The structure refined as (H
3O)
+·{[(C
10H
8N
2)V(O)O]
2(AsO
4)}
−·H
2O by Zheng, Zhang & Yang [
Solid State Sci. (2005),
7, 149–154] has been reformulated as {[(C
10H
8N
2)V(=O)O]
2(HAsO
4)}·2H
2O or [V
2(HAsO
4)O
4(C
10H
8N
2)
2]·2H
2O, whose crystal structure features a disordered [HAsO
4]
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
CCDC reference: 643677
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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]·2H2O | F(000) = 1312 |
Mr = 654.21 | Dx = 1.561 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6142 reflections |
a = 13.867 (3) Å | θ = 2.5–28.3° |
b = 22.351 (2) Å | µ = 1.91 mm−1 |
c = 9.252 (5) Å | T = 293 K |
β = 103.857 (7)° | Prism, yellow |
V = 2784.1 (16) Å3 | 0.80 × 0.50 × 0.04 mm |
Z = 4 | |
Data collection top
Rigaku Mercury diffractometer | 3181 independent reflections |
Radiation source: large-focus sealed tube | 2919 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
ω scans | θmax = 27.5°, θmin = 2.6° |
Absorption correction: multi-scan Jacobson (1998) | h = −18→17 |
Tmin = 0.331, Tmax = 0.927 | k = −27→29 |
10588 measured reflections | l = −8→12 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.153 | H-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 parameters | Δρmax = 0.83 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
As1 | 0.0000 | 0.047237 (19) | 0.2500 | 0.0517 (2) | |
V1 | 0.11550 (4) | 0.17201 (2) | 0.25462 (5) | 0.03721 (18) | |
O1 | 0.2324 (2) | 0.16948 (12) | 0.3341 (3) | 0.0603 (7) | |
O2 | 0.05507 (18) | 0.18326 (11) | 0.3856 (2) | 0.0470 (5) | |
O3 | 0.09100 (17) | 0.08891 (9) | 0.2109 (3) | 0.0459 (5) | |
O4 | 0.0477 (3) | 0.00520 (17) | 0.3979 (5) | 0.1034 (14) | |
H4o | 0.0039 | 0.0004 | 0.4489 | 0.124* | 0.50 |
O1w | 0.2554 (6) | 0.0061 (4) | 0.5329 (11) | 0.124 (4) | 0.553 (9) |
H1w1 | 0.1918 | 0.0028 | 0.5010 | 0.149* | 0.553 (9) |
H1w2 | 0.2721 | −0.0156 | 0.6112 | 0.149* | 0.553 (9) |
O2w | 0.3339 (8) | −0.0581 (5) | 0.7853 (14) | 0.123 (4) | 0.447 (9) |
H2w1 | 0.3012 | −0.0902 | 0.7941 | 0.147* | 0.447 (9) |
H2w2 | 0.3361 | −0.0359 | 0.8610 | 0.147* | 0.447 (9) |
N1 | 0.1195 (2) | 0.26523 (12) | 0.2119 (3) | 0.0454 (6) | |
N2 | 0.12182 (19) | 0.18123 (12) | 0.0200 (3) | 0.0409 (5) | |
C1 | 0.1245 (3) | 0.30517 (17) | 0.3225 (5) | 0.0621 (10) | |
H1 | 0.1253 | 0.2914 | 0.4177 | 0.074* | |
C2 | 0.1283 (4) | 0.3659 (2) | 0.2985 (7) | 0.0837 (14) | |
H2 | 0.1339 | 0.3927 | 0.3771 | 0.100* | |
C3 | 0.1239 (4) | 0.3861 (2) | 0.1589 (7) | 0.0908 (16) | |
H3 | 0.1229 | 0.4270 | 0.1398 | 0.109* | |
C4 | 0.1207 (3) | 0.34524 (19) | 0.0442 (6) | 0.0726 (12) | |
H4 | 0.1189 | 0.3585 | −0.0517 | 0.087* | |
C5 | 0.1204 (2) | 0.28491 (15) | 0.0744 (4) | 0.0482 (7) | |
C6 | 0.1224 (2) | 0.23723 (16) | −0.0339 (3) | 0.0441 (7) | |
C7 | 0.1268 (3) | 0.2471 (2) | −0.1801 (4) | 0.0599 (10) | |
H7 | 0.1278 | 0.2859 | −0.2158 | 0.072* | |
C8 | 0.1296 (3) | 0.1992 (3) | −0.2716 (4) | 0.0732 (13) | |
H8 | 0.1345 | 0.2051 | −0.3691 | 0.088* | |
C9 | 0.1252 (3) | 0.1437 (2) | −0.2185 (4) | 0.0681 (12) | |
H9 | 0.1240 | 0.1108 | −0.2807 | 0.082* | |
C10 | 0.1225 (3) | 0.13518 (18) | −0.0709 (4) | 0.0546 (8) | |
H10 | 0.1211 | 0.0964 | −0.0347 | 0.065* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
As1 | 0.0730 (4) | 0.0292 (3) | 0.0655 (4) | 0.000 | 0.0417 (3) | 0.000 |
V1 | 0.0491 (3) | 0.0381 (3) | 0.0259 (3) | −0.00343 (19) | 0.0119 (2) | 0.00240 (16) |
O1 | 0.0559 (15) | 0.0642 (17) | 0.0577 (15) | −0.0068 (11) | 0.0071 (11) | 0.0121 (12) |
O2 | 0.0649 (14) | 0.0522 (13) | 0.0271 (10) | −0.0066 (10) | 0.0169 (9) | −0.0014 (8) |
O3 | 0.0575 (12) | 0.0347 (11) | 0.0525 (13) | 0.0018 (9) | 0.0268 (10) | 0.0026 (9) |
O4 | 0.118 (3) | 0.095 (3) | 0.123 (3) | 0.052 (2) | 0.078 (2) | 0.072 (2) |
O1w | 0.112 (6) | 0.087 (5) | 0.151 (8) | −0.028 (4) | −0.014 (5) | 0.004 (5) |
O2w | 0.115 (8) | 0.117 (8) | 0.142 (9) | −0.071 (6) | 0.042 (6) | −0.006 (6) |
N1 | 0.0555 (15) | 0.0394 (13) | 0.0430 (14) | −0.0079 (11) | 0.0150 (11) | −0.0003 (10) |
N2 | 0.0449 (13) | 0.0498 (14) | 0.0314 (12) | −0.0068 (10) | 0.0156 (10) | 0.0006 (10) |
C1 | 0.079 (3) | 0.050 (2) | 0.061 (2) | −0.0144 (18) | 0.0245 (18) | −0.0140 (16) |
C2 | 0.104 (3) | 0.048 (2) | 0.107 (4) | −0.020 (2) | 0.043 (3) | −0.026 (2) |
C3 | 0.107 (4) | 0.040 (2) | 0.127 (5) | −0.009 (2) | 0.031 (3) | 0.003 (2) |
C4 | 0.081 (3) | 0.055 (2) | 0.080 (3) | −0.008 (2) | 0.017 (2) | 0.026 (2) |
C5 | 0.0439 (15) | 0.0489 (18) | 0.0517 (18) | −0.0086 (13) | 0.0113 (13) | 0.0117 (14) |
C6 | 0.0370 (13) | 0.0604 (19) | 0.0345 (14) | −0.0106 (13) | 0.0076 (11) | 0.0095 (13) |
C7 | 0.0481 (17) | 0.091 (3) | 0.0387 (17) | −0.0173 (18) | 0.0062 (13) | 0.0195 (17) |
C8 | 0.059 (2) | 0.135 (4) | 0.0265 (15) | −0.023 (2) | 0.0114 (14) | 0.004 (2) |
C9 | 0.066 (2) | 0.102 (3) | 0.0413 (18) | −0.020 (2) | 0.0231 (16) | −0.025 (2) |
C10 | 0.0593 (19) | 0.066 (2) | 0.0442 (17) | −0.0071 (16) | 0.0233 (14) | −0.0121 (15) |
Geometric parameters (Å, º) top
As1—O3 | 1.676 (2) | N2—C6 | 1.348 (4) |
As1—O4i | 1.662 (3) | C1—C2 | 1.379 (6) |
As1—O4 | 1.662 (3) | C1—H1 | 0.9300 |
As1—O3i | 1.676 (2) | C2—C3 | 1.356 (8) |
V1—O1 | 1.612 (3) | C2—H2 | 0.9300 |
V1—O2 | 1.650 (2) | C3—C4 | 1.394 (8) |
V1—O2i | 2.423 (2) | C3—H3 | 0.9300 |
V1—O3 | 1.914 (2) | C4—C5 | 1.377 (5) |
V1—N1 | 2.124 (3) | C4—H4 | 0.9300 |
V1—N2 | 2.203 (3) | C5—C6 | 1.467 (5) |
O4—H4o | 0.86 | C6—C7 | 1.385 (4) |
O1w—H1w1 | 0.86 | C7—C8 | 1.371 (7) |
O1w—H1w2 | 0.86 | C7—H7 | 0.9300 |
O2w—H2w1 | 0.86 | C8—C9 | 1.341 (7) |
O2w—H2w2 | 0.85 | C8—H8 | 0.9300 |
N1—C1 | 1.348 (5) | C9—C10 | 1.389 (5) |
N1—C5 | 1.349 (4) | C9—H9 | 0.9300 |
N2—C10 | 1.330 (4) | C10—H10 | 0.9300 |
| | | |
O4i—As1—O4 | 111.1 (3) | C6—N2—V1 | 117.2 (2) |
O4i—As1—O3i | 108.67 (16) | N1—C1—C2 | 121.8 (4) |
O4—As1—O3i | 107.96 (14) | N1—C1—H1 | 119.1 |
O4i—As1—O3 | 107.96 (14) | C2—C1—H1 | 119.1 |
O4—As1—O3 | 108.67 (16) | C3—C2—C1 | 119.1 (4) |
O3i—As1—O3 | 112.49 (15) | C3—C2—H2 | 120.4 |
O1—V1—O2 | 107.59 (14) | C1—C2—H2 | 120.4 |
O1—V1—O3 | 99.81 (12) | C2—C3—C4 | 119.6 (4) |
O2—V1—O3 | 101.98 (11) | C2—C3—H3 | 120.2 |
O1—V1—N1 | 92.93 (12) | C4—C3—H3 | 120.2 |
O2—V1—N1 | 91.60 (12) | C5—C4—C3 | 119.3 (4) |
O3—V1—N1 | 157.49 (11) | C5—C4—H4 | 120.4 |
O1—V1—N2 | 100.37 (13) | C3—C4—H4 | 120.4 |
O2—V1—N2 | 148.97 (11) | N1—C5—C4 | 120.8 (4) |
O3—V1—N2 | 85.94 (10) | N1—C5—C6 | 114.4 (3) |
N1—V1—N2 | 73.49 (10) | C4—C5—C6 | 124.8 (4) |
O1—V1—O2i | 173.48 (11) | N2—C6—C7 | 120.9 (3) |
O2—V1—O2i | 77.01 (10) | N2—C6—C5 | 114.8 (3) |
O3—V1—O2i | 83.47 (9) | C7—C6—C5 | 124.3 (3) |
N1—V1—O2i | 82.20 (10) | C8—C7—C6 | 119.5 (4) |
N2—V1—O2i | 74.14 (9) | C8—C7—H7 | 120.2 |
V1—O2—V1i | 101.14 (10) | C6—C7—H7 | 120.2 |
As1—O3—V1 | 126.74 (13) | C9—C8—C7 | 119.1 (3) |
As1—O4—H4o | 109.1 | C9—C8—H8 | 120.5 |
H1w1—O1w—H1w2 | 106.7 | C7—C8—H8 | 120.5 |
H2w1—O2w—H2w2 | 108.9 | C8—C9—C10 | 120.0 (4) |
C1—N1—C5 | 119.4 (3) | C8—C9—H9 | 120.0 |
C1—N1—V1 | 120.5 (3) | C10—C9—H9 | 120.0 |
C5—N1—V1 | 120.1 (2) | N2—C10—C9 | 121.5 (4) |
C10—N2—C6 | 118.9 (3) | N2—C10—H10 | 119.3 |
C10—N2—V1 | 123.9 (2) | C9—C10—H10 | 119.3 |
| | | |
O1—V1—O2—V1i | −172.77 (11) | O3—V1—N2—C6 | 169.1 (2) |
O3—V1—O2—V1i | −68.29 (11) | N1—V1—N2—C6 | −1.6 (2) |
N1—V1—O2—V1i | 93.65 (11) | O2i—V1—N2—C6 | 84.8 (2) |
N2—V1—O2—V1i | 34.0 (2) | C5—N1—C1—C2 | 1.4 (6) |
O2i—V1—O2—V1i | 12.03 (11) | V1—N1—C1—C2 | 179.2 (4) |
O4i—As1—O3—V1 | 136.6 (2) | N1—C1—C2—C3 | 2.1 (8) |
O4—As1—O3—V1 | −102.7 (2) | C1—C2—C3—C4 | −3.4 (8) |
O3i—As1—O3—V1 | 16.73 (10) | C2—C3—C4—C5 | 1.2 (8) |
O1—V1—O3—As1 | 129.88 (18) | C1—N1—C5—C4 | −3.7 (5) |
O2—V1—O3—As1 | 19.39 (19) | V1—N1—C5—C4 | 178.5 (3) |
N1—V1—O3—As1 | −106.5 (3) | C1—N1—C5—C6 | 175.6 (3) |
N2—V1—O3—As1 | −130.28 (17) | V1—N1—C5—C6 | −2.3 (4) |
O2i—V1—O3—As1 | −55.81 (16) | C3—C4—C5—N1 | 2.4 (6) |
O1—V1—N1—C1 | −75.7 (3) | C3—C4—C5—C6 | −176.7 (4) |
O2—V1—N1—C1 | 32.0 (3) | C10—N2—C6—C7 | −2.0 (4) |
O3—V1—N1—C1 | 159.5 (3) | V1—N2—C6—C7 | 179.7 (2) |
N2—V1—N1—C1 | −175.7 (3) | C10—N2—C6—C5 | 179.3 (3) |
O2i—V1—N1—C1 | 108.6 (3) | V1—N2—C6—C5 | 1.0 (3) |
O1—V1—N1—C5 | 102.1 (3) | N1—C5—C6—N2 | 0.7 (4) |
O2—V1—N1—C5 | −150.2 (3) | C4—C5—C6—N2 | 179.9 (3) |
O3—V1—N1—C5 | −22.7 (5) | N1—C5—C6—C7 | −177.8 (3) |
N2—V1—N1—C5 | 2.1 (2) | C4—C5—C6—C7 | 1.3 (5) |
O2i—V1—N1—C5 | −73.6 (3) | N2—C6—C7—C8 | 0.7 (5) |
O1—V1—N2—C10 | 90.1 (3) | C5—C6—C7—C8 | 179.1 (3) |
O2—V1—N2—C10 | −115.7 (3) | C6—C7—C8—C9 | 1.8 (6) |
O3—V1—N2—C10 | −9.1 (3) | C7—C8—C9—C10 | −2.9 (6) |
N1—V1—N2—C10 | −179.8 (3) | C6—N2—C10—C9 | 1.0 (5) |
O2i—V1—N2—C10 | −93.5 (3) | V1—N2—C10—C9 | 179.1 (3) |
O1—V1—N2—C6 | −91.6 (2) | C8—C9—C10—N2 | 1.6 (6) |
O2—V1—N2—C6 | 62.5 (3) | | |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4o···O4ii | 0.86 | 1.74 | 2.564 (7) | 160 |
O1w—H1w1···O4 | 0.86 | 2.00 | 2.851 (9) | 170 |
O2w—H2w1···O1iii | 0.86 | 2.09 | 2.948 (9) | 175 |
Symmetry codes: (ii) −x, −y, −z+1; (iii) x, −y, z+1/2. |