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The title compound, sodium trirubidium metavanadate monohydrate, NaRb3(VO3)4(H2O), crystallizes in the ortho­rhombic space group Pnma. 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024024/br6122sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024024/br6122Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](V-O) = 0.002 Å
  • R factor = 0.034
  • wR factor = 0.077
  • Data-to-parameter ratio = 21.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: 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 refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and local procedures.

(I) top
Crystal data top
NaRb3(VO3)4(H2O)F(000) = 1280
Mr = 693.18Dx = 3.140 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2407 reflections
a = 11.1610 (5) Åθ = 2.9–33.1°
b = 8.3050 (11) ŵ = 12.45 mm1
c = 15.8180 (8) ÅT = 150 K
V = 1466.2 (2) Å3Prism, light yellow
Z = 40.14 × 0.13 × 0.10 mm
Data collection top
Nonius KappaCCD
diffractometer
2271 independent reflections
Radiation source: fine-focus sealed tube, KappaCCD2175 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.083
φ and ω scansθmax = 30.0°, θmin = 3.2°
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski & Minor, 1997)
h = 1515
Tmin = 0.203, Tmax = 0.288k = 1111
24175 measured reflectionsl = 2222
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.034 w = 1/[σ2(Fo2) + (0.0136P)2 + 4.7048P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.077(Δ/σ)max = 0.001
S = 1.14Δρmax = 1.09 e Å3
2271 reflectionsΔρmin = 1.87 e Å3
107 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0036 (5)
Primary atom site location: structure-invariant direct methods
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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) top
xyzUiso*/Ueq
Rb10.52769 (4)0.75000.89948 (3)0.02539 (14)
Rb20.48559 (4)0.75000.62101 (3)0.01808 (12)
Rb30.48232 (5)0.25000.69433 (4)0.02690 (14)
V10.71486 (4)0.45993 (6)0.52643 (3)0.01183 (13)
V20.74207 (5)0.54938 (7)0.73235 (3)0.01450 (14)
Na0.68488 (18)0.25000.91556 (11)0.0189 (4)
O10.8537 (2)0.5234 (3)0.51424 (14)0.0216 (5)
O20.7038 (3)0.75000.4986 (2)0.0218 (7)
O30.6281 (2)0.5647 (3)0.46424 (15)0.0218 (5)
O40.6691 (2)0.4897 (3)0.63472 (13)0.0203 (5)
O50.8889 (2)0.5460 (3)0.72709 (16)0.0260 (6)
O60.6904 (3)0.75000.7572 (2)0.0227 (7)
O70.6958 (3)0.4309 (4)0.80725 (17)0.0349 (7)
Ow0.4771 (3)0.25000.8920 (2)0.0251 (8)
H80.43330.34130.91460.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0199 (2)0.0300 (3)0.0263 (3)0.0000.00265 (17)0.000
Rb20.0153 (2)0.0185 (2)0.0205 (2)0.0000.00518 (15)0.000
Rb30.0239 (3)0.0157 (2)0.0411 (3)0.0000.00626 (19)0.000
V10.0129 (2)0.0109 (3)0.0117 (2)0.00049 (17)0.00012 (17)0.00071 (18)
V20.0165 (3)0.0146 (3)0.0124 (2)0.00063 (19)0.00209 (18)0.00365 (19)
Na0.0260 (10)0.0164 (9)0.0143 (8)0.0000.0009 (7)0.000
O10.0162 (11)0.0292 (13)0.0194 (11)0.0075 (10)0.0018 (8)0.0008 (10)
O20.0298 (18)0.0129 (16)0.0226 (17)0.0000.0080 (14)0.000
O30.0254 (12)0.0211 (12)0.0190 (11)0.0049 (10)0.0029 (9)0.0041 (9)
O40.0165 (11)0.0310 (14)0.0134 (10)0.0005 (9)0.0005 (8)0.0022 (10)
O50.0187 (12)0.0296 (14)0.0298 (13)0.0043 (10)0.0049 (10)0.0028 (11)
O60.0213 (17)0.0166 (16)0.0302 (18)0.0000.0033 (14)0.000
O70.0488 (18)0.0349 (16)0.0211 (13)0.0178 (14)0.0072 (12)0.0135 (12)
Ow0.0216 (18)0.025 (2)0.0287 (19)0.0000.0025 (14)0.000
Geometric parameters (Å, º) top
Rb1—O62.892 (4)V1—O31.632 (2)
Rb1—O1i3.029 (2)V1—O11.648 (2)
Rb1—O1ii3.029 (2)V1—O2xiv1.8025 (10)
Rb1—O5i3.046 (3)V1—O41.804 (2)
Rb1—O5ii3.046 (3)V2—O71.624 (3)
Rb1—O1iii3.194 (3)V2—O51.641 (2)
Rb1—O1iv3.194 (3)V2—O61.8064 (15)
Rb1—Owv3.299 (4)V2—O41.815 (2)
Rb1—O2vi3.382 (4)Na—O72.282 (3)
Rb1—O73.560 (3)Na—O7xii2.282 (3)
Rb1—O7vii3.560 (4)Na—Ow2.349 (4)
Rb2—O2viii2.837 (3)Na—O1iv2.483 (3)
Rb2—O42.986 (3)Na—O1xv2.483 (3)
Rb2—O4vii2.986 (3)Na—O3iv2.705 (3)
Rb2—O5ii3.132 (3)Na—O3xv2.705 (3)
Rb2—O5i3.132 (3)O6—V2vii1.8064 (15)
Rb2—O63.140 (4)O5—Rb3xvi2.946 (3)
Rb2—O3ix3.203 (3)O5—Rb1xvi3.046 (3)
Rb2—O3x3.203 (3)O5—Rb2xvi3.132 (3)
Rb2—O3vii3.324 (2)O2—V1xvii1.8025 (10)
Rb2—O33.324 (2)O2—V1xviii1.8025 (10)
Rb3—O5i2.946 (3)O2—Rb2viii2.837 (3)
Rb3—O5xi2.946 (3)O2—Rb1xix3.382 (4)
Rb3—O43.033 (3)O1—Naxx2.483 (3)
Rb3—O4xii3.033 (2)O1—Rb1xvi3.029 (2)
Rb3—Ow3.127 (4)O1—Rb1xx3.194 (3)
Rb3—O3xiii3.190 (2)O3—Naxx2.705 (3)
Rb3—O3ix3.190 (2)O3—Rb3ix3.190 (2)
Rb3—O73.335 (3)O3—Rb2ix3.203 (3)
Rb3—O7xii3.335 (3)Ow—Rb1v3.299 (4)
Rb3—O7xi3.533 (3)Ow—H80.9704
Rb3—O7i3.533 (3)O7—Rb3xvi3.533 (3)
O6—Rb1—O1i138.87 (5)O3ix—Rb2—O359.85 (8)
O6—Rb1—O1ii138.87 (5)O3x—Rb2—O3104.67 (4)
O1i—Rb1—O1ii76.82 (10)O3vii—Rb2—O355.16 (9)
O6—Rb1—O5i78.90 (8)O5i—Rb3—O5xi113.16 (10)
O1i—Rb1—O5i67.96 (7)O5i—Rb3—O480.02 (7)
O1ii—Rb1—O5i108.40 (7)O5xi—Rb3—O4157.27 (7)
O6—Rb1—O5ii78.90 (8)O5i—Rb3—O4xii157.26 (7)
O1i—Rb1—O5ii108.40 (7)O5xi—Rb3—O4xii80.02 (7)
O1ii—Rb1—O5ii67.96 (7)O4—Rb3—O4xii82.04 (10)
O5i—Rb1—O5ii67.58 (10)O5i—Rb3—Ow64.63 (6)
O6—Rb1—O1iii100.50 (7)O5xi—Rb3—Ow64.63 (6)
O1i—Rb1—O1iii116.82 (3)O4—Rb3—Ow108.89 (6)
O1ii—Rb1—O1iii64.40 (7)O4xii—Rb3—Ow108.89 (6)
O5i—Rb1—O1iii168.42 (7)O5i—Rb3—O3xiii126.70 (7)
O5ii—Rb1—O1iii100.89 (7)O5xi—Rb3—O3xiii78.02 (7)
O6—Rb1—O1iv100.50 (7)O4—Rb3—O3xiii109.73 (6)
O1i—Rb1—O1iv64.40 (7)O4xii—Rb3—O3xiii72.82 (6)
O1ii—Rb1—O1iv116.82 (3)Ow—Rb3—O3xiii141.16 (6)
O5i—Rb1—O1iv100.89 (7)O5i—Rb3—O3ix78.02 (7)
O5ii—Rb1—O1iv168.42 (7)O5xi—Rb3—O3ix126.70 (7)
O1iii—Rb1—O1iv90.61 (9)O4—Rb3—O3ix72.82 (6)
O6—Rb1—Owv142.04 (10)O4xii—Rb3—O3ix109.73 (6)
O1i—Rb1—Owv62.55 (6)Ow—Rb3—O3ix141.16 (6)
O1ii—Rb1—Owv62.55 (6)O3xiii—Rb3—O3ix57.68 (9)
O5i—Rb1—Owv130.47 (7)O5i—Rb3—O769.57 (8)
O5ii—Rb1—Owv130.47 (7)O5xi—Rb3—O7113.75 (7)
O1iii—Rb1—Owv55.84 (5)O4—Rb3—O751.67 (6)
O1iv—Rb1—Owv55.84 (5)O4xii—Rb3—O788.34 (8)
O6—Rb1—O2vi78.73 (9)Ow—Rb3—O758.53 (7)
O1i—Rb1—O2vi111.05 (6)O3xiii—Rb3—O7156.10 (7)
O1ii—Rb1—O2vi111.05 (6)O3ix—Rb3—O7118.67 (7)
O5i—Rb1—O2vi139.05 (6)O5i—Rb3—O7xii113.75 (7)
O5ii—Rb1—O2vi139.05 (6)O5xi—Rb3—O7xii69.57 (8)
O1iii—Rb1—O2vi50.91 (5)O4—Rb3—O7xii88.34 (8)
O1iv—Rb1—O2vi50.91 (5)O4xii—Rb3—O7xii51.67 (6)
Owv—Rb1—O2vi63.31 (8)Ow—Rb3—O7xii58.53 (7)
O6—Rb1—O749.47 (5)O3xiii—Rb3—O7xii118.67 (7)
O1i—Rb1—O793.44 (7)O3ix—Rb3—O7xii156.10 (7)
O1ii—Rb1—O7170.09 (7)O7—Rb3—O7xii53.53 (11)
O5i—Rb1—O765.46 (7)O5i—Rb3—O7xi92.15 (7)
O5ii—Rb1—O7114.37 (7)O5xi—Rb3—O7xi47.76 (7)
O1iii—Rb1—O7122.94 (6)O4—Rb3—O7xi154.03 (6)
O1iv—Rb1—O759.02 (6)O4xii—Rb3—O7xi109.94 (7)
Owv—Rb1—O7114.72 (6)Ow—Rb3—O7xi89.44 (7)
O2vi—Rb1—O773.91 (6)O3xiii—Rb3—O7xi55.93 (6)
O6—Rb1—O7vii49.47 (5)O3ix—Rb3—O7xi81.37 (6)
O1i—Rb1—O7vii170.09 (7)O7—Rb3—O7xi147.34 (4)
O1ii—Rb1—O7vii93.44 (7)O7xii—Rb3—O7xi117.32 (8)
O5i—Rb1—O7vii114.37 (7)O5i—Rb3—O7i47.76 (7)
O5ii—Rb1—O7vii65.46 (7)O5xi—Rb3—O7i92.15 (7)
O1iii—Rb1—O7vii59.02 (6)O4—Rb3—O7i109.94 (7)
O1iv—Rb1—O7vii122.94 (7)O4xii—Rb3—O7i154.03 (6)
Owv—Rb1—O7vii114.72 (6)Ow—Rb3—O7i89.44 (7)
O2vi—Rb1—O7vii73.91 (6)O3xiii—Rb3—O7i81.37 (6)
O7—Rb1—O7vii96.23 (9)O3ix—Rb3—O7i55.93 (6)
O2viii—Rb2—O4124.03 (6)O7—Rb3—O7i117.32 (8)
O2viii—Rb2—O4vii124.03 (6)O7xii—Rb3—O7i147.34 (4)
O4—Rb2—O4vii92.77 (10)O7xi—Rb3—O7i50.32 (10)
O2viii—Rb2—O5ii104.76 (8)O3—V1—O1108.47 (13)
O4—Rb2—O5ii124.91 (6)O3—V1—O2xiv109.15 (14)
O4vii—Rb2—O5ii77.82 (6)O1—V1—O2xiv110.18 (15)
O2viii—Rb2—O5i104.76 (8)O3—V1—O4109.36 (12)
O4—Rb2—O5i77.82 (6)O1—V1—O4109.47 (11)
O4vii—Rb2—O5i124.91 (6)O2xiv—V1—O4110.19 (14)
O5ii—Rb2—O5i65.49 (10)O7—V2—O5110.13 (15)
O2viii—Rb2—O6178.52 (10)O7—V2—O6107.39 (16)
O4—Rb2—O656.70 (6)O5—V2—O6110.22 (15)
O4vii—Rb2—O656.70 (6)O7—V2—O4108.21 (13)
O5ii—Rb2—O674.01 (7)O5—V2—O4113.59 (12)
O5i—Rb2—O674.01 (7)O6—V2—O4107.07 (15)
O2viii—Rb2—O3ix54.83 (4)O7—Na—O7xii82.34 (17)
O4—Rb2—O3ix73.23 (6)O7—Na—Ow86.20 (12)
O4vii—Rb2—O3ix153.26 (6)O7xii—Na—Ow86.20 (12)
O5ii—Rb2—O3ix128.90 (7)O7—Na—O1iv88.99 (10)
O5i—Rb2—O3ix75.24 (6)O7xii—Na—O1iv168.63 (12)
O6—Rb2—O3ix125.24 (4)Ow—Na—O1iv85.90 (10)
O2viii—Rb2—O3x54.83 (4)O7—Na—O1xv168.63 (12)
O4—Rb2—O3x153.26 (6)O7xii—Na—O1xv88.99 (10)
O4vii—Rb2—O3x73.23 (6)Ow—Na—O1xv85.90 (10)
O5ii—Rb2—O3x75.24 (6)O1iv—Na—O1xv98.58 (13)
O5i—Rb2—O3x128.90 (7)O7—Na—O3iv78.35 (10)
O6—Rb2—O3x125.24 (4)O7xii—Na—O3iv123.16 (12)
O3ix—Rb2—O3x109.37 (8)Ow—Na—O3iv143.80 (7)
O2viii—Rb2—O3vii81.90 (8)O1iv—Na—O3iv61.56 (8)
O4—Rb2—O3vii93.50 (6)O1xv—Na—O3iv112.71 (10)
O4vii—Rb2—O3vii52.46 (6)O7—Na—O3xv123.16 (12)
O5ii—Rb2—O3vii119.14 (7)O7xii—Na—O3xv78.35 (10)
O5i—Rb2—O3vii171.03 (6)Ow—Na—O3xv143.80 (7)
O6—Rb2—O3vii99.40 (7)O1iv—Na—O3xv112.71 (10)
O3ix—Rb2—O3vii104.67 (4)O1xv—Na—O3xv61.56 (8)
O3x—Rb2—O3vii59.85 (8)O3iv—Na—O3xv69.34 (12)
O2viii—Rb2—O381.90 (8)V2vii—O6—V2134.5 (2)
O4—Rb2—O352.46 (6)V1xvii—O2—V1xviii150.6 (2)
O4vii—Rb2—O393.50 (6)V1—O4—V2135.92 (14)
O5ii—Rb2—O3171.03 (6)Na—Ow—H8116.0
O5i—Rb2—O3119.14 (7)Rb3—Ow—H8112.2
O6—Rb2—O399.40 (7)Rb1v—Ow—H867.9
Symmetry codes: (i) x1/2, y, z+3/2; (ii) x1/2, y+3/2, z+3/2; (iii) x+3/2, y+1/2, z+1/2; (iv) x+3/2, y+1, z+1/2; (v) x+1, y+1, z+2; (vi) x+3/2, y, z+1/2; (vii) x, y+3/2, z; (viii) x+1, y, z+1; (ix) x+1, y+1, z+1; (x) x+1, y+1/2, z+1; (xi) x1/2, y+1/2, z+3/2; (xii) x, y+1/2, z; (xiii) x+1, y1/2, z+1; (xiv) x, y+1, z; (xv) x+3/2, y1/2, z+1/2; (xvi) x+1/2, y, z+3/2; (xvii) x, y1, z; (xviii) x, y1/2, z; (xix) x+3/2, y, z1/2; (xx) x+3/2, y+1, z1/2.
 

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