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The title compound, [Ti(C23H15)Cl3], has the triphenyl-substituted cyclo­penta­diene ring π-bonded to the TiCl3 fragment. The phenyl rings subtend dihedral angles in the range 10.8 (2)–40.2 (3)° with the cyclo­penta­diene ring.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680701269X/sj2249sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680701269X/sj2249Isup2.hkl
Contains datablock I

CCDC reference: 639514

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.054
  • wR factor = 0.142
  • Data-to-parameter ratio = 19.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ti1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003) and Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXL97.

Trichlorido(η5-1,2,4-triphenylcyclopentadienyl)titanium(IV) top
Crystal data top
[Ti(C23H15)Cl3]F(000) = 904
Mr = 445.60Dx = 1.430 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 12742 reflections
a = 11.298 (2) Åθ = 6.2–54.9°
b = 16.340 (3) ŵ = 0.81 mm1
c = 12.481 (3) ÅT = 295 K
β = 116.08 (3)°Block, red
V = 2069.6 (7) Å30.25 × 0.19 × 0.17 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID CCD area-detector
diffractometer
2948 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.061
Graphite monochromatorθmax = 27.5°, θmin = 3.1°
ω scansh = 1414
20121 measured reflectionsk = 2121
4723 independent 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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0592P)2 + 1.089P]
where P = (Fo2 + 2Fc2)/3
4723 reflections(Δ/σ)max < 0.001
244 parametersΔρmax = 0.64 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
Ti10.28742 (6)0.15816 (3)0.47112 (5)0.04088 (18)
Cl10.49158 (11)0.12463 (7)0.50419 (15)0.0912 (4)
Cl20.32108 (11)0.27815 (5)0.56202 (10)0.0649 (3)
Cl30.19358 (15)0.18915 (9)0.27884 (10)0.1084 (6)
C10.0855 (3)0.10811 (18)0.4651 (3)0.0380 (7)
C20.1408 (3)0.04402 (18)0.4236 (3)0.0398 (7)
C30.2640 (3)0.02262 (19)0.5172 (3)0.0418 (7)
C40.2864 (3)0.07119 (18)0.6187 (3)0.0395 (7)
C50.1770 (3)0.12494 (18)0.5856 (3)0.0391 (7)
C60.0444 (3)0.14989 (19)0.4061 (3)0.0437 (7)
C70.1085 (4)0.1694 (2)0.4752 (4)0.0583 (10)
H70.06880.15820.55650.070*
C80.2317 (4)0.2055 (3)0.4229 (5)0.0777 (13)
H80.27530.21700.46930.093*
C90.2904 (4)0.2244 (3)0.3046 (5)0.0876 (16)
H90.37260.24950.27070.105*
C100.2271 (5)0.2060 (3)0.2366 (4)0.0816 (14)
H100.26650.21900.15580.098*
C110.1053 (4)0.1683 (2)0.2860 (3)0.0637 (11)
H110.06410.15520.23810.076*
C120.0831 (3)0.00116 (19)0.3079 (3)0.0434 (8)
C130.0495 (3)0.02247 (19)0.2552 (3)0.0483 (8)
H130.10450.00400.28780.058*
C140.0998 (4)0.0712 (2)0.1542 (4)0.0606 (10)
H140.18820.08600.12000.073*
C150.0207 (5)0.0978 (3)0.1044 (4)0.0749 (12)
H150.05540.12990.03590.090*
C160.1104 (5)0.0768 (3)0.1560 (4)0.0817 (14)
H160.16480.09480.12250.098*
C170.1616 (4)0.0288 (3)0.2578 (4)0.0660 (11)
H170.25050.01510.29250.079*
C180.4014 (3)0.06772 (19)0.7364 (3)0.0423 (7)
C190.4919 (4)0.0041 (2)0.7654 (4)0.0583 (10)
H190.48100.03680.70990.070*
C200.5976 (4)0.0017 (3)0.8765 (4)0.0718 (12)
H200.65790.04100.89500.086*
C210.6160 (4)0.0600 (3)0.9599 (4)0.0635 (10)
H210.68770.05711.03470.076*
C220.5276 (4)0.1235 (2)0.9325 (3)0.0618 (10)
H220.53940.16390.98870.074*
C230.4215 (3)0.1272 (2)0.8216 (3)0.0530 (9)
H230.36240.17050.80370.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0409 (3)0.0406 (3)0.0462 (3)0.0042 (2)0.0238 (3)0.0001 (2)
Cl10.0661 (7)0.0696 (7)0.1698 (13)0.0001 (5)0.0812 (8)0.0071 (7)
Cl20.0860 (7)0.0384 (4)0.0839 (7)0.0041 (4)0.0498 (6)0.0040 (4)
Cl30.1267 (11)0.1341 (11)0.0489 (6)0.0746 (9)0.0242 (7)0.0129 (6)
C10.0334 (16)0.0417 (16)0.0400 (17)0.0003 (12)0.0173 (14)0.0061 (13)
C20.0364 (17)0.0405 (16)0.0459 (18)0.0036 (12)0.0212 (14)0.0017 (13)
C30.0361 (17)0.0382 (16)0.0476 (19)0.0012 (13)0.0152 (15)0.0014 (13)
C40.0354 (16)0.0390 (16)0.0456 (18)0.0004 (13)0.0192 (14)0.0071 (13)
C50.0343 (16)0.0433 (16)0.0421 (17)0.0027 (13)0.0191 (14)0.0095 (13)
C60.0355 (17)0.0412 (16)0.051 (2)0.0011 (13)0.0157 (15)0.0035 (14)
C70.045 (2)0.069 (2)0.063 (2)0.0107 (17)0.0262 (19)0.0091 (18)
C80.052 (2)0.090 (3)0.091 (3)0.024 (2)0.031 (2)0.005 (3)
C90.047 (2)0.094 (3)0.091 (4)0.025 (2)0.002 (3)0.000 (3)
C100.073 (3)0.087 (3)0.057 (3)0.025 (2)0.003 (2)0.002 (2)
C110.059 (2)0.071 (2)0.048 (2)0.0157 (19)0.0110 (18)0.0014 (18)
C120.0427 (19)0.0403 (16)0.0457 (19)0.0046 (13)0.0180 (15)0.0012 (13)
C130.0423 (19)0.0450 (17)0.053 (2)0.0042 (15)0.0166 (16)0.0022 (15)
C140.049 (2)0.058 (2)0.061 (2)0.0120 (17)0.0109 (19)0.0052 (18)
C150.080 (3)0.069 (3)0.067 (3)0.015 (2)0.024 (2)0.025 (2)
C160.071 (3)0.097 (3)0.085 (3)0.013 (2)0.041 (3)0.041 (3)
C170.050 (2)0.076 (3)0.075 (3)0.0107 (19)0.030 (2)0.025 (2)
C180.0374 (17)0.0449 (17)0.0436 (18)0.0041 (13)0.0169 (15)0.0083 (14)
C190.053 (2)0.053 (2)0.058 (2)0.0127 (17)0.0142 (18)0.0004 (17)
C200.058 (3)0.063 (2)0.074 (3)0.0240 (19)0.010 (2)0.012 (2)
C210.049 (2)0.076 (3)0.051 (2)0.0077 (19)0.0089 (18)0.0055 (19)
C220.049 (2)0.073 (2)0.052 (2)0.0064 (19)0.0121 (18)0.0079 (19)
C230.0418 (19)0.059 (2)0.052 (2)0.0098 (16)0.0150 (17)0.0002 (16)
Geometric parameters (Å, º) top
Ti1—Cl22.2129 (11)C10—H100.9300
Ti1—Cl32.2142 (15)C11—H110.9300
Ti1—Cl12.2258 (13)C12—C171.366 (5)
Ti1—C42.331 (3)C12—C131.391 (5)
Ti1—C32.332 (3)C13—C141.384 (5)
Ti1—C52.337 (3)C13—H130.9300
Ti1—C22.390 (3)C14—C151.364 (6)
Ti1—C12.393 (3)C14—H140.9300
C1—C51.428 (4)C15—C161.375 (6)
C1—C21.428 (4)C15—H150.9300
C1—C61.488 (4)C16—C171.385 (5)
C2—C31.412 (4)C16—H160.9300
C2—C121.493 (4)C17—H170.9300
C3—C41.421 (5)C18—C231.384 (5)
C4—C51.422 (4)C18—C191.390 (5)
C4—C181.474 (4)C19—C201.377 (5)
C6—C111.380 (5)C19—H190.9300
C6—C71.385 (5)C20—C211.358 (6)
C7—C81.383 (5)C20—H200.9300
C7—H70.9300C21—C221.375 (5)
C8—C91.362 (7)C21—H210.9300
C8—H80.9300C22—C231.377 (5)
C9—C101.362 (7)C22—H220.9300
C9—H90.9300C23—H230.9300
C10—C111.381 (6)
Cl2—Ti1—Cl3104.21 (6)C11—C6—C1123.4 (3)
Cl2—Ti1—Cl1101.10 (5)C7—C6—C1118.0 (3)
Cl3—Ti1—Cl1102.75 (7)C8—C7—C6119.9 (4)
Cl2—Ti1—C4101.21 (9)C8—C7—H7120.1
Cl3—Ti1—C4146.07 (9)C6—C7—H7120.1
Cl1—Ti1—C493.92 (9)C9—C8—C7121.2 (5)
Cl2—Ti1—C3136.69 (9)C9—C8—H8119.4
Cl3—Ti1—C3115.61 (9)C7—C8—H8119.4
Cl1—Ti1—C386.62 (9)C8—C9—C10119.1 (4)
C4—Ti1—C335.48 (11)C8—C9—H9120.4
Cl2—Ti1—C584.83 (9)C10—C9—H9120.4
Cl3—Ti1—C5125.86 (9)C9—C10—C11120.9 (4)
Cl1—Ti1—C5128.16 (9)C9—C10—H10119.6
C4—Ti1—C535.46 (10)C11—C10—H10119.6
C3—Ti1—C558.66 (11)C6—C11—C10120.4 (4)
Cl2—Ti1—C2139.73 (9)C6—C11—H11119.8
Cl3—Ti1—C287.71 (9)C10—C11—H11119.8
Cl1—Ti1—C2113.75 (8)C17—C12—C13118.8 (3)
C4—Ti1—C258.44 (11)C17—C12—C2120.7 (3)
C3—Ti1—C234.78 (10)C13—C12—C2120.2 (3)
C5—Ti1—C258.15 (11)C14—C13—C12120.0 (4)
Cl2—Ti1—C1105.39 (8)C14—C13—H13120.0
Cl3—Ti1—C192.78 (9)C12—C13—H13120.0
Cl1—Ti1—C1144.84 (8)C15—C14—C13120.6 (4)
C4—Ti1—C158.70 (11)C15—C14—H14119.7
C3—Ti1—C158.23 (11)C13—C14—H14119.7
C5—Ti1—C135.11 (11)C14—C15—C16119.6 (4)
C2—Ti1—C134.75 (10)C14—C15—H15120.2
C5—C1—C2107.1 (3)C16—C15—H15120.2
C5—C1—C6122.2 (3)C15—C16—C17120.0 (4)
C2—C1—C6130.6 (3)C15—C16—H16120.0
C5—C1—Ti170.30 (17)C17—C16—H16120.0
C2—C1—Ti172.48 (17)C12—C17—C16120.9 (4)
C6—C1—Ti1125.3 (2)C12—C17—H17119.5
C3—C2—C1108.1 (3)C16—C17—H17119.5
C3—C2—C12122.0 (3)C23—C18—C19118.2 (3)
C1—C2—C12129.7 (3)C23—C18—C4120.9 (3)
C3—C2—Ti170.38 (17)C19—C18—C4120.9 (3)
C1—C2—Ti172.76 (17)C20—C19—C18119.8 (4)
C12—C2—Ti1125.9 (2)C20—C19—H19120.1
C2—C3—C4108.9 (3)C18—C19—H19120.1
C2—C3—Ti174.83 (17)C21—C20—C19121.6 (4)
C4—C3—Ti172.21 (17)C21—C20—H20119.2
C3—C4—C5107.1 (3)C19—C20—H20119.2
C3—C4—C18126.9 (3)C20—C21—C22119.3 (4)
C5—C4—C18125.9 (3)C20—C21—H21120.4
C3—C4—Ti172.30 (18)C22—C21—H21120.4
C5—C4—Ti172.51 (17)C21—C22—C23120.0 (4)
C18—C4—Ti1120.2 (2)C21—C22—H22120.0
C4—C5—C1108.7 (3)C23—C22—H22120.0
C4—C5—Ti172.03 (18)C22—C23—C18121.1 (3)
C1—C5—Ti174.59 (18)C22—C23—H23119.4
C11—C6—C7118.6 (3)C18—C23—H23119.4
 

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