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The low-temperature study of the title compound, [V4O10(C12H8N2)2]n, confirms the P21/m space group revision made by Ng & Hu (2004) [J. Solid State Chem. 177, 1780]. Almost all atoms lie on mirror planes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045867/ng2140sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045867/ng2140Isup2.hkl
Contains datablock I

CCDC reference: 630183

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.030
  • wR factor = 0.081
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C 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 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.53 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 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 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXL97.

poly[hexa-µ2-oxo-tetraoxobis(1,10-phenanthroline)tetravanadium(V)] top
Crystal data top
[V4O10(C12H8N2)2]F(000) = 720
Mr = 724.16Dx = 1.933 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 3073 reflections
a = 9.8024 (7) Åθ = 2.1–27.5°
b = 6.5184 (4) ŵ = 1.53 mm1
c = 19.8144 (13) ÅT = 173 K
β = 100.650 (2)°Prism, red
V = 1244.25 (14) Å30.22 × 0.20 × 0.15 mm
Z = 2
Data collection top
Mercury70 (2x2 bin mode)
diffractometer
3094 independent reflections
Radiation source: fine-focus sealed tube2772 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 14.6306 pixels mm-1θmax = 27.5°, θmin = 2.1°
φ? ω? scansh = 1212
Absorption correction: empirical (using intensity measurements)
(XEMP in SHELXTL; Siemens, 1994)
k = 87
Tmin = 0.720, Tmax = 0.798l = 2425
9785 measured reflections
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0429P)2 + 0.7806P]
where P = (Fo2 + 2Fc2)/3
3094 reflections(Δ/σ)max = 0.001
247 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.40 e Å3
Special details top

Experimental. empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994)

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
V10.54868 (4)0.25000.36814 (2)0.01517 (11)
O10.4115 (2)0.25000.40075 (12)0.0295 (5)
N10.6806 (2)0.25000.46998 (11)0.0182 (4)
C10.8207 (3)0.25000.47340 (13)0.0176 (5)
V20.37288 (4)0.25000.19748 (2)0.01467 (11)
O20.4930 (2)0.25000.27640 (10)0.0260 (4)
N20.7754 (2)0.25000.35150 (11)0.0181 (4)
C20.9152 (3)0.25000.53598 (14)0.0229 (6)
V30.43421 (4)0.75000.15829 (2)0.01560 (11)
O30.58259 (14)0.5347 (2)0.37348 (7)0.0222 (3)
N30.1972 (2)0.75000.15286 (11)0.0190 (5)
C30.8595 (3)0.25000.59677 (15)0.0314 (7)
H30.91940.25000.64030.038*
V40.60000 (4)0.75000.32423 (2)0.01519 (11)
O40.2165 (2)0.25000.21176 (12)0.0370 (6)
N40.3372 (2)0.75000.04937 (11)0.0185 (5)
C40.7191 (4)0.25000.59265 (16)0.0364 (8)
H40.68060.25000.63330.044*
O50.40120 (14)0.4650 (2)0.15021 (7)0.0230 (3)
C50.6326 (3)0.25000.52838 (15)0.0280 (6)
H50.53500.25000.52630.034*
O60.5838 (2)0.75000.13736 (12)0.0323 (5)
C60.8713 (3)0.25000.40999 (13)0.0179 (5)
O70.4631 (2)0.75000.25048 (10)0.0237 (4)
C71.0156 (3)0.25000.41117 (15)0.0217 (6)
O80.7481 (2)0.75000.30000 (11)0.0329 (5)
C81.1095 (3)0.25000.47576 (16)0.0285 (7)
H81.20680.25000.47680.034*
C91.0607 (3)0.25000.53535 (15)0.0278 (6)
H91.12460.25000.57770.033*
C100.8201 (3)0.25000.29229 (15)0.0278 (6)
H100.75360.25000.25080.033*
C110.9611 (3)0.25000.28844 (16)0.0330 (7)
H110.98890.25000.24500.040*
C121.0582 (3)0.25000.34702 (17)0.0302 (7)
H121.15420.25000.34480.036*
C130.1304 (3)0.75000.20516 (16)0.0297 (7)
H130.18310.75000.25050.036*
C140.0147 (3)0.75000.19643 (19)0.0377 (8)
H140.05910.75000.23520.045*
C150.0912 (3)0.75000.1317 (2)0.0372 (8)
H150.18970.75000.12500.045*
C160.0242 (3)0.75000.07469 (17)0.0273 (6)
C170.1217 (3)0.75000.08863 (14)0.0187 (5)
C180.0949 (3)0.75000.00422 (19)0.0381 (8)
H180.19350.75000.00560.046*
C190.0250 (3)0.75000.04805 (18)0.0366 (8)
H190.07490.75000.09400.044*
C200.1246 (3)0.75000.03545 (15)0.0285 (7)
C210.1964 (3)0.75000.03284 (14)0.0195 (5)
C220.2039 (4)0.75000.08722 (17)0.0421 (9)
H220.15930.75000.13410.051*
C230.3459 (4)0.75000.07066 (17)0.0447 (9)
H230.40030.75000.10570.054*
C240.4092 (3)0.75000.00165 (16)0.0318 (7)
H240.50770.75000.00960.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0151 (2)0.0127 (2)0.0161 (2)0.0000.00103 (16)0.000
O10.0199 (9)0.0297 (12)0.0397 (12)0.0000.0072 (9)0.000
N10.0209 (10)0.0145 (11)0.0185 (11)0.0000.0024 (8)0.000
C10.0204 (12)0.0136 (12)0.0176 (12)0.0000.0006 (10)0.000
V20.0154 (2)0.0133 (2)0.0141 (2)0.0000.00034 (16)0.000
O20.0351 (11)0.0214 (11)0.0171 (9)0.0000.0067 (8)0.000
N20.0203 (10)0.0165 (11)0.0171 (10)0.0000.0020 (8)0.000
C20.0258 (13)0.0195 (14)0.0208 (13)0.0000.0021 (11)0.000
V30.0146 (2)0.0137 (2)0.0174 (2)0.0000.00009 (16)0.000
O30.0317 (7)0.0118 (6)0.0212 (6)0.0007 (6)0.0001 (5)0.0004 (5)
N30.0200 (10)0.0194 (12)0.0181 (11)0.0000.0049 (9)0.000
C30.0374 (16)0.0382 (18)0.0157 (13)0.0000.0026 (12)0.000
V40.0168 (2)0.0120 (2)0.0152 (2)0.0000.00117 (16)0.000
O40.0232 (10)0.0507 (15)0.0402 (13)0.0000.0139 (10)0.000
N40.0214 (10)0.0165 (11)0.0183 (11)0.0000.0055 (9)0.000
C40.0417 (18)0.049 (2)0.0195 (14)0.0000.0094 (13)0.000
O50.0344 (7)0.0131 (6)0.0207 (6)0.0011 (6)0.0031 (5)0.0005 (5)
C50.0281 (14)0.0354 (17)0.0210 (14)0.0000.0058 (11)0.000
O60.0182 (9)0.0362 (13)0.0434 (13)0.0000.0082 (9)0.000
C60.0177 (11)0.0153 (13)0.0200 (13)0.0000.0016 (10)0.000
O70.0281 (10)0.0218 (10)0.0180 (9)0.0000.0044 (8)0.000
C70.0186 (12)0.0191 (14)0.0271 (14)0.0000.0038 (11)0.000
O80.0259 (10)0.0426 (14)0.0317 (12)0.0000.0093 (9)0.000
C80.0173 (12)0.0305 (17)0.0348 (16)0.0000.0027 (12)0.000
C90.0226 (13)0.0279 (16)0.0272 (15)0.0000.0098 (11)0.000
C100.0286 (14)0.0353 (17)0.0194 (13)0.0000.0044 (11)0.000
C110.0319 (16)0.043 (2)0.0267 (15)0.0000.0128 (13)0.000
C120.0214 (13)0.0323 (17)0.0386 (17)0.0000.0103 (12)0.000
C130.0322 (15)0.0346 (17)0.0248 (15)0.0000.0122 (12)0.000
C140.0323 (16)0.041 (2)0.045 (2)0.0000.0229 (15)0.000
C150.0189 (13)0.0370 (19)0.058 (2)0.0000.0127 (14)0.000
C160.0178 (13)0.0251 (16)0.0379 (17)0.0000.0020 (12)0.000
C170.0160 (11)0.0152 (13)0.0237 (13)0.0000.0010 (10)0.000
C180.0204 (14)0.0366 (19)0.050 (2)0.0000.0125 (14)0.000
C190.0338 (16)0.0372 (19)0.0314 (17)0.0000.0135 (14)0.000
C200.0386 (16)0.0250 (16)0.0188 (14)0.0000.0030 (12)0.000
C210.0235 (13)0.0152 (13)0.0185 (12)0.0000.0007 (10)0.000
C220.062 (2)0.043 (2)0.0192 (15)0.0000.0024 (15)0.000
C230.057 (2)0.059 (3)0.0232 (16)0.0000.0218 (15)0.000
C240.0362 (16)0.0344 (18)0.0287 (16)0.0000.0159 (13)0.000
Geometric parameters (Å, º) top
V1—O11.596 (2)C4—C51.394 (4)
V1—O21.7987 (19)C4—H40.9500
V1—O31.8851 (13)C5—H50.9500
V1—O3i1.8851 (13)C6—C71.411 (4)
V1—N12.186 (2)C7—C121.409 (4)
V1—N22.307 (2)C7—C81.431 (4)
N1—C51.327 (4)C8—C91.354 (4)
N1—C11.363 (3)C8—H80.9500
C1—C21.404 (4)C9—H90.9500
C1—C61.433 (4)C10—C111.398 (4)
V2—O41.609 (2)C10—H100.9500
V2—O5i1.7363 (14)C11—C121.358 (4)
V2—O51.7363 (14)C11—H110.9500
V2—O21.7752 (19)C12—H120.9500
N2—C101.326 (4)C13—C141.401 (4)
N2—C61.350 (3)C13—H130.9500
C2—C31.412 (4)C14—C151.361 (5)
C2—C91.428 (4)C14—H140.9500
V3—O61.596 (2)C15—C161.408 (5)
V3—O71.7962 (19)C15—H150.9500
V3—O51.8873 (14)C16—C171.405 (4)
V3—O5ii1.8873 (14)C16—C181.440 (4)
V3—N42.192 (2)C17—C211.435 (4)
V3—N32.306 (2)C18—C191.343 (5)
O3—V41.7355 (13)C18—H180.9500
N3—C131.324 (4)C19—C201.442 (4)
N3—C171.349 (3)C19—H190.9500
C3—C41.363 (5)C20—C221.397 (5)
C3—H30.9500C20—C211.405 (4)
V4—O81.611 (2)C22—C231.369 (5)
V4—O3ii1.7355 (13)C22—H220.9500
V4—O71.7919 (19)C23—C241.393 (5)
N4—C241.335 (4)C23—H230.9500
N4—C211.358 (3)C24—H240.9500
O1—V1—O2106.75 (11)C3—C4—C5119.5 (3)
O1—V1—O397.49 (4)C3—C4—H4120.3
O2—V1—O394.25 (4)C5—C4—H4120.3
O1—V1—O3i97.49 (4)V2—O5—V3142.26 (8)
O2—V1—O3i94.25 (4)N1—C5—C4122.9 (3)
O3—V1—O3i159.85 (8)N1—C5—H5118.6
O1—V1—N191.44 (10)C4—C5—H5118.6
O2—V1—N1161.81 (10)N2—C6—C7123.4 (2)
O3—V1—N183.11 (4)N2—C6—C1117.0 (2)
O3i—V1—N183.11 (4)C7—C6—C1119.6 (2)
O1—V1—N2164.63 (10)V4—O7—V3141.53 (12)
O2—V1—N288.62 (9)C12—C7—C6116.6 (3)
O3—V1—N280.99 (4)C12—C7—C8123.9 (3)
O3i—V1—N280.99 (4)C6—C7—C8119.5 (2)
N1—V1—N273.19 (8)C9—C8—C7120.5 (3)
C5—N1—C1118.2 (2)C9—C8—H8119.8
C5—N1—V1124.08 (19)C7—C8—H8119.8
C1—N1—V1117.69 (17)C8—C9—C2121.5 (3)
N1—C1—C2122.6 (2)C8—C9—H9119.3
N1—C1—C6117.7 (2)C2—C9—H9119.3
C2—C1—C6119.7 (2)N2—C10—C11122.7 (3)
O4—V2—O5i110.32 (6)N2—C10—H10118.7
O4—V2—O5110.32 (6)C11—C10—H10118.7
O5i—V2—O5107.65 (9)C12—C11—C10119.8 (3)
O4—V2—O2110.09 (11)C12—C11—H11120.1
O5i—V2—O2109.20 (6)C10—C11—H11120.1
O5—V2—O2109.20 (6)C11—C12—C7119.6 (3)
V2—O2—V1156.65 (14)C11—C12—H12120.2
C10—N2—C6117.9 (2)C7—C12—H12120.2
C10—N2—V1127.66 (19)N3—C13—C14122.8 (3)
C6—N2—V1114.41 (17)N3—C13—H13118.6
C1—C2—C3117.2 (3)C14—C13—H13118.6
C1—C2—C9119.3 (3)C15—C14—C13119.1 (3)
C3—C2—C9123.5 (3)C15—C14—H14120.4
O6—V3—O7106.52 (11)C13—C14—H14120.4
O6—V3—O597.43 (4)C14—C15—C16119.9 (3)
O7—V3—O594.51 (4)C14—C15—H15120.0
O6—V3—O5ii97.43 (4)C16—C15—H15120.0
O7—V3—O5ii94.51 (4)C17—C16—C15116.8 (3)
O5—V3—O5ii159.65 (8)C17—C16—C18118.7 (3)
O6—V3—N489.80 (10)C15—C16—C18124.4 (3)
O7—V3—N4163.68 (9)N3—C17—C16123.1 (3)
O5—V3—N483.11 (4)N3—C17—C21117.2 (2)
O5ii—V3—N483.11 (4)C16—C17—C21119.6 (3)
O6—V3—N3162.58 (10)C19—C18—C16121.7 (3)
O7—V3—N390.89 (8)C19—C18—H18119.2
O5—V3—N380.83 (4)C16—C18—H18119.2
O5ii—V3—N380.83 (4)C18—C19—C20120.9 (3)
N4—V3—N372.78 (8)C18—C19—H19119.5
V4—O3—V1143.05 (8)C20—C19—H19119.5
C13—N3—C17118.3 (2)C22—C20—C21117.3 (3)
C13—N3—V3127.1 (2)C22—C20—C19124.0 (3)
C17—N3—V3114.64 (16)C21—C20—C19118.6 (3)
C4—C3—C2119.6 (3)N4—C21—C20122.5 (3)
C4—C3—H3120.2N4—C21—C17117.1 (2)
C2—C3—H3120.2C20—C21—C17120.4 (3)
O8—V4—O3ii110.81 (6)C23—C22—C20120.2 (3)
O8—V4—O3110.81 (6)C23—C22—H22119.9
O3ii—V4—O3107.90 (9)C20—C22—H22119.9
O8—V4—O7109.71 (10)C22—C23—C24118.9 (3)
O3ii—V4—O7108.78 (6)C22—C23—H23120.5
O3—V4—O7108.78 (6)C24—C23—H23120.5
C24—N4—C21118.2 (2)N4—C24—C23122.8 (3)
C24—N4—V3123.5 (2)N4—C24—H24118.6
C21—N4—V3118.29 (17)C23—C24—H24118.6
Symmetry codes: (i) x, y+1/2, z; (ii) x, y+3/2, z.
 

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