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The Ti atom in the title compound, [Ti(C6H7)2(C7H4O3)], is four-coordinate; the salicylate ligand chelates to it to form a six-membered ring.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806039675/ng2113sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806039675/ng2113Isup2.hkl
Contains datablock I

CCDC reference: 613545

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.050
  • wR factor = 0.160
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 3113.00 Ang-3 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C19
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 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Bis(η5-methylcyclopentadienyl)(salicylato-κ2O,O')titanium(IV) top
Crystal data top
[Ti(C6H7)2(C7H4O3)]Dx = 1.460 Mg m3
Mr = 342.23Melting point: 427.65 K
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 2747 reflections
a = 15.768 (9) Åθ = 2.5–25.0°
b = 12.437 (7) ŵ = 0.56 mm1
c = 15.877 (9) ÅT = 298 K
V = 3113 (3) Å3Plate, dark red
Z = 80.49 × 0.46 × 0.17 mm
F(000) = 1424
Data collection top
Bruker APEX CCD area-detector
diffractometer
2747 independent reflections
Radiation source: fine-focus sealed tube1507 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.099
φ and ω scansθmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 1718
Tmin = 0.770, Tmax = 0.911k = 1114
15353 measured reflectionsl = 1518
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)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.160H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0654P)2 + 2.9187P]
where P = (Fo2 + 2Fc2)/3
2747 reflections(Δ/σ)max < 0.001
209 parametersΔρmax = 0.38 e Å3
0 restraintsΔρmin = 0.46 e Å3
Special details top

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
Ti10.25584 (5)0.82278 (6)0.49136 (4)0.0304 (3)
O10.17303 (19)0.7062 (2)0.49507 (19)0.0403 (8)
O20.0655 (2)0.6029 (3)0.4578 (3)0.0608 (11)
O30.17370 (19)0.9048 (2)0.42950 (18)0.0352 (8)
C10.1091 (3)0.6832 (4)0.4465 (3)0.0382 (12)
C20.0893 (3)0.7579 (4)0.3760 (3)0.0354 (11)
C30.1225 (3)0.8630 (4)0.3706 (3)0.0333 (11)
C40.0983 (3)0.9272 (4)0.3023 (3)0.0438 (12)
H40.11790.99760.29880.053*
C50.0460 (3)0.8879 (5)0.2404 (3)0.0534 (14)
H50.03170.93170.19510.064*
C60.0144 (3)0.7847 (5)0.2442 (3)0.0514 (14)
H60.02070.75840.20190.062*
C70.0357 (3)0.7218 (4)0.3116 (3)0.0479 (13)
H70.01380.65250.31470.058*
C80.3358 (3)0.8513 (4)0.3630 (3)0.0391 (12)
C90.3012 (3)0.7469 (4)0.3587 (3)0.0422 (12)
H90.26130.72330.31970.051*
C100.3371 (3)0.6846 (4)0.4233 (3)0.0443 (12)
H100.32570.61260.43420.053*
C110.3929 (3)0.7499 (4)0.4682 (3)0.0431 (12)
H110.42550.72900.51410.052*
C120.3909 (3)0.8537 (4)0.4314 (3)0.0396 (12)
H120.42140.91330.44980.048*
C130.3188 (3)0.9417 (4)0.3034 (3)0.0614 (16)
H13A0.27870.91880.26170.092*
H13B0.37070.96250.27640.092*
H13C0.29611.00180.33400.092*
C140.1848 (3)0.9167 (4)0.6047 (3)0.0446 (13)
C150.2130 (4)0.8191 (4)0.6362 (3)0.0512 (14)
H150.17840.76430.65640.061*
C160.3017 (4)0.8160 (5)0.6327 (3)0.0558 (15)
H160.33580.75880.64950.067*
C170.3299 (3)0.9126 (5)0.6000 (3)0.0520 (15)
H170.38620.93240.59150.062*
C180.2589 (4)0.9747 (4)0.5822 (3)0.0492 (13)
H180.25981.04340.55910.059*
C190.0958 (4)0.9530 (6)0.5959 (4)0.081 (2)
H19A0.09481.02390.57200.121*
H19B0.06930.95440.65030.121*
H19C0.06570.90440.55970.121*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0336 (5)0.0303 (5)0.0272 (5)0.0021 (4)0.0013 (3)0.0016 (3)
O10.0382 (19)0.0382 (19)0.045 (2)0.0059 (14)0.0001 (15)0.0078 (15)
O20.055 (2)0.041 (2)0.087 (3)0.019 (2)0.001 (2)0.010 (2)
O30.0436 (19)0.0296 (17)0.0323 (17)0.0010 (14)0.0003 (14)0.0028 (14)
C10.031 (3)0.034 (3)0.049 (3)0.003 (2)0.009 (2)0.006 (2)
C20.027 (2)0.042 (3)0.037 (3)0.004 (2)0.0051 (19)0.004 (2)
C30.030 (3)0.037 (3)0.032 (3)0.000 (2)0.002 (2)0.003 (2)
C40.043 (3)0.042 (3)0.047 (3)0.003 (2)0.003 (2)0.004 (2)
C50.046 (3)0.068 (4)0.046 (3)0.010 (3)0.012 (2)0.005 (3)
C60.039 (3)0.065 (4)0.051 (3)0.001 (3)0.016 (2)0.008 (3)
C70.035 (3)0.051 (3)0.058 (4)0.004 (2)0.002 (2)0.013 (3)
C80.039 (3)0.049 (3)0.029 (3)0.005 (2)0.011 (2)0.001 (2)
C90.039 (3)0.054 (3)0.034 (3)0.003 (3)0.006 (2)0.014 (2)
C100.044 (3)0.035 (3)0.054 (3)0.002 (2)0.010 (2)0.003 (3)
C110.037 (3)0.047 (3)0.045 (3)0.009 (3)0.005 (2)0.005 (3)
C120.033 (3)0.046 (3)0.041 (3)0.006 (2)0.006 (2)0.001 (2)
C130.059 (4)0.070 (4)0.055 (4)0.002 (3)0.012 (3)0.024 (3)
C140.052 (3)0.058 (4)0.025 (3)0.009 (3)0.007 (2)0.010 (2)
C150.069 (4)0.060 (4)0.025 (3)0.009 (3)0.012 (2)0.003 (3)
C160.065 (4)0.074 (4)0.028 (3)0.012 (3)0.008 (2)0.001 (3)
C170.052 (3)0.079 (4)0.026 (3)0.014 (3)0.004 (2)0.014 (3)
C180.076 (4)0.042 (3)0.029 (3)0.008 (3)0.001 (3)0.010 (2)
C190.068 (4)0.122 (6)0.053 (4)0.027 (4)0.014 (3)0.016 (4)
Geometric parameters (Å, º) top
Ti1—O31.919 (3)C8—C121.391 (6)
Ti1—O11.952 (3)C8—C91.410 (6)
Ti1—C162.359 (5)C8—C131.493 (6)
Ti1—C172.364 (5)C9—C101.405 (7)
Ti1—C122.365 (5)C9—H90.9300
Ti1—C112.372 (5)C10—C111.392 (7)
Ti1—C182.377 (5)C10—H100.9300
Ti1—C152.397 (5)C11—C121.418 (6)
Ti1—C102.400 (5)C11—H110.9300
Ti1—C92.416 (4)C12—H120.9300
Ti1—C142.420 (4)C13—H13A0.9600
Ti1—C82.423 (4)C13—H13B0.9600
O1—C11.301 (5)C13—H13C0.9600
O2—C11.226 (5)C14—C151.385 (7)
O3—C31.340 (5)C14—C181.419 (7)
C1—C21.487 (6)C14—C191.481 (7)
C2—C71.401 (6)C15—C161.401 (7)
C2—C31.412 (6)C15—H150.9300
C3—C41.400 (6)C16—C171.382 (7)
C4—C51.372 (7)C16—H160.9300
C4—H40.9300C17—C181.390 (7)
C5—C61.379 (7)C17—H170.9300
C5—H50.9300C18—H180.9300
C6—C71.367 (7)C19—H19A0.9600
C6—H60.9300C19—H19B0.9600
C7—H70.9300C19—H19C0.9600
O3—Ti1—O187.66 (13)C4—C5—H5119.4
O3—Ti1—C16135.46 (17)C6—C5—H5119.4
O1—Ti1—C1698.61 (18)C7—C6—C5118.6 (5)
O3—Ti1—C17117.12 (18)C7—C6—H6120.7
O1—Ti1—C17131.26 (16)C5—C6—H6120.7
C16—Ti1—C1734.03 (17)C6—C7—C2122.5 (5)
O3—Ti1—C12108.38 (15)C6—C7—H7118.8
O1—Ti1—C12137.34 (15)C2—C7—H7118.8
C16—Ti1—C1296.46 (19)C12—C8—C9107.4 (4)
C17—Ti1—C1276.80 (18)C12—C8—C13126.2 (5)
O3—Ti1—C11137.61 (15)C9—C8—C13126.3 (5)
O1—Ti1—C11109.26 (16)C12—C8—Ti170.8 (2)
C16—Ti1—C1181.63 (19)C9—C8—Ti172.8 (3)
C17—Ti1—C1181.00 (19)C13—C8—Ti1123.3 (3)
C12—Ti1—C1134.84 (16)C10—C9—C8108.5 (4)
O3—Ti1—C1884.34 (16)C10—C9—Ti172.4 (3)
O1—Ti1—C18125.85 (16)C8—C9—Ti173.3 (3)
C16—Ti1—C1856.32 (19)C10—C9—H9125.8
C17—Ti1—C1834.10 (17)C8—C9—H9125.8
C12—Ti1—C1895.55 (18)Ti1—C9—H9120.2
C11—Ti1—C18112.31 (19)C11—C10—C9107.9 (4)
O3—Ti1—C15108.11 (17)C11—C10—Ti171.9 (3)
O1—Ti1—C1576.60 (16)C9—C10—Ti173.7 (3)
C16—Ti1—C1534.25 (18)C11—C10—H10126.1
C17—Ti1—C1556.52 (19)C9—C10—H10126.1
C12—Ti1—C15130.04 (18)Ti1—C10—H10120.2
C11—Ti1—C15113.47 (18)C10—C11—C12107.8 (4)
C18—Ti1—C1555.88 (18)C10—C11—Ti174.2 (3)
O3—Ti1—C10120.70 (16)C12—C11—Ti172.3 (3)
O1—Ti1—C1080.73 (16)C10—C11—H11126.1
C16—Ti1—C10103.81 (19)C12—C11—H11126.1
C17—Ti1—C10113.74 (19)Ti1—C11—H11119.3
C12—Ti1—C1056.93 (17)C8—C12—C11108.4 (4)
C11—Ti1—C1033.92 (16)C8—C12—Ti175.4 (3)
C18—Ti1—C10146.21 (19)C11—C12—Ti172.9 (3)
C15—Ti1—C10124.65 (19)C8—C12—H12125.8
O3—Ti1—C987.78 (15)C11—C12—H12125.8
O1—Ti1—C986.24 (15)Ti1—C12—H12117.9
C16—Ti1—C9136.41 (19)C8—C13—H13A109.5
C17—Ti1—C9132.39 (17)C8—C13—H13B109.5
C12—Ti1—C956.34 (16)H13A—C13—H13B109.5
C11—Ti1—C956.34 (16)C8—C13—H13C109.5
C18—Ti1—C9146.41 (18)H13A—C13—H13C109.5
C15—Ti1—C9155.81 (19)H13B—C13—H13C109.5
C10—Ti1—C933.91 (16)C15—C14—C18105.8 (5)
O3—Ti1—C1479.16 (15)C15—C14—C19127.3 (5)
O1—Ti1—C1491.52 (16)C18—C14—C19126.9 (5)
C16—Ti1—C1456.76 (18)C15—C14—Ti172.4 (3)
C17—Ti1—C1457.18 (18)C18—C14—Ti171.1 (3)
C12—Ti1—C14129.63 (17)C19—C14—Ti1121.0 (3)
C11—Ti1—C14136.16 (17)C14—C15—C16109.3 (5)
C18—Ti1—C1434.39 (16)C14—C15—Ti174.2 (3)
C15—Ti1—C1433.42 (16)C16—C15—Ti171.4 (3)
C10—Ti1—C14157.99 (18)C14—C15—H15125.4
C9—Ti1—C14166.83 (17)C16—C15—H15125.4
O3—Ti1—C880.96 (14)Ti1—C15—H15120.7
O1—Ti1—C8118.85 (15)C17—C16—C15108.2 (5)
C16—Ti1—C8130.20 (19)C17—C16—Ti173.2 (3)
C17—Ti1—C8106.69 (18)C15—C16—Ti174.4 (3)
C12—Ti1—C833.75 (15)C17—C16—H16125.9
C11—Ti1—C856.72 (16)C15—C16—H16125.9
C18—Ti1—C8112.53 (18)Ti1—C16—H16118.5
C15—Ti1—C8163.02 (18)C16—C17—C18107.5 (5)
C10—Ti1—C856.52 (17)C16—C17—Ti172.8 (3)
C9—Ti1—C833.89 (15)C18—C17—Ti173.5 (3)
C14—Ti1—C8142.73 (18)C16—C17—H17126.3
C1—O1—Ti1131.5 (3)C18—C17—H17126.3
C3—O3—Ti1123.9 (3)Ti1—C17—H17119.4
O2—C1—O1121.7 (5)C17—C18—C14109.2 (5)
O2—C1—C2120.1 (5)C17—C18—Ti172.4 (3)
O1—C1—C2118.2 (4)C14—C18—Ti174.5 (3)
C7—C2—C3118.4 (4)C17—C18—H18125.4
C7—C2—C1118.5 (4)C14—C18—H18125.4
C3—C2—C1123.1 (4)Ti1—C18—H18119.5
O3—C3—C4118.9 (4)C14—C19—H19A109.5
O3—C3—C2122.7 (4)C14—C19—H19B109.5
C4—C3—C2118.3 (4)H19A—C19—H19B109.5
C5—C4—C3121.0 (5)C14—C19—H19C109.5
C5—C4—H4119.5H19A—C19—H19C109.5
C3—C4—H4119.5H19B—C19—H19C109.5
C4—C5—C6121.2 (5)
 

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