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The title compound, trisodium vanadium oxide tri­sulfide, has been synthesized by the reaction of the elements in an Li2O/Na2S flux at 723 K. The structure comprises isolated tetrahedral VOS33- anions separated by Na+ cations. The anion has symmetry m. Bond distances include V-O = 1.673 (2) Å, and V-S = 2.1746 (4) and 2.1971 (6) Å. Each Na+ cation is coordinated in a distorted octahedron by one O and five S atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803028939/wm6005sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803028939/wm6005Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](V-O) = 0.003 Å
  • R factor = 0.017
  • wR factor = 0.044
  • Data-to-parameter ratio = 19.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 PLAT031_ALERT_4_B Refined Extinction Parameter within Range ...... 1.80 Sigma
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.79 From the CIF: _reflns_number_total 872 Count of symmetry unique reflns 507 Completeness (_total/calc) 171.99% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 365 Fraction of Friedel pairs measured 0.720 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXTL.

Trisodium vanadium oxide trisulfide top
Crystal data top
Na3(VOS3)F(000) = 448
Mr = 232.09Dx = 2.275 Mg m3
Orthorhombic, Cmc21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2Cell parameters from 3805 reflections
a = 9.6673 (11) Åθ = 2.7–28.8°
b = 11.9122 (14) ŵ = 2.47 mm1
c = 5.8846 (7) ÅT = 153 K
V = 677.66 (14) Å3Flat needle, red
Z = 40.58 × 0.16 × 0.04 mm
Data collection top
Bruker SMART-1000 CCD
diffractometer
872 independent reflections
Radiation source: fine-focus sealed tube867 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
0.3° ω scansθmax = 28.8°, θmin = 2.7°
Absorption correction: integration
(XPREP; Sheldrick, 2000)
h = 1212
Tmin = 0.337, Tmax = 0.902k = 1515
3902 measured reflectionsl = 77
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.03P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.017(Δ/σ)max = 0.006
wR(F2) = 0.044Δρmax = 0.65 e Å3
S = 1.15Δρmin = 0.37 e Å3
872 reflectionsExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
44 parametersExtinction coefficient: 0.0009 (5)
0 restraintsAbsolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.21 (2)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Na11.00000.88164 (8)1.00000.0152 (2)
Na20.79336 (7)0.61995 (5)0.98035 (19)0.01556 (15)
V1.00000.70360 (2)0.5789 (2)0.00851 (10)
S11.00000.88180 (4)0.48267 (19)0.01130 (12)
S20.68988 (4)0.87609 (3)0.9639 (2)0.01272 (11)
O1.00000.69877 (12)0.8630 (4)0.0112 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0194 (5)0.0116 (4)0.0146 (5)0.0000.0000.0023 (3)
Na20.0133 (3)0.0185 (3)0.0149 (3)0.0016 (2)0.0021 (3)0.0004 (3)
V0.00835 (15)0.00893 (17)0.00826 (17)0.0000.0000.00038 (13)
S10.0106 (2)0.0093 (2)0.0140 (2)0.0000.0000.00230 (18)
S20.01136 (19)0.01397 (19)0.0128 (2)0.00304 (11)0.00159 (14)0.00061 (12)
O0.0110 (7)0.0142 (9)0.0085 (8)0.0000.0000.0011 (5)
Geometric parameters (Å, º) top
Na1—O2.3228 (19)Na2—Na2iii3.9952 (14)
Na1—S1i2.8198 (10)Na2—Na1viii4.0042 (10)
Na1—S1ii2.8403 (12)Na2—Na1ix4.0144 (10)
Na1—S2iii3.0063 (5)V—O1.6726 (18)
Na1—S23.0063 (5)V—S2viii2.1746 (4)
Na1—S13.0443 (12)V—S2x2.1746 (4)
Na1—V3.2616 (11)V—S12.1971 (6)
Na1—Na23.7042 (11)V—Na2iii3.2501 (8)
Na1—Na2iii3.7042 (11)V—Na2x3.5774 (7)
Na1—Na2iv4.0042 (10)V—Na2viii3.5774 (7)
Na1—Na2v4.0042 (10)S1—Na1xi2.8198 (10)
Na1—Na2vi4.0144 (10)S1—Na2x2.8361 (7)
Na2—O2.3128 (10)S1—Na2viii2.8361 (8)
Na2—S1v2.8361 (7)S1—Na1xii2.8403 (12)
Na2—S2v2.8504 (9)S2—Vv2.1746 (4)
Na2—S2vii2.9111 (7)S2—Na2viii2.8504 (9)
Na2—S2viii3.0439 (9)S2—Na2xiii2.9111 (7)
Na2—S23.2125 (7)S2—Na2v3.0439 (9)
Na2—V3.2501 (8)O—Na2iii2.3128 (10)
Na2—Vv3.5774 (7)
O—Na1—S1i157.62 (7)O—Na2—Na2iii30.26 (4)
O—Na1—S1ii110.35 (6)S1v—Na2—Na2iii179.496 (17)
S1i—Na1—S1ii92.03 (3)S2v—Na2—Na2iii86.742 (16)
O—Na1—S2iii87.411 (19)S2vii—Na2—Na2iii86.810 (16)
S1i—Na1—S2iii91.113 (19)S2viii—Na2—Na2iii86.949 (15)
S1ii—Na1—S2iii94.06 (2)S2—Na2—Na2iii108.145 (13)
O—Na1—S287.411 (19)V—Na2—Na2iii52.075 (15)
S1i—Na1—S291.113 (19)Vv—Na2—Na2iii142.445 (11)
S1ii—Na1—S294.06 (2)Na1—Na2—Na2iii57.365 (14)
S2iii—Na1—S2171.51 (4)O—Na2—Na1viii113.76 (4)
O—Na1—S169.72 (5)S1v—Na2—Na1viii45.18 (2)
S1i—Na1—S187.89 (3)S2v—Na2—Na1viii138.16 (3)
S1ii—Na1—S1179.93 (4)S2vii—Na2—Na1viii90.64 (2)
S2iii—Na1—S185.95 (2)S2viii—Na2—Na1viii48.158 (16)
S2—Na1—S185.95 (2)S2—Na2—Na1viii76.27 (2)
O—Na1—V29.13 (5)V—Na2—Na1viii85.62 (2)
S1i—Na1—V128.49 (4)Vv—Na2—Na1viii63.63 (2)
S1ii—Na1—V139.48 (4)Na1—Na2—Na1viii114.08 (2)
S2iii—Na1—V86.10 (2)Na2iii—Na2—Na1viii135.094 (14)
S2—Na1—V86.10 (2)O—Na2—Na1ix154.94 (4)
S1—Na1—V40.597 (18)S1v—Na2—Na1ix44.620 (14)
O—Na1—Na236.86 (2)S2v—Na2—Na1ix91.32 (2)
S1i—Na1—Na2147.126 (14)S2vii—Na2—Na1ix48.287 (17)
S1ii—Na1—Na291.82 (3)S2viii—Na2—Na1ix94.43 (2)
S2iii—Na1—Na2121.14 (3)S2—Na2—Na1ix116.91 (2)
S2—Na1—Na256.047 (15)V—Na2—Na1ix132.22 (2)
S1—Na1—Na288.24 (2)Vv—Na2—Na1ix81.417 (19)
V—Na1—Na255.184 (18)Na1—Na2—Na1ix167.21 (3)
O—Na1—Na2iii36.86 (2)Na2iii—Na2—Na1ix134.948 (14)
S1i—Na1—Na2iii147.126 (15)Na1viii—Na2—Na1ix61.093 (19)
S1ii—Na1—Na2iii91.82 (3)O—V—S2viii107.23 (3)
S2iii—Na1—Na2iii56.047 (15)O—V—S2x107.23 (3)
S2—Na1—Na2iii121.14 (3)S2viii—V—S2x115.15 (2)
S1—Na1—Na2iii88.24 (2)O—V—S1106.91 (5)
V—Na1—Na2iii55.184 (18)S2viii—V—S1109.968 (17)
Na2—Na1—Na2iii65.27 (3)S2x—V—S1109.968 (17)
O—Na1—Na2iv103.92 (4)O—V—Na2iii42.53 (3)
S1i—Na1—Na2iv91.73 (2)S2viii—V—Na2iii127.68 (2)
S1ii—Na1—Na2iv45.096 (15)S2x—V—Na2iii64.763 (17)
S2iii—Na1—Na2iv48.966 (17)S1—V—Na2iii118.920 (19)
S2—Na1—Na2iv139.12 (3)O—V—Na242.53 (3)
S1—Na1—Na2iv134.905 (15)S2viii—V—Na264.763 (17)
V—Na1—Na2iv122.223 (19)S2x—V—Na2127.68 (2)
Na2—Na1—Na2iv113.58 (3)S1—V—Na2118.920 (19)
Na2iii—Na1—Na2iv68.659 (16)Na2iii—V—Na275.85 (3)
O—Na1—Na2v103.92 (4)O—V—Na142.53 (6)
S1i—Na1—Na2v91.74 (2)S2viii—V—Na1121.357 (14)
S1ii—Na1—Na2v45.096 (15)S2x—V—Na1121.357 (14)
S2iii—Na1—Na2v139.12 (3)S1—V—Na164.38 (2)
S2—Na1—Na2v48.966 (17)Na2iii—V—Na169.34 (2)
S1—Na1—Na2v134.905 (15)Na2—V—Na169.34 (2)
V—Na1—Na2v122.223 (19)O—V—Na2x100.50 (3)
Na2—Na1—Na2v68.659 (16)S2viii—V—Na2x151.07 (2)
Na2iii—Na1—Na2v113.58 (3)S2x—V—Na2x62.407 (16)
Na2iv—Na1—Na2v90.19 (3)S1—V—Na2x52.447 (11)
O—Na1—Na2vi130.78 (3)Na2iii—V—Na2x79.089 (15)
S1i—Na1—Na2vi44.949 (14)Na2—V—Na2x141.74 (3)
S1ii—Na1—Na2vi91.62 (2)Na1—V—Na2x74.996 (16)
S2iii—Na1—Na2vi46.290 (14)O—V—Na2viii100.50 (3)
S2—Na1—Na2vi135.89 (3)S2viii—V—Na2viii62.407 (16)
S1—Na1—Na2vi88.32 (2)S2x—V—Na2viii151.07 (2)
V—Na1—Na2vi115.97 (2)S1—V—Na2viii52.447 (11)
Na2—Na1—Na2vi167.21 (3)Na2iii—V—Na2viii141.74 (3)
Na2iii—Na1—Na2vi102.311 (9)Na2—V—Na2viii79.089 (15)
Na2iv—Na1—Na2vi61.531 (16)Na1—V—Na2viii74.996 (16)
Na2v—Na1—Na2vi121.60 (3)Na2x—V—Na2viii104.89 (2)
O—Na2—S1v150.24 (4)V—S1—Na1xi162.99 (3)
O—Na2—S2v104.02 (5)V—S1—Na2x89.663 (16)
S1v—Na2—S2v92.99 (2)Na1xi—S1—Na2x90.432 (15)
O—Na2—S2vii110.31 (4)V—S1—Na2viii89.663 (16)
S1v—Na2—S2vii92.78 (2)Na1xi—S1—Na2viii90.432 (15)
S2v—Na2—S2vii92.67 (2)Na2x—S1—Na2viii178.99 (3)
O—Na2—S2viii69.49 (5)V—S1—Na1xii104.90 (3)
S1v—Na2—S2viii93.33 (2)Na1xi—S1—Na1xii92.11 (3)
S2v—Na2—S2viii173.43 (3)Na2x—S1—Na1xii89.725 (18)
S2vii—Na2—S2viii88.81 (2)Na2viii—S1—Na1xii89.725 (18)
O—Na2—S282.78 (4)V—S1—Na175.02 (3)
S1v—Na2—S272.286 (19)Na1xi—S1—Na187.96 (3)
S2v—Na2—S291.84 (2)Na2x—S1—Na190.275 (18)
S2vii—Na2—S2164.61 (3)Na2viii—S1—Na190.275 (18)
S2viii—Na2—S288.38 (2)Na1xii—S1—Na1179.93 (4)
O—Na2—V29.27 (4)Vv—S2—Na2viii111.47 (2)
S1v—Na2—V128.34 (3)Vv—S2—Na2xiii118.18 (2)
S2v—Na2—V133.28 (3)Na2viii—S2—Na2xiii90.78 (2)
S2vii—Na2—V104.33 (2)Vv—S2—Na1146.04 (3)
S2viii—Na2—V40.257 (14)Na2viii—S2—Na190.78 (3)
S2—Na2—V83.010 (16)Na2xiii—S2—Na185.42 (2)
O—Na2—Vv119.64 (4)Vv—S2—Na2v74.980 (19)
S1v—Na2—Vv37.890 (14)Na2viii—S2—Na2v173.43 (3)
S2v—Na2—Vv82.73 (2)Na2xiii—S2—Na2v87.04 (2)
S2vii—Na2—Vv129.48 (2)Na1—S2—Na2v82.88 (3)
S2viii—Na2—Vv101.24 (2)Vv—S2—Na280.728 (18)
S2—Na2—Vv36.865 (11)Na2viii—S2—Na291.61 (2)
V—Na2—Vv115.15 (2)Na2xiii—S2—Na2158.350 (15)
O—Na2—Na137.05 (4)Na1—S2—Na273.03 (2)
S1v—Na2—Na1123.05 (2)Na2v—S2—Na288.17 (2)
S2v—Na2—Na185.66 (2)V—O—Na2iii108.20 (5)
S2vii—Na2—Na1144.17 (3)V—O—Na2108.20 (5)
S2viii—Na2—Na189.39 (2)Na2iii—O—Na2119.47 (7)
S2—Na2—Na150.919 (15)V—O—Na1108.34 (8)
V—Na2—Na155.475 (19)Na2iii—O—Na1106.09 (5)
Vv—Na2—Na185.872 (18)Na2—O—Na1106.09 (5)
Symmetry codes: (i) x+2, y+2, z+1/2; (ii) x, y, z+1; (iii) x+2, y, z; (iv) x+1/2, y+3/2, z+1/2; (v) x+3/2, y+3/2, z+1/2; (vi) x+1/2, y+1/2, z; (vii) x+3/2, y1/2, z; (viii) x+3/2, y+3/2, z1/2; (ix) x1/2, y1/2, z; (x) x+1/2, y+3/2, z1/2; (xi) x+2, y+2, z1/2; (xii) x, y, z1; (xiii) x+3/2, y+1/2, z.
 

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