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The NbV atom in [NbO(C9H6NO)3]·2CH2Cl2 is chelated by the 8-hydroxy­quinolinato ligand and it exists in a pentagonal bipyramidal geometry. The Nb and oxo O atoms, and one of the 8-hydroxy­quinolinate groups lie on a crystallographic mirror plane. The structural features of the mol­ecule in the di­chloro­methane solvate are almost identical to those in the chloro­form solvate reported by García-Granda et al. [Acta Cryst. (1990). C46, 753–755].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029556/ci6322sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029556/ci6322Isup2.hkl
Contains datablock I

CCDC reference: 234788

Key indicators

  • Single-crystal X-ray study
  • T = 163 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.036
  • wR factor = 0.097
  • Data-to-parameter ratio = 14.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C19 PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.11
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Tris(8-hydroxyquinolinato-κ2O,N)oxoniobium(V) dichloromethane disolvate top
Crystal data top
[NbO(C9H6NO)3]·2CH2Cl2F(000) = 1432
Mr = 711.21Dx = 1.630 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 5268 reflections
a = 12.599 (1) Åθ = 2.4–26.0°
b = 17.659 (1) ŵ = 0.83 mm1
c = 13.024 (1) ÅT = 163 K
V = 2897.5 (4) Å3Plate, orange
Z = 40.35 × 0.13 × 0.07 mm
Data collection top
Siemens P4/CCD area-detector
diffractometer
3058 independent reflections
Radiation source: fine-focus sealed tube2422 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.066
φ and ω scansθmax = 26.5°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1515
Tmin = 0.711, Tmax = 0.945k = 1021
35672 measured reflectionsl = 1616
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.097H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0517P)2 + 2.9577P]
where P = (Fo2 + 2Fc2)/3
3058 reflections(Δ/σ)max = 0.001
205 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = 0.61 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nb10.12824 (3)0.25000.01209 (3)0.0196 (1)
Cl10.5196 (1)0.40630 (7)0.07858 (9)0.0756 (4)
Cl20.4555 (1)0.36682 (8)0.12763 (9)0.0803 (4)
O10.2534 (2)0.25000.0429 (2)0.0290 (6)
O20.1452 (2)0.3190 (1)0.1378 (1)0.0272 (5)
O30.0417 (2)0.25000.1216 (2)0.0219 (6)
N10.1121 (2)0.3779 (1)0.0399 (2)0.0229 (5)
N20.0552 (3)0.25000.0580 (2)0.0213 (7)
C10.0926 (2)0.4054 (2)0.1329 (2)0.028 (1)
C20.0975 (3)0.4841 (2)0.1542 (3)0.034 (1)
C30.1234 (2)0.5338 (2)0.0787 (3)0.034 (1)
C40.1437 (2)0.5076 (2)0.0219 (3)0.030 (1)
C50.1686 (3)0.5525 (2)0.1083 (3)0.037 (1)
C60.1825 (3)0.5197 (2)0.2020 (3)0.040 (1)
C70.1748 (3)0.4399 (2)0.2167 (3)0.034 (1)
C80.1526 (2)0.3944 (2)0.1340 (2)0.026 (1)
C90.1362 (2)0.4283 (2)0.0369 (2)0.023 (1)
C100.1001 (4)0.25000.1496 (3)0.030 (1)
C110.2114 (4)0.25000.1636 (4)0.037 (1)
C120.2749 (4)0.25000.0790 (4)0.036 (1)
C130.2316 (3)0.25000.0203 (3)0.027 (1)
C140.2889 (4)0.25000.1138 (4)0.034 (1)
C150.2352 (4)0.25000.2065 (4)0.034 (1)
C160.1248 (3)0.25000.2113 (3)0.029 (1)
C170.0648 (3)0.25000.1230 (3)0.022 (1)
C180.1188 (3)0.25000.0273 (3)0.021 (1)
C190.4120 (3)0.3933 (2)0.0056 (3)0.053 (1)
H10.07470.37130.18670.034*
H20.08260.50200.22150.040*
H30.12800.58640.09360.041*
H50.17580.60580.10100.044*
H60.19780.55100.25940.048*
H70.18490.41850.28290.041*
H100.05570.25000.20860.035*
H110.24120.25000.23060.044*
H120.34980.25000.08730.043*
H140.36430.25000.11290.041*
H150.27480.25000.26860.040*
H160.09050.25000.27620.034*
H19a0.37100.44100.01060.064*
H19b0.36440.35370.02200.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0232 (2)0.0124 (2)0.0231 (2)0.0000.0030 (1)0.000
Cl10.100 (1)0.0586 (7)0.0683 (7)0.0042 (6)0.0305 (7)0.0030 (6)
Cl20.114 (1)0.0667 (8)0.0601 (7)0.0148 (7)0.0179 (7)0.0081 (6)
O10.029 (2)0.019 (2)0.039 (2)0.0000.002 (1)0.000
O20.042 (1)0.013 (1)0.026 (1)0.002 (1)0.010 (1)0.002 (1)
O30.025 (1)0.021 (2)0.020 (1)0.0000.001 (1)0.000
N10.025 (1)0.016 (1)0.028 (1)0.002 (1)0.001 (1)0.003 (1)
N20.029 (2)0.014 (2)0.021 (2)0.0000.002 (1)0.000
C10.032 (2)0.025 (2)0.028 (2)0.003 (1)0.003 (1)0.006 (1)
C20.038 (2)0.026 (2)0.038 (2)0.006 (1)0.010 (1)0.013 (1)
C30.033 (2)0.018 (2)0.052 (2)0.000 (1)0.011 (2)0.010 (1)
C40.022 (2)0.016 (1)0.051 (2)0.002 (1)0.003 (1)0.002 (1)
C50.036 (2)0.013 (2)0.062 (2)0.001 (1)0.006 (2)0.006 (1)
C60.042 (2)0.020 (2)0.059 (2)0.003 (1)0.018 (2)0.015 (2)
C70.041 (2)0.021 (2)0.041 (2)0.003 (1)0.016 (2)0.008 (1)
C80.026 (2)0.016 (1)0.037 (2)0.001 (1)0.006 (1)0.003 (1)
C90.020 (1)0.016 (1)0.034 (2)0.000 (1)0.001 (1)0.001 (1)
C100.042 (3)0.023 (2)0.024 (2)0.0000.003 (2)0.000
C110.050 (3)0.023 (2)0.038 (3)0.0000.021 (2)0.000
C120.032 (2)0.021 (2)0.055 (3)0.0000.015 (2)0.000
C130.026 (2)0.012 (2)0.042 (2)0.0000.001 (2)0.000
C140.026 (2)0.020 (2)0.058 (3)0.0000.009 (2)0.000
C150.039 (3)0.023 (2)0.038 (3)0.0000.018 (2)0.000
C160.043 (3)0.020 (2)0.024 (2)0.0000.006 (2)0.000
C170.028 (2)0.011 (2)0.026 (2)0.0000.001 (2)0.000
C180.026 (2)0.007 (2)0.030 (2)0.0000.000 (2)0.000
C190.039 (2)0.045 (2)0.075 (3)0.007 (2)0.005 (2)0.008 (2)
Geometric parameters (Å, º) top
Nb1—O11.732 (3)C10—C111.414 (7)
Nb1—O22.052 (2)C11—C121.362 (7)
Nb1—O2i2.052 (2)C12—C131.403 (6)
Nb1—O32.054 (3)C13—C141.416 (6)
Nb1—N12.366 (2)C13—C181.424 (5)
Nb1—N1i2.366 (2)C14—C151.384 (7)
Nb1—N22.386 (3)C15—C161.393 (6)
Cl1—C191.759 (4)C16—C171.376 (6)
Cl2—C191.745 (4)C17—C181.420 (6)
O2—C81.337 (3)C1—H10.95
O3—C171.342 (5)C2—H20.95
N1—C11.328 (4)C3—H30.95
N1—C91.373 (4)C5—H50.95
N2—C101.321 (5)C6—H60.95
N2—C181.370 (5)C7—H70.95
C1—C21.419 (4)C10—H100.95
C2—C31.358 (5)C11—H110.95
C3—C41.413 (5)C12—H120.95
C4—C51.412 (5)C14—H140.95
C4—C91.417 (4)C15—H150.95
C5—C61.362 (5)C16—H160.95
C6—C71.425 (4)C19—H19a0.99
C7—C81.372 (4)C19—H19b0.99
C8—C91.414 (4)
O1—Nb1—O2103.6 (1)C12—C11—C10118.6 (4)
O1—Nb1—O2i103.6 (1)C11—C12—C13121.1 (4)
O1—Nb1—O397.6 (1)C12—C13—C14126.5 (4)
O1—Nb1—N187.7 (1)C12—C13—C18116.6 (4)
O1—Nb1—N1i87.7 (1)C14—C13—C18116.9 (4)
O1—Nb1—N2170.1 (1)C15—C14—C13120.1 (4)
O2—Nb1—O2i72.8 (1)C16—C15—C14121.7 (4)
O2—Nb1—O3137.0 (1)C17—C16—C15120.8 (4)
O2—Nb1—N170.8 (1)O3—C17—C16124.2 (4)
O2—Nb1—N1i143.5 (1)O3—C17—C18117.8 (3)
O2—Nb1—N284.3 (1)C16—C17—C18118.0 (4)
O2i—Nb1—O3137.0 (1)N2—C18—C17115.6 (3)
O2i—Nb1—N1143.5 (1)N2—C18—C13122.1 (4)
O2i—Nb1—N1i70.8 (1)C17—C18—C13122.3 (4)
O2i—Nb1—N284.3 (1)Cl2—C19—Cl1111.1 (2)
O3—Nb1—N173.3 (1)N1—C1—H1119.0
O3—Nb1—N1i73.3 (1)C2—C1—H1119.0
N1i—Nb1—N1145.2 (1)C3—C2—H2119.9
O3—Nb1—N272.5 (1)C1—C2—H2119.9
N1—Nb1—N289.4 (1)C2—C3—H3119.9
N1i—Nb1—N289.4 (1)C4—C3—H3119.9
C8—O2—Nb1124.7 (2)C6—C5—H5119.9
C17—O3—Nb1122.9 (2)C4—C5—H5119.9
C1—N1—C9117.9 (3)C5—C6—H6118.9
C1—N1—Nb1128.8 (2)C7—C6—H6118.9
C9—N1—Nb1113.0 (2)C8—C7—H7120.4
C10—N2—C18118.8 (4)C6—C7—H7120.4
C10—N2—Nb1129.9 (3)N2—C10—H10118.6
C18—N2—Nb1111.3 (2)C11—C10—H10118.6
N1—C1—C2121.9 (3)C12—C11—H11120.7
C3—C2—C1120.1 (3)C10—C11—H11120.7
C2—C3—C4120.1 (3)C11—C12—H12119.4
C5—C4—C9117.4 (3)C13—C12—H12119.4
C5—C4—C3126.5 (3)C15—C14—H14119.9
C9—C4—C3116.1 (3)C13—C14—H14119.9
C6—C5—C4120.3 (3)C16—C15—H15119.1
C5—C6—C7122.1 (3)C14—C15—H15119.1
C8—C7—C6119.2 (3)C17—C16—H16119.6
O2—C8—C7124.7 (3)C15—C16—H16119.6
O2—C8—C9116.4 (2)Cl2—C19—H19a109.4
C7—C8—C9118.9 (3)Cl1—C19—H19a109.4
N1—C9—C8114.2 (2)Cl2—C19—H19b109.4
N1—C9—C4123.7 (3)Cl1—C19—H19b109.4
C8—C9—C4122.1 (3)H19a—C19—H19b108.0
N2—C10—C11122.8 (4)
O1—Nb1—O2—C874.5 (2)N1i—Nb1—N2—C1872.6 (1)
O2i—Nb1—O2—C8174.8 (2)N1—Nb1—N2—C1872.6 (1)
O3—Nb1—O2—C842.8 (3)C9—N1—C1—C20.9 (4)
N1i—Nb1—O2—C8179.5 (2)Nb1—N1—C1—C2172.5 (2)
N1—Nb1—O2—C88.1 (2)N1—C1—C2—C30.4 (5)
N2—Nb1—O2—C899.4 (2)C1—C2—C3—C41.2 (5)
O2—Nb1—O3—C1760.5 (1)C2—C3—C4—C5178.2 (3)
O2i—Nb1—O3—C1760.5 (1)C2—C3—C4—C90.7 (4)
N1i—Nb1—O3—C1794.7 (1)C9—C4—C5—C61.3 (5)
N1—Nb1—O3—C1794.7 (1)C3—C4—C5—C6177.6 (3)
O1—Nb1—N1—C176.4 (3)C4—C5—C6—C71.3 (5)
O2—Nb1—N1—C1178.3 (3)C5—C6—C7—C80.0 (5)
O2i—Nb1—N1—C1173.6 (2)Nb1—O2—C8—C7173.0 (2)
O3—Nb1—N1—C122.3 (2)Nb1—O2—C8—C97.0 (4)
N1i—Nb1—N1—C16.2 (4)C6—C7—C8—O2178.8 (3)
N2—Nb1—N1—C194.1 (3)C6—C7—C8—C91.1 (5)
O1—Nb1—N1—C997.2 (2)C1—N1—C9—C8178.1 (2)
O2—Nb1—N1—C98.03 (17)Nb1—N1—C9—C87.5 (3)
O2i—Nb1—N1—C912.7 (3)C1—N1—C9—C41.5 (4)
O3—Nb1—N1—C9164.1 (2)Nb1—N1—C9—C4172.9 (2)
N1i—Nb1—N1—C9179.9 (1)O2—C8—C9—N11.5 (4)
N2—Nb1—N1—C992.2 (2)C7—C8—C9—N1178.5 (3)
O2—Nb1—N2—C1036.6 (1)O2—C8—C9—C4178.9 (2)
O2i—Nb1—N2—C1036.6 (1)C7—C8—C9—C41.1 (4)
N1i—Nb1—N2—C10107.4 (1)C5—C4—C9—N1179.7 (3)
N1—Nb1—N2—C10107.4 (1)C3—C4—C9—N10.7 (4)
O2—Nb1—N2—C18143.4 (1)C5—C4—C9—C80.1 (4)
O2i—Nb1—N2—C18143.4 (1)C3—C4—C9—C8178.9 (3)
Symmetry code: (i) x, y+1/2, z.
 

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