metal-organic compounds
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
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029556/ci6322sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029556/ci6322Isup2.hkl |
CCDC reference: 234788
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.
Crystal data top
[NbO(C9H6NO)3]·2CH2Cl2 | F(000) = 1432 |
Mr = 711.21 | Dx = 1.630 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 5268 reflections |
a = 12.599 (1) Å | θ = 2.4–26.0° |
b = 17.659 (1) Å | µ = 0.83 mm−1 |
c = 13.024 (1) Å | T = 163 K |
V = 2897.5 (4) Å3 | Plate, orange |
Z = 4 | 0.35 × 0.13 × 0.07 mm |
Data collection top
Siemens P4/CCD area-detector diffractometer | 3058 independent reflections |
Radiation source: fine-focus sealed tube | 2422 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
φ and ω scans | θmax = 26.5°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.711, Tmax = 0.945 | k = −10→21 |
35672 measured reflections | l = −16→16 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-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 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Nb1 | 0.12824 (3) | 0.2500 | 0.01209 (3) | 0.0196 (1) | |
Cl1 | 0.5196 (1) | 0.40630 (7) | −0.07858 (9) | 0.0756 (4) | |
Cl2 | 0.4555 (1) | 0.36682 (8) | 0.12763 (9) | 0.0803 (4) | |
O1 | 0.2534 (2) | 0.2500 | −0.0429 (2) | 0.0290 (6) | |
O2 | 0.1452 (2) | 0.3190 (1) | 0.1378 (1) | 0.0272 (5) | |
O3 | 0.0417 (2) | 0.2500 | −0.1216 (2) | 0.0219 (6) | |
N1 | 0.1121 (2) | 0.3779 (1) | −0.0399 (2) | 0.0229 (5) | |
N2 | −0.0552 (3) | 0.2500 | 0.0580 (2) | 0.0213 (7) | |
C1 | 0.0926 (2) | 0.4054 (2) | −0.1329 (2) | 0.028 (1) | |
C2 | 0.0975 (3) | 0.4841 (2) | −0.1542 (3) | 0.034 (1) | |
C3 | 0.1234 (2) | 0.5338 (2) | −0.0787 (3) | 0.034 (1) | |
C4 | 0.1437 (2) | 0.5076 (2) | 0.0219 (3) | 0.030 (1) | |
C5 | 0.1686 (3) | 0.5525 (2) | 0.1083 (3) | 0.037 (1) | |
C6 | 0.1825 (3) | 0.5197 (2) | 0.2020 (3) | 0.040 (1) | |
C7 | 0.1748 (3) | 0.4399 (2) | 0.2167 (3) | 0.034 (1) | |
C8 | 0.1526 (2) | 0.3944 (2) | 0.1340 (2) | 0.026 (1) | |
C9 | 0.1362 (2) | 0.4283 (2) | 0.0369 (2) | 0.023 (1) | |
C10 | −0.1001 (4) | 0.2500 | 0.1496 (3) | 0.030 (1) | |
C11 | −0.2114 (4) | 0.2500 | 0.1636 (4) | 0.037 (1) | |
C12 | −0.2749 (4) | 0.2500 | 0.0790 (4) | 0.036 (1) | |
C13 | −0.2316 (3) | 0.2500 | −0.0203 (3) | 0.027 (1) | |
C14 | −0.2889 (4) | 0.2500 | −0.1138 (4) | 0.034 (1) | |
C15 | −0.2352 (4) | 0.2500 | −0.2065 (4) | 0.034 (1) | |
C16 | −0.1248 (3) | 0.2500 | −0.2113 (3) | 0.029 (1) | |
C17 | −0.0648 (3) | 0.2500 | −0.1230 (3) | 0.022 (1) | |
C18 | −0.1188 (3) | 0.2500 | −0.0273 (3) | 0.021 (1) | |
C19 | 0.4120 (3) | 0.3933 (2) | 0.0056 (3) | 0.053 (1) | |
H1 | 0.0747 | 0.3713 | −0.1867 | 0.034* | |
H2 | 0.0826 | 0.5020 | −0.2215 | 0.040* | |
H3 | 0.1280 | 0.5864 | −0.0936 | 0.041* | |
H5 | 0.1758 | 0.6058 | 0.1010 | 0.044* | |
H6 | 0.1978 | 0.5510 | 0.2594 | 0.048* | |
H7 | 0.1849 | 0.4185 | 0.2829 | 0.041* | |
H10 | −0.0557 | 0.2500 | 0.2086 | 0.035* | |
H11 | −0.2412 | 0.2500 | 0.2306 | 0.044* | |
H12 | −0.3498 | 0.2500 | 0.0873 | 0.043* | |
H14 | −0.3643 | 0.2500 | −0.1129 | 0.041* | |
H15 | −0.2748 | 0.2500 | −0.2686 | 0.040* | |
H16 | −0.0905 | 0.2500 | −0.2762 | 0.034* | |
H19a | 0.3710 | 0.4410 | 0.0106 | 0.064* | |
H19b | 0.3644 | 0.3537 | −0.0220 | 0.064* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.0232 (2) | 0.0124 (2) | 0.0231 (2) | 0.000 | −0.0030 (1) | 0.000 |
Cl1 | 0.100 (1) | 0.0586 (7) | 0.0683 (7) | 0.0042 (6) | 0.0305 (7) | 0.0030 (6) |
Cl2 | 0.114 (1) | 0.0667 (8) | 0.0601 (7) | 0.0148 (7) | 0.0179 (7) | 0.0081 (6) |
O1 | 0.029 (2) | 0.019 (2) | 0.039 (2) | 0.000 | −0.002 (1) | 0.000 |
O2 | 0.042 (1) | 0.013 (1) | 0.026 (1) | −0.002 (1) | −0.010 (1) | −0.002 (1) |
O3 | 0.025 (1) | 0.021 (2) | 0.020 (1) | 0.000 | 0.001 (1) | 0.000 |
N1 | 0.025 (1) | 0.016 (1) | 0.028 (1) | 0.002 (1) | 0.001 (1) | 0.003 (1) |
N2 | 0.029 (2) | 0.014 (2) | 0.021 (2) | 0.000 | 0.002 (1) | 0.000 |
C1 | 0.032 (2) | 0.025 (2) | 0.028 (2) | 0.003 (1) | 0.003 (1) | 0.006 (1) |
C2 | 0.038 (2) | 0.026 (2) | 0.038 (2) | 0.006 (1) | 0.010 (1) | 0.013 (1) |
C3 | 0.033 (2) | 0.018 (2) | 0.052 (2) | 0.000 (1) | 0.011 (2) | 0.010 (1) |
C4 | 0.022 (2) | 0.016 (1) | 0.051 (2) | 0.002 (1) | 0.003 (1) | 0.002 (1) |
C5 | 0.036 (2) | 0.013 (2) | 0.062 (2) | 0.001 (1) | −0.006 (2) | −0.006 (1) |
C6 | 0.042 (2) | 0.020 (2) | 0.059 (2) | 0.003 (1) | −0.018 (2) | −0.015 (2) |
C7 | 0.041 (2) | 0.021 (2) | 0.041 (2) | 0.003 (1) | −0.016 (2) | −0.008 (1) |
C8 | 0.026 (2) | 0.016 (1) | 0.037 (2) | 0.001 (1) | −0.006 (1) | −0.003 (1) |
C9 | 0.020 (1) | 0.016 (1) | 0.034 (2) | 0.000 (1) | −0.001 (1) | −0.001 (1) |
C10 | 0.042 (3) | 0.023 (2) | 0.024 (2) | 0.000 | 0.003 (2) | 0.000 |
C11 | 0.050 (3) | 0.023 (2) | 0.038 (3) | 0.000 | 0.021 (2) | 0.000 |
C12 | 0.032 (2) | 0.021 (2) | 0.055 (3) | 0.000 | 0.015 (2) | 0.000 |
C13 | 0.026 (2) | 0.012 (2) | 0.042 (2) | 0.000 | 0.001 (2) | 0.000 |
C14 | 0.026 (2) | 0.020 (2) | 0.058 (3) | 0.000 | −0.009 (2) | 0.000 |
C15 | 0.039 (3) | 0.023 (2) | 0.038 (3) | 0.000 | −0.018 (2) | 0.000 |
C16 | 0.043 (3) | 0.020 (2) | 0.024 (2) | 0.000 | −0.006 (2) | 0.000 |
C17 | 0.028 (2) | 0.011 (2) | 0.026 (2) | 0.000 | −0.001 (2) | 0.000 |
C18 | 0.026 (2) | 0.007 (2) | 0.030 (2) | 0.000 | 0.000 (2) | 0.000 |
C19 | 0.039 (2) | 0.045 (2) | 0.075 (3) | −0.007 (2) | −0.005 (2) | −0.008 (2) |
Geometric parameters (Å, º) top
Nb1—O1 | 1.732 (3) | C10—C11 | 1.414 (7) |
Nb1—O2 | 2.052 (2) | C11—C12 | 1.362 (7) |
Nb1—O2i | 2.052 (2) | C12—C13 | 1.403 (6) |
Nb1—O3 | 2.054 (3) | C13—C14 | 1.416 (6) |
Nb1—N1 | 2.366 (2) | C13—C18 | 1.424 (5) |
Nb1—N1i | 2.366 (2) | C14—C15 | 1.384 (7) |
Nb1—N2 | 2.386 (3) | C15—C16 | 1.393 (6) |
Cl1—C19 | 1.759 (4) | C16—C17 | 1.376 (6) |
Cl2—C19 | 1.745 (4) | C17—C18 | 1.420 (6) |
O2—C8 | 1.337 (3) | C1—H1 | 0.95 |
O3—C17 | 1.342 (5) | C2—H2 | 0.95 |
N1—C1 | 1.328 (4) | C3—H3 | 0.95 |
N1—C9 | 1.373 (4) | C5—H5 | 0.95 |
N2—C10 | 1.321 (5) | C6—H6 | 0.95 |
N2—C18 | 1.370 (5) | C7—H7 | 0.95 |
C1—C2 | 1.419 (4) | C10—H10 | 0.95 |
C2—C3 | 1.358 (5) | C11—H11 | 0.95 |
C3—C4 | 1.413 (5) | C12—H12 | 0.95 |
C4—C5 | 1.412 (5) | C14—H14 | 0.95 |
C4—C9 | 1.417 (4) | C15—H15 | 0.95 |
C5—C6 | 1.362 (5) | C16—H16 | 0.95 |
C6—C7 | 1.425 (4) | C19—H19a | 0.99 |
C7—C8 | 1.372 (4) | C19—H19b | 0.99 |
C8—C9 | 1.414 (4) | ||
O1—Nb1—O2 | 103.6 (1) | C12—C11—C10 | 118.6 (4) |
O1—Nb1—O2i | 103.6 (1) | C11—C12—C13 | 121.1 (4) |
O1—Nb1—O3 | 97.6 (1) | C12—C13—C14 | 126.5 (4) |
O1—Nb1—N1 | 87.7 (1) | C12—C13—C18 | 116.6 (4) |
O1—Nb1—N1i | 87.7 (1) | C14—C13—C18 | 116.9 (4) |
O1—Nb1—N2 | 170.1 (1) | C15—C14—C13 | 120.1 (4) |
O2—Nb1—O2i | 72.8 (1) | C16—C15—C14 | 121.7 (4) |
O2—Nb1—O3 | 137.0 (1) | C17—C16—C15 | 120.8 (4) |
O2—Nb1—N1 | 70.8 (1) | O3—C17—C16 | 124.2 (4) |
O2—Nb1—N1i | 143.5 (1) | O3—C17—C18 | 117.8 (3) |
O2—Nb1—N2 | 84.3 (1) | C16—C17—C18 | 118.0 (4) |
O2i—Nb1—O3 | 137.0 (1) | N2—C18—C17 | 115.6 (3) |
O2i—Nb1—N1 | 143.5 (1) | N2—C18—C13 | 122.1 (4) |
O2i—Nb1—N1i | 70.8 (1) | C17—C18—C13 | 122.3 (4) |
O2i—Nb1—N2 | 84.3 (1) | Cl2—C19—Cl1 | 111.1 (2) |
O3—Nb1—N1 | 73.3 (1) | N1—C1—H1 | 119.0 |
O3—Nb1—N1i | 73.3 (1) | C2—C1—H1 | 119.0 |
N1i—Nb1—N1 | 145.2 (1) | C3—C2—H2 | 119.9 |
O3—Nb1—N2 | 72.5 (1) | C1—C2—H2 | 119.9 |
N1—Nb1—N2 | 89.4 (1) | C2—C3—H3 | 119.9 |
N1i—Nb1—N2 | 89.4 (1) | C4—C3—H3 | 119.9 |
C8—O2—Nb1 | 124.7 (2) | C6—C5—H5 | 119.9 |
C17—O3—Nb1 | 122.9 (2) | C4—C5—H5 | 119.9 |
C1—N1—C9 | 117.9 (3) | C5—C6—H6 | 118.9 |
C1—N1—Nb1 | 128.8 (2) | C7—C6—H6 | 118.9 |
C9—N1—Nb1 | 113.0 (2) | C8—C7—H7 | 120.4 |
C10—N2—C18 | 118.8 (4) | C6—C7—H7 | 120.4 |
C10—N2—Nb1 | 129.9 (3) | N2—C10—H10 | 118.6 |
C18—N2—Nb1 | 111.3 (2) | C11—C10—H10 | 118.6 |
N1—C1—C2 | 121.9 (3) | C12—C11—H11 | 120.7 |
C3—C2—C1 | 120.1 (3) | C10—C11—H11 | 120.7 |
C2—C3—C4 | 120.1 (3) | C11—C12—H12 | 119.4 |
C5—C4—C9 | 117.4 (3) | C13—C12—H12 | 119.4 |
C5—C4—C3 | 126.5 (3) | C15—C14—H14 | 119.9 |
C9—C4—C3 | 116.1 (3) | C13—C14—H14 | 119.9 |
C6—C5—C4 | 120.3 (3) | C16—C15—H15 | 119.1 |
C5—C6—C7 | 122.1 (3) | C14—C15—H15 | 119.1 |
C8—C7—C6 | 119.2 (3) | C17—C16—H16 | 119.6 |
O2—C8—C7 | 124.7 (3) | C15—C16—H16 | 119.6 |
O2—C8—C9 | 116.4 (2) | Cl2—C19—H19a | 109.4 |
C7—C8—C9 | 118.9 (3) | Cl1—C19—H19a | 109.4 |
N1—C9—C8 | 114.2 (2) | Cl2—C19—H19b | 109.4 |
N1—C9—C4 | 123.7 (3) | Cl1—C19—H19b | 109.4 |
C8—C9—C4 | 122.1 (3) | H19a—C19—H19b | 108.0 |
N2—C10—C11 | 122.8 (4) | ||
O1—Nb1—O2—C8 | 74.5 (2) | N1i—Nb1—N2—C18 | −72.6 (1) |
O2i—Nb1—O2—C8 | 174.8 (2) | N1—Nb1—N2—C18 | 72.6 (1) |
O3—Nb1—O2—C8 | −42.8 (3) | C9—N1—C1—C2 | 0.9 (4) |
N1i—Nb1—O2—C8 | 179.5 (2) | Nb1—N1—C1—C2 | −172.5 (2) |
N1—Nb1—O2—C8 | −8.1 (2) | N1—C1—C2—C3 | 0.4 (5) |
N2—Nb1—O2—C8 | −99.4 (2) | C1—C2—C3—C4 | −1.2 (5) |
O2—Nb1—O3—C17 | −60.5 (1) | C2—C3—C4—C5 | −178.2 (3) |
O2i—Nb1—O3—C17 | 60.5 (1) | C2—C3—C4—C9 | 0.7 (4) |
N1i—Nb1—O3—C17 | 94.7 (1) | C9—C4—C5—C6 | −1.3 (5) |
N1—Nb1—O3—C17 | −94.7 (1) | C3—C4—C5—C6 | 177.6 (3) |
O1—Nb1—N1—C1 | 76.4 (3) | C4—C5—C6—C7 | 1.3 (5) |
O2—Nb1—N1—C1 | −178.3 (3) | C5—C6—C7—C8 | 0.0 (5) |
O2i—Nb1—N1—C1 | −173.6 (2) | Nb1—O2—C8—C7 | −173.0 (2) |
O3—Nb1—N1—C1 | −22.3 (2) | Nb1—O2—C8—C9 | 7.0 (4) |
N1i—Nb1—N1—C1 | −6.2 (4) | C6—C7—C8—O2 | 178.8 (3) |
N2—Nb1—N1—C1 | −94.1 (3) | C6—C7—C8—C9 | −1.1 (5) |
O1—Nb1—N1—C9 | −97.2 (2) | C1—N1—C9—C8 | 178.1 (2) |
O2—Nb1—N1—C9 | 8.03 (17) | Nb1—N1—C9—C8 | −7.5 (3) |
O2i—Nb1—N1—C9 | 12.7 (3) | C1—N1—C9—C4 | −1.5 (4) |
O3—Nb1—N1—C9 | 164.1 (2) | Nb1—N1—C9—C4 | 172.9 (2) |
N1i—Nb1—N1—C9 | −179.9 (1) | O2—C8—C9—N1 | 1.5 (4) |
N2—Nb1—N1—C9 | 92.2 (2) | C7—C8—C9—N1 | −178.5 (3) |
O2—Nb1—N2—C10 | −36.6 (1) | O2—C8—C9—C4 | −178.9 (2) |
O2i—Nb1—N2—C10 | 36.6 (1) | C7—C8—C9—C4 | 1.1 (4) |
N1i—Nb1—N2—C10 | 107.4 (1) | C5—C4—C9—N1 | 179.7 (3) |
N1—Nb1—N2—C10 | −107.4 (1) | C3—C4—C9—N1 | 0.7 (4) |
O2—Nb1—N2—C18 | 143.4 (1) | C5—C4—C9—C8 | 0.1 (4) |
O2i—Nb1—N2—C18 | −143.4 (1) | C3—C4—C9—C8 | −178.9 (3) |
Symmetry code: (i) x, −y+1/2, z. |