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The hydroxy­quinolinate group chelates to the Ti atom in the centrosymmetric title compound, [Ti2(C9H6NO)2(C2H5O)6]. Two of the four ethoxy groups function as bridges, and the geometry of the six-coordinate Ti atom is that of an octahedron.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029544/ci6321sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029544/ci6321Isup2.hkl
Contains datablock I

CCDC reference: 234787

Key indicators

  • Single-crystal X-ray study
  • T = 163 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.031
  • wR factor = 0.091
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.56 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 - C3 = 5.87 su PLAT702_ALERT_1_C Angle Calc 168.87(6), Rep 168.80(10), Dev.. 1.17 Sigma O2 -TI1 -N1 1.555 1.555 1.555
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 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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

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.

Di-µ-ethoxy-bis[diethoxy(8-quinolinato)titanium(IV)] top
Crystal data top
[Ti2(C9H6NO)2(C2H5O)6]F(000) = 688
Mr = 654.46Dx = 1.321 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5733 reflections
a = 8.7135 (6) Åθ = 2.7–26.3°
b = 13.5629 (9) ŵ = 0.53 mm1
c = 13.930 (1) ÅT = 163 K
β = 91.986 (1)°Block, yellow
V = 1645.3 (2) Å30.50 × 0.30 × 0.17 mm
Z = 2
Data collection top
Bruker P4/CCD area-detector
diffractometer
3344 independent reflections
Radiation source: normal-focus sealed tube2793 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
φ and ω scansθmax = 26.4°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 109
Tmin = 0.693, Tmax = 0.915k = 1616
20052 measured reflectionsl = 1717
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0467P)2 + 0.625P]
where P = (Fo2 + 2Fc2)/3
3344 reflections(Δ/σ)max < 0.001
190 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.30 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ti10.54947 (4)0.39295 (2)0.45545 (2)0.0314 (1)
O10.6304 (1)0.5277 (1)0.4905 (1)0.0321 (3)
O20.4848 (2)0.4048 (1)0.3304 (1)0.0402 (3)
O30.7358 (2)0.3424 (1)0.4335 (1)0.0423 (3)
O40.4379 (2)0.2683 (1)0.4740 (1)0.0391 (3)
N10.6069 (2)0.3491 (1)0.6116 (1)0.0343 (3)
C10.7831 (2)0.5615 (2)0.4753 (1)0.0418 (4)
C20.8073 (3)0.5872 (2)0.3714 (2)0.0568 (6)
C30.5440 (3)0.3626 (2)0.2449 (2)0.0557 (6)
C40.4949 (4)0.4203 (3)0.1590 (2)0.0818 (9)
C50.8572 (3)0.2771 (2)0.4556 (2)0.0543 (5)
C60.8293 (4)0.1775 (2)0.4125 (2)0.0775 (8)
C70.6932 (2)0.3930 (1)0.6792 (1)0.0408 (4)
C80.7381 (2)0.3454 (2)0.7658 (1)0.0454 (5)
C90.6903 (2)0.2518 (2)0.7827 (1)0.0448 (5)
C100.5949 (2)0.2020 (1)0.7135 (1)0.0382 (4)
C110.5371 (3)0.1051 (2)0.7222 (2)0.0492 (5)
C120.4495 (3)0.0647 (2)0.6488 (2)0.0510 (5)
C130.4124 (2)0.1174 (1)0.5629 (2)0.0438 (4)
C140.4656 (2)0.2124 (1)0.5516 (2)0.0343 (4)
C150.5576 (2)0.2549 (1)0.6278 (1)0.0322 (4)
H1a0.85700.50940.49570.050*
H1b0.80400.62030.51570.050*
H2a0.91300.61010.36430.085*
H2b0.73560.63960.35130.085*
H2c0.78900.52870.33130.085*
H3a0.50690.29390.23780.067*
H3b0.65760.36100.25030.067*
H4a0.53670.39000.10160.123*
H4b0.53300.48800.16550.123*
H4c0.38250.42100.15310.123*
H5a0.86990.27070.52620.065*
H5b0.95370.30450.43110.065*
H6a0.91630.13420.42900.116*
H6b0.81810.18350.34250.116*
H6c0.73520.14950.43780.116*
H70.72600.45890.66890.049*
H80.80160.37870.81220.054*
H90.72080.21960.84090.054*
H110.55920.06800.77890.059*
H120.41210.00060.65550.061*
H130.35120.08720.51330.053*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0383 (2)0.0294 (2)0.0262 (2)0.0025 (1)0.0028 (1)0.0013 (1)
O10.0332 (6)0.0322 (6)0.0307 (6)0.0051 (5)0.0016 (5)0.0009 (5)
O20.0529 (8)0.0414 (7)0.0261 (6)0.0038 (6)0.0032 (5)0.0001 (5)
O30.0443 (7)0.0391 (7)0.0433 (7)0.0035 (6)0.0001 (6)0.0009 (6)
O40.0507 (7)0.0327 (6)0.0333 (6)0.0080 (5)0.0084 (5)0.0020 (5)
N10.0363 (8)0.0342 (8)0.0320 (7)0.0002 (6)0.0050 (6)0.0030 (6)
C10.035 (1)0.044 (1)0.047 (1)0.010 (1)0.001 (1)0.007 (1)
C20.056 (1)0.056 (1)0.059 (1)0.006 (1)0.021 (1)0.004 (1)
C30.065 (1)0.064 (1)0.039 (1)0.016 (1)0.006 (1)0.008 (1)
C40.090 (2)0.119 (2)0.037 (1)0.012 (2)0.002 (1)0.008 (1)
C50.046 (1)0.059 (1)0.058 (1)0.010 (1)0.003 (1)0.007 (1)
C60.096 (2)0.052 (1)0.086 (2)0.019 (1)0.008 (2)0.012 (1)
C70.044 (1)0.040 (1)0.038 (1)0.004 (1)0.009 (1)0.002 (1)
C80.043 (1)0.057 (1)0.036 (1)0.000 (1)0.011 (1)0.002 (1)
C90.042 (1)0.058 (1)0.033 (1)0.009 (1)0.005 (1)0.013 (1)
C100.036 (1)0.042 (1)0.037 (1)0.009 (1)0.003 (1)0.009 (1)
C110.054 (1)0.043 (1)0.051 (1)0.005 (1)0.004 (1)0.020 (1)
C120.059 (1)0.033 (1)0.062 (1)0.003 (1)0.008 (1)0.013 (1)
C130.048 (1)0.035 (1)0.049 (1)0.004 (1)0.003 (1)0.002 (1)
C140.037 (1)0.033 (1)0.034 (1)0.001 (1)0.003 (1)0.003 (1)
C150.032 (1)0.031 (1)0.033 (1)0.004 (1)0.002 (1)0.004 (1)
Geometric parameters (Å, º) top
Ti1—O12.013 (1)C14—C151.429 (2)
Ti1—O1i2.065 (1)C1—H1a0.99
Ti1—O21.819 (1)C1—H1b0.99
Ti1—O31.799 (1)C2—H2a0.98
Ti1—O41.972 (1)C2—H2b0.98
Ti1—N12.294 (1)C2—H2c0.98
O1—C11.430 (2)C3—H3a0.99
O2—C31.434 (2)C3—H3b0.99
O3—C51.405 (2)C4—H4a0.98
O4—C141.335 (2)C4—H4b0.98
N1—C71.326 (2)C4—H4c0.98
N1—C151.368 (2)C5—H5a0.99
C1—C21.511 (3)C5—H5b0.99
C3—C41.480 (3)C6—H6a0.98
C5—C61.495 (3)C6—H6b0.98
C7—C81.412 (3)C6—H6c0.98
C8—C91.358 (3)C7—H70.95
C9—C101.422 (3)C8—H80.95
C10—C111.415 (3)C9—H90.95
C10—C151.421 (2)C11—H110.95
C11—C121.369 (3)C12—H120.95
C12—C131.421 (3)C13—H130.95
C13—C141.381 (3)
O1—Ti1—O1i72.7 (1)O1—C1—H1b109.2
O1—Ti1—O2104.3 (1)C2—C1—H1b109.2
O1—Ti1—O394.4 (1)H1a—C1—H1b107.9
O1—Ti1—O4156.5 (1)C1—C2—H2a109.5
O1—Ti1—N186.7 (1)C1—C2—H2b109.5
O1i—Ti1—O295.1 (1)H2a—C2—H2b109.5
O1i—Ti1—O3164.1 (1)C1—C2—H2c109.5
O1i—Ti1—O490.9 (1)H2a—C2—H2c109.5
O1i—Ti1—N186.1 (1)H2b—C2—H2c109.5
O2—Ti1—O397.0 (1)O2—C3—H3a109.4
O2—Ti1—O493.6 (1)C4—C3—H3a109.4
O2—Ti1—N1168.8 (1)O2—C3—H3b109.4
O3—Ti1—O498.5 (1)C4—C3—H3b109.4
O3—Ti1—N183.9 (1)H3a—C3—H3b108.0
O4—Ti1—N175.3 (1)C3—C4—H4a109.5
C1—O1—Ti1125.1 (1)C3—C4—H4b109.5
C1—O1—Ti1i127.5 (1)H4a—C4—H4b109.5
Ti1—O1—Ti1i107.3 (1)C3—C4—H4c109.5
C3—O2—Ti1130.7 (1)H4a—C4—H4c109.5
C5—O3—Ti1151.6 (1)H4b—C4—H4c109.5
C14—O4—Ti1121.1 (1)O3—C5—H5a109.3
C7—N1—C15118.5 (2)C6—C5—H5a109.3
C7—N1—Ti1131.0 (1)O3—C5—H5b109.3
C15—N1—Ti1109.8 (1)C6—C5—H5b109.3
O1—C1—C2112.1 (2)H5a—C5—H5b107.9
O2—C3—C4111.0 (2)C5—C6—H6a109.5
O3—C5—C6111.8 (2)C5—C6—H6b109.5
N1—C7—C8122.3 (2)H6a—C6—H6b109.5
C9—C8—C7119.9 (2)C5—C6—H6c109.5
C8—C9—C10120.1 (2)H6a—C6—H6c109.5
C11—C10—C15118.0 (2)H6b—C6—H6c109.5
C11—C10—C9125.8 (2)N1—C7—H7118.8
C15—C10—C9116.2 (2)C8—C7—H7118.8
C12—C11—C10119.9 (2)C9—C8—H8120.1
C11—C12—C13122.2 (2)C7—C8—H8120.1
C14—C13—C12119.8 (2)C8—C9—H9119.9
O4—C14—C13124.7 (2)C10—C9—H9119.9
O4—C14—C15117.0 (2)C12—C11—H11120.1
C13—C14—C15118.3 (2)C10—C11—H11120.1
N1—C15—C10123.1 (2)C11—C12—H12118.9
N1—C15—C14115.2 (2)C13—C12—H12118.9
C10—C15—C14121.8 (2)C14—C13—H13120.1
O1—C1—H1a109.2C12—C13—H13120.1
C2—C1—H1a109.2
O3—Ti1—O1—C112.2 (1)O1—Ti1—N1—C15175.4 (1)
O2—Ti1—O1—C186.2 (1)O1i—Ti1—N1—C15102.5 (1)
O4—Ti1—O1—C1135.4 (2)Ti1—O1—C1—C276.3 (2)
O1i—Ti1—O1—C1177.2 (2)Ti1i—O1—C1—C2100.4 (2)
N1—Ti1—O1—C195.8 (1)Ti1—O2—C3—C4158.4 (2)
O3—Ti1—O1—Ti1i170.6 (1)Ti1—O3—C5—C683.7 (3)
O2—Ti1—O1—Ti1i91.0 (1)C15—N1—C7—C81.2 (3)
O4—Ti1—O1—Ti1i47.4 (2)Ti1—N1—C7—C8167.8 (1)
O1i—Ti1—O1—Ti1i0.0N1—C7—C8—C91.1 (3)
N1—Ti1—O1—Ti1i87.0 (1)C7—C8—C9—C100.2 (3)
O3—Ti1—O2—C315.2 (2)C8—C9—C10—C11179.9 (2)
O4—Ti1—O2—C383.8 (2)C8—C9—C10—C151.3 (3)
O1—Ti1—O2—C3111.5 (2)C15—C10—C11—C120.6 (3)
O1i—Ti1—O2—C3175.1 (2)C9—C10—C11—C12178.2 (2)
N1—Ti1—O2—C379.1 (4)C10—C11—C12—C130.4 (3)
O2—Ti1—O3—C5140.5 (3)C11—C12—C13—C140.0 (3)
O4—Ti1—O3—C545.8 (3)Ti1—O4—C14—C13168.8 (2)
O1—Ti1—O3—C5114.5 (3)Ti1—O4—C14—C1511.0 (2)
O1i—Ti1—O3—C579.8 (3)C12—C13—C14—O4179.9 (2)
N1—Ti1—O3—C528.3 (3)C12—C13—C14—C150.1 (3)
O3—Ti1—O4—C1469.8 (1)C7—N1—C15—C100.1 (3)
O2—Ti1—O4—C14167.4 (1)Ti1—N1—C15—C10171.2 (1)
O1—Ti1—O4—C1452.7 (2)C7—N1—C15—C14179.8 (2)
O1i—Ti1—O4—C1497.4 (1)Ti1—N1—C15—C148.6 (2)
N1—Ti1—O4—C1411.6 (1)C11—C10—C15—N1179.9 (2)
O3—Ti1—N1—C779.9 (2)C9—C10—C15—N11.2 (3)
O2—Ti1—N1—C7175.4 (3)C11—C10—C15—C140.4 (3)
O4—Ti1—N1—C7179.7 (2)C9—C10—C15—C14178.5 (2)
O1—Ti1—N1—C714.9 (2)O4—C14—C15—N10.0 (2)
O1i—Ti1—N1—C787.7 (2)C13—C14—C15—N1179.8 (2)
O3—Ti1—N1—C1589.9 (1)O4—C14—C15—C10179.7 (2)
O2—Ti1—N1—C155.7 (4)C13—C14—C15—C100.0 (3)
O4—Ti1—N1—C1510.6 (1)
Symmetry code: (i) x+1, y+1, z+1.
 

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