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The structure refined as (H3O)+·{[(C10H8N2)V(O)O]2(AsO4)}·H2O by Zheng, Zhang & Yang [Solid State Sci. (2005), 7, 149–154] has been reformulated as {[(C10H8N2)V(=O)O]2(HAsO4)}·2H2O or [V2(HAsO4)O4(C10H8N2)2]·2H2O, whose crystal structure features a disordered [HAsO4]2− group that links the dinuclear mol­ecules, through O–H...O hydrogen bonds, into a chain running along the a axis. A crystallographic twofold rotation axis passes through the As atom.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680701241X/xu2220sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680701241X/xu2220Isup2.hkl
Contains datablock I

CCDC reference: 643677

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in solvent or counterion
  • R factor = 0.047
  • wR factor = 0.153
  • Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor >O1W - >H1W2 ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.80 mm PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for As1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 66.00 A   3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: atomic coordinates from published structure; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

µ-Hydrogenarsenato-κ2O:O'-di-µ-oxo-κ2O:O'-bis[(2,2'-bipyridine- κ2N,N')vanadium(V)] dihydrate top
Crystal data top
[V2(HAsO4)O4(C10H8N2)2]·2H2OF(000) = 1312
Mr = 654.21Dx = 1.561 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6142 reflections
a = 13.867 (3) Åθ = 2.5–28.3°
b = 22.351 (2) ŵ = 1.91 mm1
c = 9.252 (5) ÅT = 293 K
β = 103.857 (7)°Prism, yellow
V = 2784.1 (16) Å30.80 × 0.50 × 0.04 mm
Z = 4
Data collection top
Rigaku Mercury
diffractometer
3181 independent reflections
Radiation source: large-focus sealed tube2919 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ω scansθmax = 27.5°, θmin = 2.6°
Absorption correction: multi-scan
Jacobson (1998)
h = 1817
Tmin = 0.331, Tmax = 0.927k = 2729
10588 measured reflectionsl = 812
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.153H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0971P)2 + 1.5523P]
where P = (Fo2 + 2Fc2)/3
3181 reflections(Δ/σ)max = 0.001
178 parametersΔρmax = 0.83 e Å3
0 restraintsΔρmin = 0.49 e Å3
Special details top

Experimental. A large-focus collimator was used on the diffractometer.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
As10.00000.047237 (19)0.25000.0517 (2)
V10.11550 (4)0.17201 (2)0.25462 (5)0.03721 (18)
O10.2324 (2)0.16948 (12)0.3341 (3)0.0603 (7)
O20.05507 (18)0.18326 (11)0.3856 (2)0.0470 (5)
O30.09100 (17)0.08891 (9)0.2109 (3)0.0459 (5)
O40.0477 (3)0.00520 (17)0.3979 (5)0.1034 (14)
H4o0.00390.00040.44890.124*0.50
O1w0.2554 (6)0.0061 (4)0.5329 (11)0.124 (4)0.553 (9)
H1w10.19180.00280.50100.149*0.553 (9)
H1w20.27210.01560.61120.149*0.553 (9)
O2w0.3339 (8)0.0581 (5)0.7853 (14)0.123 (4)0.447 (9)
H2w10.30120.09020.79410.147*0.447 (9)
H2w20.33610.03590.86100.147*0.447 (9)
N10.1195 (2)0.26523 (12)0.2119 (3)0.0454 (6)
N20.12182 (19)0.18123 (12)0.0200 (3)0.0409 (5)
C10.1245 (3)0.30517 (17)0.3225 (5)0.0621 (10)
H10.12530.29140.41770.074*
C20.1283 (4)0.3659 (2)0.2985 (7)0.0837 (14)
H20.13390.39270.37710.100*
C30.1239 (4)0.3861 (2)0.1589 (7)0.0908 (16)
H30.12290.42700.13980.109*
C40.1207 (3)0.34524 (19)0.0442 (6)0.0726 (12)
H40.11890.35850.05170.087*
C50.1204 (2)0.28491 (15)0.0744 (4)0.0482 (7)
C60.1224 (2)0.23723 (16)0.0339 (3)0.0441 (7)
C70.1268 (3)0.2471 (2)0.1801 (4)0.0599 (10)
H70.12780.28590.21580.072*
C80.1296 (3)0.1992 (3)0.2716 (4)0.0732 (13)
H80.13450.20510.36910.088*
C90.1252 (3)0.1437 (2)0.2185 (4)0.0681 (12)
H90.12400.11080.28070.082*
C100.1225 (3)0.13518 (18)0.0709 (4)0.0546 (8)
H100.12110.09640.03470.065*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.0730 (4)0.0292 (3)0.0655 (4)0.0000.0417 (3)0.000
V10.0491 (3)0.0381 (3)0.0259 (3)0.00343 (19)0.0119 (2)0.00240 (16)
O10.0559 (15)0.0642 (17)0.0577 (15)0.0068 (11)0.0071 (11)0.0121 (12)
O20.0649 (14)0.0522 (13)0.0271 (10)0.0066 (10)0.0169 (9)0.0014 (8)
O30.0575 (12)0.0347 (11)0.0525 (13)0.0018 (9)0.0268 (10)0.0026 (9)
O40.118 (3)0.095 (3)0.123 (3)0.052 (2)0.078 (2)0.072 (2)
O1w0.112 (6)0.087 (5)0.151 (8)0.028 (4)0.014 (5)0.004 (5)
O2w0.115 (8)0.117 (8)0.142 (9)0.071 (6)0.042 (6)0.006 (6)
N10.0555 (15)0.0394 (13)0.0430 (14)0.0079 (11)0.0150 (11)0.0003 (10)
N20.0449 (13)0.0498 (14)0.0314 (12)0.0068 (10)0.0156 (10)0.0006 (10)
C10.079 (3)0.050 (2)0.061 (2)0.0144 (18)0.0245 (18)0.0140 (16)
C20.104 (3)0.048 (2)0.107 (4)0.020 (2)0.043 (3)0.026 (2)
C30.107 (4)0.040 (2)0.127 (5)0.009 (2)0.031 (3)0.003 (2)
C40.081 (3)0.055 (2)0.080 (3)0.008 (2)0.017 (2)0.026 (2)
C50.0439 (15)0.0489 (18)0.0517 (18)0.0086 (13)0.0113 (13)0.0117 (14)
C60.0370 (13)0.0604 (19)0.0345 (14)0.0106 (13)0.0076 (11)0.0095 (13)
C70.0481 (17)0.091 (3)0.0387 (17)0.0173 (18)0.0062 (13)0.0195 (17)
C80.059 (2)0.135 (4)0.0265 (15)0.023 (2)0.0114 (14)0.004 (2)
C90.066 (2)0.102 (3)0.0413 (18)0.020 (2)0.0231 (16)0.025 (2)
C100.0593 (19)0.066 (2)0.0442 (17)0.0071 (16)0.0233 (14)0.0121 (15)
Geometric parameters (Å, º) top
As1—O31.676 (2)N2—C61.348 (4)
As1—O4i1.662 (3)C1—C21.379 (6)
As1—O41.662 (3)C1—H10.9300
As1—O3i1.676 (2)C2—C31.356 (8)
V1—O11.612 (3)C2—H20.9300
V1—O21.650 (2)C3—C41.394 (8)
V1—O2i2.423 (2)C3—H30.9300
V1—O31.914 (2)C4—C51.377 (5)
V1—N12.124 (3)C4—H40.9300
V1—N22.203 (3)C5—C61.467 (5)
O4—H4o0.86C6—C71.385 (4)
O1w—H1w10.86C7—C81.371 (7)
O1w—H1w20.86C7—H70.9300
O2w—H2w10.86C8—C91.341 (7)
O2w—H2w20.85C8—H80.9300
N1—C11.348 (5)C9—C101.389 (5)
N1—C51.349 (4)C9—H90.9300
N2—C101.330 (4)C10—H100.9300
O4i—As1—O4111.1 (3)C6—N2—V1117.2 (2)
O4i—As1—O3i108.67 (16)N1—C1—C2121.8 (4)
O4—As1—O3i107.96 (14)N1—C1—H1119.1
O4i—As1—O3107.96 (14)C2—C1—H1119.1
O4—As1—O3108.67 (16)C3—C2—C1119.1 (4)
O3i—As1—O3112.49 (15)C3—C2—H2120.4
O1—V1—O2107.59 (14)C1—C2—H2120.4
O1—V1—O399.81 (12)C2—C3—C4119.6 (4)
O2—V1—O3101.98 (11)C2—C3—H3120.2
O1—V1—N192.93 (12)C4—C3—H3120.2
O2—V1—N191.60 (12)C5—C4—C3119.3 (4)
O3—V1—N1157.49 (11)C5—C4—H4120.4
O1—V1—N2100.37 (13)C3—C4—H4120.4
O2—V1—N2148.97 (11)N1—C5—C4120.8 (4)
O3—V1—N285.94 (10)N1—C5—C6114.4 (3)
N1—V1—N273.49 (10)C4—C5—C6124.8 (4)
O1—V1—O2i173.48 (11)N2—C6—C7120.9 (3)
O2—V1—O2i77.01 (10)N2—C6—C5114.8 (3)
O3—V1—O2i83.47 (9)C7—C6—C5124.3 (3)
N1—V1—O2i82.20 (10)C8—C7—C6119.5 (4)
N2—V1—O2i74.14 (9)C8—C7—H7120.2
V1—O2—V1i101.14 (10)C6—C7—H7120.2
As1—O3—V1126.74 (13)C9—C8—C7119.1 (3)
As1—O4—H4o109.1C9—C8—H8120.5
H1w1—O1w—H1w2106.7C7—C8—H8120.5
H2w1—O2w—H2w2108.9C8—C9—C10120.0 (4)
C1—N1—C5119.4 (3)C8—C9—H9120.0
C1—N1—V1120.5 (3)C10—C9—H9120.0
C5—N1—V1120.1 (2)N2—C10—C9121.5 (4)
C10—N2—C6118.9 (3)N2—C10—H10119.3
C10—N2—V1123.9 (2)C9—C10—H10119.3
O1—V1—O2—V1i172.77 (11)O3—V1—N2—C6169.1 (2)
O3—V1—O2—V1i68.29 (11)N1—V1—N2—C61.6 (2)
N1—V1—O2—V1i93.65 (11)O2i—V1—N2—C684.8 (2)
N2—V1—O2—V1i34.0 (2)C5—N1—C1—C21.4 (6)
O2i—V1—O2—V1i12.03 (11)V1—N1—C1—C2179.2 (4)
O4i—As1—O3—V1136.6 (2)N1—C1—C2—C32.1 (8)
O4—As1—O3—V1102.7 (2)C1—C2—C3—C43.4 (8)
O3i—As1—O3—V116.73 (10)C2—C3—C4—C51.2 (8)
O1—V1—O3—As1129.88 (18)C1—N1—C5—C43.7 (5)
O2—V1—O3—As119.39 (19)V1—N1—C5—C4178.5 (3)
N1—V1—O3—As1106.5 (3)C1—N1—C5—C6175.6 (3)
N2—V1—O3—As1130.28 (17)V1—N1—C5—C62.3 (4)
O2i—V1—O3—As155.81 (16)C3—C4—C5—N12.4 (6)
O1—V1—N1—C175.7 (3)C3—C4—C5—C6176.7 (4)
O2—V1—N1—C132.0 (3)C10—N2—C6—C72.0 (4)
O3—V1—N1—C1159.5 (3)V1—N2—C6—C7179.7 (2)
N2—V1—N1—C1175.7 (3)C10—N2—C6—C5179.3 (3)
O2i—V1—N1—C1108.6 (3)V1—N2—C6—C51.0 (3)
O1—V1—N1—C5102.1 (3)N1—C5—C6—N20.7 (4)
O2—V1—N1—C5150.2 (3)C4—C5—C6—N2179.9 (3)
O3—V1—N1—C522.7 (5)N1—C5—C6—C7177.8 (3)
N2—V1—N1—C52.1 (2)C4—C5—C6—C71.3 (5)
O2i—V1—N1—C573.6 (3)N2—C6—C7—C80.7 (5)
O1—V1—N2—C1090.1 (3)C5—C6—C7—C8179.1 (3)
O2—V1—N2—C10115.7 (3)C6—C7—C8—C91.8 (6)
O3—V1—N2—C109.1 (3)C7—C8—C9—C102.9 (6)
N1—V1—N2—C10179.8 (3)C6—N2—C10—C91.0 (5)
O2i—V1—N2—C1093.5 (3)V1—N2—C10—C9179.1 (3)
O1—V1—N2—C691.6 (2)C8—C9—C10—N21.6 (6)
O2—V1—N2—C662.5 (3)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4o···O4ii0.861.742.564 (7)160
O1w—H1w1···O40.862.002.851 (9)170
O2w—H2w1···O1iii0.862.092.948 (9)175
Symmetry codes: (ii) x, y, z+1; (iii) x, y, z+1/2.
 

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