—O7vii 114.72 (6) Ow—Rb3—O7i 89.44 (7)
O2vi—Rb1—O7vii 73.91 (6) O3xiii—Rb3—O7i 81.37 (6)
O7—Rb1—O7vii 96.23 (9) O3ix—Rb3—O7i 55.93 (6)
O2viii—Rb2—O4 124.03 (6) O7—Rb3—O7i 117.32 (8)
O2viii—Rb2—O4vii 124.03 (6) O7xii—Rb3—O7i 147.34 (4)
O4—Rb2—O4vii 92.77 (10) O7xi—Rb3—O7i 50.32 (10)
O2viii—Rb2—O5ii 104.76 (8) O3—V1—O1 108.47 (13)
O4—Rb2—O5ii 124.91 (6) O3—V1—O2xiv 109.15 (14)
O4vii—Rb2—O5ii 77.82 (6) O1—V1—O2xiv 110.18 (15)
O2viii—Rb2—O5i 104.76 (8) O3—V1—O4 109.36 (12)
O4—Rb2—O5i 77.82 (6) O1—V1—O4 109.47 (11)
O4vii—Rb2—O5i 124.91 (6) O2xiv—V1—O4 110.19 (14)
O5ii—Rb2—O5i 65.49 (10) O7—V2—O5 110.13 (15)
O2viii—Rb2—O6 178.52 (10) O7—V2—O6 107.39 (16)
supporting information
sup-5
Acta Cryst. (2003). E59, i151–i153
O4vii—Rb2—O6 56.70 (6) O7—V2—O4 108.21 (13)
O5ii—Rb2—O6 74.01 (7) O5—V2—O4 113.59 (12)
O5i—Rb2—O6 74.01 (7) O6—V2—O4 107.07 (15)
O2viii—Rb2—O3ix 54.83 (4) O7—Na—O7xii 82.34 (17)
O4—Rb2—O3ix 73.23 (6) O7—Na—Ow 86.20 (12)
O4vii—Rb2—O3ix 153.26 (6) O7xii—Na—Ow 86.20 (12)
O5ii—Rb2—O3ix 128.90 (7) O7—Na—O1iv 88.99 (10)
O5i—Rb2—O3ix 75.24 (6) O7xii—Na—O1iv 168.63 (12)
O6—Rb2—O3ix 125.24 (4) Ow—Na—O1iv 85.90 (10)
O2viii—Rb2—O3x 54.83 (4) O7—Na—O1xv 168.63 (12)
O4—Rb2—O3x 153.26 (6) O7xii—Na—O1xv 88.99 (10)
O4vii—Rb2—O3x 73.23 (6) Ow—Na—O1xv 85.90 (10)
O5ii—Rb2—O3x 75.24 (6) O1iv—Na—O1xv 98.58 (13)
O5i—Rb2—O3x 128.90 (7) O7—Na—O3iv 78.35 (10)
O6—Rb2—O3x 125.24 (4) O7xii—Na—O3iv 123.16 (12)
O3ix—Rb2—O3x 109.37 (8) Ow—Na—O3iv 143.80 (7)
O2viii—Rb2—O3vii 81.90 (8) O1iv—Na—O3iv 61.56 (8)
O4—Rb2—O3vii 93.50 (6) O1xv—Na—O3iv 112.71 (10)
O4vii—Rb2—O3vii 52.46 (6) O7—Na—O3xv 123.16 (12)
O5ii—Rb2—O3vii 119.14 (7) O7xii—Na—O3xv 78.35 (10)
O5i—Rb2—O3vii 171.03 (6) Ow—Na—O3xv 143.80 (7)
O6—Rb2—O3vii 99.40 (7) O1iv—Na—O3xv 112.71 (10)
O3ix—Rb2—O3vii 104.67 (4) O1xv—Na—O3xv 61.56 (8)
O3x—Rb2—O3vii 59.85 (8) O3iv—Na—O3xv 69.34 (12)
O2viii—Rb2—O3 81.90 (8) V2vii—O6—V2 134.5 (2)
O4—Rb2—O3 52.46 (6) V1xvii—O2—V1xviii 150.6 (2)
O4vii—Rb2—O3 93.50 (6) V1—O4—V2 135.92 (14)
O5ii—Rb2—O3 171.03 (6) Na—Ow—H8 116.0
O5i—Rb2—O3 119.14 (7) Rb3—Ow—H8 112.2
O6—Rb2—O3 99.40 (7) Rb1v—Ow—H8 67.9