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A new polynuclear titanium(IV) complex, dichloro­deca-[mu]2-oxo-hexa­kis­(penta­methyl­cyclo­penta­dien­yl)hexa­titanium(IV), [Ti6(C10H15)6Cl2O10], has been synthesized by hydro­lysis of a titanium complex bearing an N-(2-hydr­oxy-3,5-dimethyl­benz­yl)diethano­lamine Mannich ligand. The mol­ecule has two O-bridged Ti3O3 rings linked to two similar rings through a tetra­hedrally O-coordinated Ti atom. All Ti atoms except the central one are coordinated to penta­methyl­cyclo­penta­dien­yl (Cp*) ligands. The Cp* ligands are arranged with approximate \overline{3} symmetry with respect to the Ti/O/Cl core.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105016021/ta1483sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105016021/ta1483Isup2.hkl
Contains datablock I

CCDC reference: 278540

Comment top

In recent years, organometallic oxides have received considerable interest as hydrocarbon-soluble models for metal oxide surfaces and thus help to provide a basic understanding of catalyst-to-support interactions in heterogeneous catalytic processes (Bottomley, 1992; Pop & Müller, 1991; Bottomley & Sutin, 1988; Day & Klemperer, 1985). Previously, chain and ring polyhedral organotitanoxanes with frameworks have been well established, starting from [Cp*TiCl3] (Cp* is η5-C5H5-nRn, R is Me, SiMe3 or tBu, and n = 0, 1, 2, 3, 4, 5) (Pilar et al., 1995; Carofiglio et al., 1992; Babcock et al., 1987). However, few organotitanoxanes have been obtained from other complexes. Hence, our work has been aimed at synthesizing new polynuclear organotitanoxanes starting from some complicated complexes. We report here the synthesis and crystal structure of the first such species, (I), [(Cp*TiCl)(µ-O)2(Cp*Ti)2(µ-O)(µ-O)2]2Ti, (Cp* is η5-C5Me5).

The Ti/O/Cl core of (I), which consists of four fused Ti3O3 rings, is illustrated in Fig. 1. In the complete molecule (Fig. 2), all Ti atoms are in an approximately tetrahedral environment, with atoms Ti1–Ti6 being coordinated to η5-Cp* in a three-legged piano-stool configuration. The Ti atoms are in three distinct stereochemical environments: Ti7 is coordinated to four bridging O atoms (Ob), Ti2, Ti3, Ti5 and Ti6 are coordinated by three Ob atoms plus η5-Cp*, and Ti1 and Ti4 are coordinated by two Ob atoms, one Cl atom and one η5-Cp* ligand.

The ranges of the Ti—O and Ti—Cl bond lengths in (I) (Table 1) are 1.805 (2)–1.857 (2) and 2.291 (1)–2.2919 (1) Å, respectively, which are in the normal ranges (Reference for standard values?). However, the Ti—O distances for Ti atoms bonded to Cl and for Ti7 are somewhat shorter than those found for Ti bonded to three Ob atoms. The atoms of the individual η5-Cp* molecules are coplanar.

When viewed along the b axis, the entire molecule gives a psuedo-hexagonal impression in projection (Fig. 2). The two six-membered core rings, Ti1/Ti2/Ti3/O1/O4/O5 and Ti4/Ti5/Ti6/O6/O7/O10, are in an almost eclipsed conformation but with Ti over O, and the η5-Cp* ligands are arrayed with approximate 3 symmetry with respect to the Ti/O/Cl core. There is a distance of 9.057 (1) Å between Ti1 and Ti4.

Experimental top

Reaction of the titanium complex bearing the N-(3,5-dimethyl-2-hydroxyl-benzyl)diethanolamine Mannich base with an excess of 1.5 M aqueous NH4OH in toluene for 3 d at ambient temperature, followed by filtration to remove NH4Cl, drying over Na2SO4, elution through a basic alumina chromatography column and removal of the solvent under reduced pressure yielded yellow crystals of (I) in 58% yield.

Refinement top

H atoms were placed geometrically and refined with fixed individual displacement parameters [Uiso(H) = 1.5Ueq(C)] using a riding model, with C—H = 0.96 Å.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT-NT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The Ti/Cl/O core of (I). The b axis is approximately horizontal. Displacement ellipsoids are shown at the 50% probability level. The η5-Cp* ligands have been omitted.
[Figure 2] Fig. 2. The structure of (I), viewed parallel to b and along the psuedo 3 axis. Hatched, cross-hatched, stippled and open circles represent Ti, Cl, O and C atoms, respectively.
dichlorodeca-µ2oxo-hexakis(pentamethylcyclopentadienyl)hexatitanium(IV) top
Crystal data top
[Ti6(C10H15)6Cl2O10]F(000) = 2872
Mr = 1377.52Dx = 1.378 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -p 2ynCell parameters from 5764 reflections
a = 11.4724 (14) Åθ = 2.5–25.9°
b = 29.713 (4) ŵ = 0.93 mm1
c = 19.495 (2) ÅT = 293 K
β = 92.090 (2)°Prismatic, pale yellow
V = 6641.0 (14) Å30.28 × 0.26 × 0.10 mm
Z = 4
Data collection top
Bruker CCD area detector
diffractometer
13061 independent reflections
Radiation source: fine-focus sealed tube10417 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ϕ and ω scansθmax = 26.1°, θmin = 1.7°
Absorption correction: multi-scan
(SHELXTL; Bruker, 1997)
h = 1314
Tmin = 0.781, Tmax = 0.917k = 3336
37338 measured reflectionsl = 2413
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0707P)2 + 2.2925P]
where P = (Fo2 + 2Fc2)/3
13061 reflections(Δ/σ)max = 0.025
741 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.24 e Å3
Crystal data top
[Ti6(C10H15)6Cl2O10]V = 6641.0 (14) Å3
Mr = 1377.52Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.4724 (14) ŵ = 0.93 mm1
b = 29.713 (4) ÅT = 293 K
c = 19.495 (2) Å0.28 × 0.26 × 0.10 mm
β = 92.090 (2)°
Data collection top
Bruker CCD area detector
diffractometer
13061 independent reflections
Absorption correction: multi-scan
(SHELXTL; Bruker, 1997)
10417 reflections with I > 2σ(I)
Tmin = 0.781, Tmax = 0.917Rint = 0.026
37338 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0430 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.02Δρmax = 0.44 e Å3
13061 reflectionsΔρmin = 0.24 e Å3
741 parameters
Special details top

Experimental. ? # Insert any comments here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ti10.46047 (4)0.131198 (16)0.80935 (3)0.03300 (12)
Ti20.65825 (4)0.192381 (15)0.73475 (2)0.02873 (12)
Ti30.40357 (4)0.188854 (15)0.66220 (2)0.02974 (12)
Ti40.61233 (4)0.430223 (16)0.82385 (3)0.03380 (12)
Ti50.56635 (4)0.386734 (16)0.66559 (2)0.03226 (12)
Ti60.36817 (4)0.378985 (14)0.77645 (2)0.02737 (11)
Ti70.49954 (4)0.285904 (14)0.72353 (3)0.02983 (12)
Cl10.48555 (9)0.05966 (3)0.76848 (5)0.0649 (2)
Cl20.57476 (9)0.50473 (3)0.80228 (6)0.0728 (3)
O10.60384 (15)0.15546 (6)0.80270 (10)0.0368 (4)
O20.60945 (14)0.24876 (6)0.76182 (10)0.0347 (4)
O30.39368 (16)0.24983 (6)0.67900 (11)0.0436 (5)
O40.37406 (15)0.15968 (7)0.74325 (10)0.0402 (4)
O50.56177 (14)0.18093 (6)0.65929 (9)0.0339 (4)
O60.65095 (15)0.40690 (7)0.74176 (10)0.0414 (5)
O70.46679 (15)0.40921 (6)0.83698 (9)0.0340 (4)
O80.42162 (15)0.32011 (6)0.78346 (9)0.0331 (4)
O90.57357 (17)0.32460 (6)0.66805 (10)0.0441 (5)
O100.41647 (15)0.39644 (6)0.69164 (9)0.0355 (4)
C10.3138 (3)0.15765 (11)0.88104 (17)0.0519 (8)
C20.3121 (3)0.11145 (11)0.88744 (17)0.0525 (8)
C30.4207 (3)0.09740 (11)0.91794 (17)0.0585 (9)
C40.4872 (3)0.13727 (14)0.92984 (16)0.0576 (9)
C50.4205 (3)0.17359 (10)0.90622 (17)0.0527 (8)
C60.2153 (4)0.18615 (17)0.8504 (2)0.1000 (18)
H6A0.24360.20380.81330.150*
H6B0.18640.20580.88500.150*
H6C0.15340.16690.83350.150*
C70.2133 (4)0.07945 (18)0.8667 (3)0.1083 (19)
H7A0.14360.09640.85650.162*
H7B0.20000.05900.90370.162*
H7C0.23420.06280.82680.162*
C80.4538 (5)0.05024 (15)0.9388 (3)0.118 (2)
H8A0.44580.04680.98740.176*
H8B0.53320.04460.92750.176*
H8C0.40350.02920.91480.176*
C90.6077 (4)0.1400 (2)0.9626 (2)0.115 (2)
H9A0.65550.15910.93560.173*
H9B0.64140.11050.96510.173*
H9C0.60330.15221.00800.173*
C100.4569 (5)0.22256 (13)0.9100 (2)0.1005 (18)
H10A0.42750.23810.86970.151*
H10B0.54040.22450.91250.151*
H10C0.42570.23620.95000.151*
C110.8422 (2)0.22504 (10)0.71677 (18)0.0447 (7)
C120.8547 (2)0.19688 (11)0.77457 (17)0.0447 (7)
C130.8369 (2)0.15204 (10)0.75244 (17)0.0424 (7)
C140.8105 (2)0.15271 (10)0.68148 (17)0.0424 (7)
C150.8141 (2)0.19782 (10)0.65915 (17)0.0435 (7)
C160.8584 (3)0.27516 (11)0.7151 (3)0.0760 (13)
H16A0.90460.28310.67690.114*
H16B0.89740.28480.75700.114*
H16C0.78370.28960.71050.114*
C170.8799 (3)0.21216 (14)0.8473 (2)0.0725 (11)
H17A0.86490.18790.87830.109*
H17B0.83060.23720.85740.109*
H17C0.96010.22110.85250.109*
C180.8439 (3)0.11073 (12)0.7974 (2)0.0689 (11)
H18A0.78650.08920.78160.103*
H18B0.82920.11900.84390.103*
H18C0.92020.09770.79540.103*
C190.7833 (3)0.11266 (12)0.6366 (2)0.0692 (11)
H19A0.85430.10080.61930.104*
H19B0.73230.12160.59890.104*
H19C0.74580.08990.66300.104*
C200.7929 (3)0.21385 (14)0.5869 (2)0.0718 (11)
H20A0.76400.24420.58740.108*
H20B0.73640.19470.56400.108*
H20C0.86460.21290.56310.108*
C210.2611 (3)0.13780 (10)0.61476 (17)0.0498 (8)
C220.2163 (2)0.18225 (11)0.60688 (16)0.0446 (7)
C230.2883 (3)0.20538 (10)0.56213 (15)0.0427 (7)
C240.3781 (2)0.17571 (11)0.54325 (15)0.0459 (7)
C250.3609 (3)0.13433 (10)0.57593 (17)0.0497 (8)
C260.2078 (4)0.10166 (14)0.6570 (2)0.0920 (16)
H26A0.16240.08190.62760.138*
H26B0.15830.11510.69000.138*
H26C0.26840.08480.68050.138*
C270.1121 (3)0.20123 (16)0.6406 (2)0.0799 (13)
H27A0.13470.21190.68560.120*
H27B0.05390.17820.64410.120*
H27C0.08100.22570.61360.120*
C280.2714 (4)0.25299 (12)0.5378 (2)0.0724 (11)
H28A0.26300.25340.48870.109*
H28B0.33790.27070.55220.109*
H28C0.20250.26530.55720.109*
C290.4731 (3)0.18607 (18)0.4953 (2)0.0852 (14)
H29A0.54740.18020.51780.128*
H29B0.46870.21720.48220.128*
H29C0.46430.16750.45520.128*
C300.4350 (4)0.09287 (13)0.5685 (2)0.0908 (16)
H30A0.43320.07540.60980.136*
H30B0.51380.10160.56040.136*
H30C0.40500.07520.53050.136*
C310.7985 (3)0.40348 (12)0.86303 (17)0.0513 (8)
C320.7918 (3)0.44805 (11)0.8853 (2)0.0582 (9)
C330.7021 (3)0.45101 (12)0.93175 (19)0.0611 (10)
C340.6529 (3)0.40822 (13)0.93863 (16)0.0555 (9)
C350.7109 (3)0.37886 (10)0.89457 (18)0.0488 (8)
C360.8844 (3)0.38527 (16)0.8136 (2)0.0844 (13)
H36A0.94020.40820.80340.127*
H36B0.84370.37620.77190.127*
H36C0.92420.35980.83370.127*
C370.8703 (4)0.48653 (16)0.8641 (3)0.111 (2)
H37A0.82740.50630.83350.167*
H37B0.93640.47460.84140.167*
H37C0.89660.50290.90420.167*
C380.6698 (5)0.49221 (17)0.9719 (3)0.117 (2)
H38A0.72760.49741.00790.176*
H38B0.59520.48770.99160.176*
H38C0.66590.51780.94190.176*
C390.5553 (4)0.39496 (19)0.9838 (2)0.0996 (17)
H39A0.58400.37421.01820.149*
H39B0.49420.38090.95650.149*
H39C0.52520.42131.00560.149*
C400.6848 (4)0.32986 (12)0.8855 (2)0.0828 (14)
H40A0.70680.32050.84060.124*
H40B0.60280.32480.89020.124*
H40C0.72800.31290.91970.124*
C410.7073 (3)0.39725 (13)0.58077 (18)0.0576 (9)
C420.6085 (4)0.37819 (13)0.54875 (17)0.0610 (9)
C430.5171 (3)0.40864 (14)0.55218 (17)0.0611 (10)
C440.5590 (3)0.44782 (12)0.58670 (18)0.0584 (9)
C450.6778 (3)0.44066 (12)0.60400 (18)0.0569 (9)
C460.8267 (4)0.37556 (18)0.5904 (3)0.1014 (18)
H46A0.81870.34340.58880.152*
H46B0.86090.38430.63410.152*
H46C0.87590.38530.55450.152*
C470.6015 (5)0.33207 (16)0.5159 (2)0.1110 (19)
H47A0.67890.32040.51100.166*
H47B0.56290.33430.47150.166*
H47C0.55840.31220.54430.166*
C480.3936 (4)0.4019 (2)0.5237 (2)0.112 (2)
H48A0.39010.40910.47560.168*
H48B0.34160.42130.54740.168*
H48C0.37080.37110.53000.168*
C490.4905 (5)0.48928 (15)0.6018 (3)0.1007 (17)
H49A0.50360.49750.64900.151*
H49B0.40900.48350.59300.151*
H49C0.51500.51340.57290.151*
C500.7598 (4)0.47297 (16)0.6395 (2)0.1017 (17)
H50A0.83420.45880.64740.153*
H50B0.72890.48170.68260.153*
H50C0.76880.49910.61130.153*
C510.2115 (2)0.38909 (13)0.85059 (17)0.0519 (8)
C520.1852 (2)0.35118 (10)0.8078 (2)0.0520 (9)
C530.1718 (2)0.36773 (11)0.73973 (17)0.0439 (7)
C540.1875 (2)0.41429 (11)0.74202 (18)0.0480 (8)
C550.2127 (3)0.42708 (11)0.8087 (2)0.0520 (8)
C560.2312 (4)0.3885 (2)0.9269 (2)0.1033 (18)
H56A0.28860.41060.94000.155*
H56B0.25810.35920.94110.155*
H56C0.15930.39520.94850.155*
C570.1715 (3)0.30361 (13)0.8304 (3)0.0991 (18)
H57A0.09270.29870.84370.149*
H57B0.22410.29770.86870.149*
H57C0.18880.28380.79320.149*
C580.1485 (3)0.34001 (17)0.6766 (2)0.0896 (15)
H58A0.06620.33960.66580.134*
H58B0.17560.30980.68460.134*
H58C0.18870.35280.63890.134*
C590.1776 (3)0.44524 (16)0.6804 (2)0.0883 (15)
H59A0.09950.45670.67580.132*
H59B0.19580.42880.63980.132*
H59C0.23120.46980.68660.132*
C600.2369 (4)0.47485 (14)0.8322 (3)0.0976 (17)
H60A0.28470.48970.79970.146*
H60B0.27700.47430.87630.146*
H60C0.16470.49080.83560.146*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0336 (2)0.0335 (3)0.0321 (3)0.00363 (19)0.0029 (2)0.0012 (2)
Ti20.0222 (2)0.0293 (2)0.0347 (3)0.00138 (17)0.00108 (19)0.0026 (2)
Ti30.0262 (2)0.0328 (2)0.0300 (3)0.00063 (18)0.00248 (19)0.0052 (2)
Ti40.0317 (2)0.0319 (2)0.0375 (3)0.00347 (18)0.0034 (2)0.0019 (2)
Ti50.0318 (2)0.0366 (3)0.0287 (3)0.00164 (19)0.0058 (2)0.0038 (2)
Ti60.0233 (2)0.0290 (2)0.0299 (3)0.00108 (17)0.00276 (18)0.00068 (19)
Ti70.0277 (2)0.0266 (2)0.0353 (3)0.00143 (17)0.00281 (19)0.00390 (19)
Cl10.0866 (6)0.0409 (4)0.0681 (6)0.0036 (4)0.0151 (5)0.0149 (4)
Cl20.0843 (6)0.0344 (4)0.0984 (8)0.0060 (4)0.0159 (6)0.0093 (4)
O10.0319 (9)0.0401 (10)0.0382 (11)0.0018 (8)0.0006 (8)0.0035 (9)
O20.0301 (9)0.0319 (9)0.0419 (11)0.0023 (7)0.0007 (8)0.0048 (8)
O30.0366 (10)0.0370 (10)0.0560 (13)0.0058 (8)0.0136 (9)0.0098 (9)
O40.0318 (10)0.0535 (12)0.0353 (11)0.0022 (8)0.0008 (8)0.0026 (9)
O50.0273 (9)0.0415 (10)0.0329 (10)0.0013 (7)0.0013 (8)0.0055 (8)
O60.0318 (9)0.0563 (12)0.0363 (11)0.0051 (9)0.0027 (8)0.0007 (10)
O70.0328 (9)0.0370 (10)0.0324 (10)0.0011 (8)0.0014 (8)0.0049 (8)
O80.0321 (9)0.0301 (9)0.0375 (11)0.0026 (7)0.0075 (8)0.0010 (8)
O90.0516 (12)0.0368 (10)0.0450 (12)0.0030 (9)0.0184 (10)0.0003 (9)
O100.0291 (9)0.0452 (11)0.0324 (10)0.0020 (8)0.0034 (8)0.0069 (8)
C10.059 (2)0.058 (2)0.0399 (18)0.0135 (16)0.0195 (15)0.0064 (15)
C20.0538 (19)0.060 (2)0.0449 (19)0.0176 (15)0.0170 (15)0.0001 (16)
C30.094 (3)0.0420 (17)0.0409 (19)0.0159 (17)0.0232 (18)0.0106 (15)
C40.0470 (18)0.096 (3)0.0302 (17)0.0024 (18)0.0022 (14)0.0029 (18)
C50.078 (2)0.0414 (17)0.0403 (18)0.0067 (16)0.0205 (17)0.0052 (14)
C60.097 (3)0.135 (4)0.070 (3)0.069 (3)0.030 (3)0.029 (3)
C70.098 (4)0.134 (4)0.095 (4)0.069 (3)0.038 (3)0.024 (3)
C80.205 (6)0.068 (3)0.082 (3)0.050 (3)0.034 (4)0.035 (3)
C90.073 (3)0.216 (7)0.056 (3)0.007 (3)0.017 (2)0.004 (3)
C100.168 (5)0.055 (2)0.082 (3)0.040 (3)0.049 (3)0.029 (2)
C110.0201 (12)0.0456 (16)0.069 (2)0.0004 (11)0.0072 (13)0.0014 (16)
C120.0233 (13)0.0581 (18)0.0524 (19)0.0048 (12)0.0027 (13)0.0131 (16)
C130.0290 (13)0.0455 (16)0.0526 (19)0.0109 (12)0.0012 (13)0.0014 (14)
C140.0296 (13)0.0450 (16)0.0529 (19)0.0098 (12)0.0039 (13)0.0082 (14)
C150.0244 (13)0.0565 (18)0.0500 (19)0.0054 (12)0.0085 (12)0.0069 (15)
C160.0432 (19)0.051 (2)0.134 (4)0.0109 (15)0.013 (2)0.003 (2)
C170.048 (2)0.100 (3)0.068 (3)0.0059 (19)0.0138 (18)0.026 (2)
C180.064 (2)0.062 (2)0.080 (3)0.0220 (18)0.003 (2)0.018 (2)
C190.069 (2)0.061 (2)0.077 (3)0.0159 (18)0.003 (2)0.028 (2)
C200.048 (2)0.106 (3)0.062 (2)0.003 (2)0.0111 (18)0.022 (2)
C210.0544 (19)0.0501 (18)0.0434 (18)0.0177 (15)0.0157 (15)0.0029 (15)
C220.0273 (13)0.0641 (19)0.0419 (17)0.0007 (13)0.0062 (12)0.0136 (15)
C230.0446 (16)0.0458 (16)0.0364 (16)0.0022 (13)0.0137 (13)0.0048 (14)
C240.0388 (15)0.068 (2)0.0307 (15)0.0013 (14)0.0035 (12)0.0128 (15)
C250.0535 (18)0.0465 (17)0.0475 (19)0.0094 (14)0.0208 (15)0.0207 (15)
C260.103 (3)0.083 (3)0.087 (3)0.057 (3)0.031 (3)0.022 (3)
C270.0376 (18)0.117 (3)0.084 (3)0.009 (2)0.0000 (19)0.027 (3)
C280.094 (3)0.058 (2)0.063 (2)0.010 (2)0.027 (2)0.0061 (19)
C290.059 (2)0.153 (4)0.044 (2)0.003 (3)0.0086 (18)0.011 (3)
C300.105 (3)0.068 (3)0.096 (3)0.039 (2)0.039 (3)0.043 (2)
C310.0335 (15)0.068 (2)0.052 (2)0.0074 (14)0.0081 (14)0.0028 (17)
C320.0454 (18)0.055 (2)0.072 (2)0.0132 (15)0.0225 (17)0.0016 (18)
C330.065 (2)0.060 (2)0.056 (2)0.0139 (17)0.0217 (18)0.0231 (18)
C340.0414 (17)0.089 (3)0.0356 (17)0.0051 (17)0.0083 (14)0.0068 (18)
C350.0474 (17)0.0435 (16)0.054 (2)0.0014 (13)0.0216 (15)0.0005 (15)
C360.053 (2)0.120 (4)0.080 (3)0.027 (2)0.006 (2)0.008 (3)
C370.074 (3)0.083 (3)0.174 (6)0.037 (2)0.038 (3)0.016 (3)
C380.150 (5)0.103 (4)0.095 (4)0.046 (3)0.040 (3)0.059 (3)
C390.061 (2)0.182 (5)0.056 (3)0.003 (3)0.002 (2)0.034 (3)
C400.089 (3)0.052 (2)0.103 (4)0.003 (2)0.047 (3)0.014 (2)
C410.0528 (19)0.076 (2)0.045 (2)0.0054 (17)0.0228 (16)0.0208 (18)
C420.081 (3)0.072 (2)0.0317 (18)0.009 (2)0.0219 (17)0.0022 (16)
C430.054 (2)0.098 (3)0.0310 (17)0.009 (2)0.0011 (15)0.0186 (19)
C440.068 (2)0.064 (2)0.0448 (19)0.0107 (18)0.0175 (17)0.0255 (17)
C450.060 (2)0.063 (2)0.049 (2)0.0165 (17)0.0163 (16)0.0165 (17)
C460.070 (3)0.145 (4)0.092 (3)0.038 (3)0.048 (3)0.048 (3)
C470.183 (6)0.091 (3)0.062 (3)0.022 (4)0.046 (3)0.022 (3)
C480.077 (3)0.205 (6)0.053 (3)0.028 (3)0.011 (2)0.029 (3)
C490.134 (4)0.078 (3)0.092 (3)0.046 (3)0.045 (3)0.041 (3)
C500.110 (4)0.105 (4)0.091 (4)0.067 (3)0.011 (3)0.019 (3)
C510.0289 (15)0.086 (2)0.0412 (18)0.0068 (15)0.0083 (13)0.0054 (17)
C520.0236 (13)0.0426 (16)0.091 (3)0.0044 (12)0.0161 (15)0.0180 (17)
C530.0200 (12)0.0586 (18)0.0531 (19)0.0023 (12)0.0011 (12)0.0125 (16)
C540.0295 (14)0.0507 (18)0.064 (2)0.0128 (13)0.0045 (14)0.0102 (16)
C550.0323 (15)0.0467 (17)0.078 (3)0.0063 (13)0.0098 (15)0.0128 (17)
C560.064 (3)0.196 (6)0.051 (3)0.001 (3)0.019 (2)0.004 (3)
C570.052 (2)0.059 (2)0.188 (6)0.0031 (18)0.032 (3)0.045 (3)
C580.048 (2)0.125 (4)0.094 (3)0.009 (2)0.007 (2)0.051 (3)
C590.063 (2)0.099 (3)0.103 (4)0.028 (2)0.007 (2)0.049 (3)
C600.069 (3)0.063 (3)0.161 (5)0.008 (2)0.016 (3)0.047 (3)
Geometric parameters (Å, º) top
Ti1—O11.8049 (18)C20—H20C0.9600
Ti1—O41.8073 (19)C21—C251.399 (5)
Ti1—Cl12.2919 (9)C21—C221.423 (4)
Ti1—C52.330 (3)C21—C261.498 (5)
Ti1—C12.361 (3)C22—C231.403 (4)
Ti1—C42.365 (3)C22—C271.495 (5)
Ti1—C22.398 (3)C23—C241.414 (4)
Ti1—C32.402 (3)C23—C281.502 (4)
Ti2—O51.8401 (18)C24—C251.402 (5)
Ti2—O11.8461 (19)C24—C291.494 (5)
Ti2—O21.8492 (18)C25—C301.507 (4)
Ti2—C112.360 (3)C26—H26A0.9600
Ti2—C122.360 (3)C26—H26B0.9600
Ti2—C152.364 (3)C26—H26C0.9600
Ti2—C142.378 (3)C27—H27A0.9600
Ti2—C132.389 (3)C27—H27B0.9600
Ti3—O51.8331 (17)C27—H27C0.9600
Ti3—O41.844 (2)C28—H28A0.9600
Ti3—O31.8454 (19)C28—H28B0.9600
Ti3—C242.359 (3)C28—H28C0.9600
Ti3—C232.368 (3)C29—H29A0.9600
Ti3—C252.373 (3)C29—H29B0.9600
Ti3—C222.376 (3)C29—H29C0.9600
Ti3—C212.391 (3)C30—H30A0.9600
Ti4—O71.8095 (18)C30—H30B0.9600
Ti4—O61.814 (2)C30—H30C0.9600
Ti4—Cl22.2914 (10)C31—C321.397 (5)
Ti4—C352.323 (3)C31—C351.403 (5)
Ti4—C342.361 (3)C31—C361.504 (5)
Ti4—C312.379 (3)C32—C331.399 (5)
Ti4—C332.390 (3)C32—C371.521 (5)
Ti4—C322.403 (3)C33—C341.400 (5)
Ti5—O101.8334 (18)C33—C381.507 (5)
Ti5—O61.844 (2)C34—C351.409 (5)
Ti5—O91.8485 (19)C34—C391.502 (5)
Ti5—C432.354 (3)C35—C401.496 (5)
Ti5—C422.359 (3)C36—H36A0.9600
Ti5—C412.375 (3)C36—H36B0.9600
Ti5—C442.378 (3)C36—H36C0.9600
Ti5—C452.399 (3)C37—H37A0.9600
Ti6—O101.8374 (18)C37—H37B0.9600
Ti6—O71.8389 (18)C37—H37C0.9600
Ti6—O81.8572 (17)C38—H38A0.9600
Ti6—C522.357 (3)C38—H38B0.9600
Ti6—C532.362 (3)C38—H38C0.9600
Ti6—C512.367 (3)C39—H39A0.9600
Ti6—C552.388 (3)C39—H39B0.9600
Ti6—C542.397 (3)C39—H39C0.9600
Ti7—O81.8091 (18)C40—H40A0.9600
Ti7—O91.811 (2)C40—H40B0.9600
Ti7—O21.8157 (18)C40—H40C0.9600
Ti7—O31.8167 (19)C41—C421.394 (5)
C1—C21.379 (5)C41—C451.412 (5)
C1—C51.386 (5)C41—C461.520 (5)
C1—C61.517 (5)C42—C431.388 (5)
C2—C31.423 (5)C42—C471.514 (6)
C2—C71.522 (5)C43—C441.420 (5)
C3—C41.424 (5)C43—C481.516 (5)
C3—C81.504 (5)C44—C451.408 (5)
C4—C51.392 (5)C44—C491.496 (5)
C4—C91.504 (5)C45—C501.496 (5)
C5—C101.515 (5)C46—H46A0.9600
C6—H6A0.9600C46—H46B0.9600
C6—H6B0.9600C46—H46C0.9600
C6—H6C0.9600C47—H47A0.9600
C7—H7A0.9600C47—H47B0.9600
C7—H7B0.9600C47—H47C0.9600
C7—H7C0.9600C48—H48A0.9600
C8—H8A0.9600C48—H48B0.9600
C8—H8B0.9600C48—H48C0.9600
C8—H8C0.9600C49—H49A0.9600
C9—H9A0.9600C49—H49B0.9600
C9—H9B0.9600C49—H49C0.9600
C9—H9C0.9600C50—H50A0.9600
C10—H10A0.9600C50—H50B0.9600
C10—H10B0.9600C50—H50C0.9600
C10—H10C0.9600C51—C551.394 (5)
C11—C121.407 (5)C51—C521.427 (5)
C11—C151.412 (4)C51—C561.497 (5)
C11—C161.501 (4)C52—C531.419 (5)
C12—C131.413 (4)C52—C571.490 (4)
C12—C171.506 (5)C53—C541.395 (4)
C13—C141.405 (4)C53—C581.497 (5)
C13—C181.509 (4)C54—C551.374 (5)
C14—C151.410 (4)C54—C591.514 (5)
C14—C191.503 (4)C55—C601.514 (5)
C15—C201.499 (5)C56—H56A0.9600
C16—H16A0.9600C56—H56B0.9600
C16—H16B0.9600C56—H56C0.9600
C16—H16C0.9600C57—H57A0.9600
C17—H17A0.9600C57—H57B0.9600
C17—H17B0.9600C57—H57C0.9600
C17—H17C0.9600C58—H58A0.9600
C18—H18A0.9600C58—H58B0.9600
C18—H18B0.9600C58—H58C0.9600
C18—H18C0.9600C59—H59A0.9600
C19—H19A0.9600C59—H59B0.9600
C19—H19B0.9600C59—H59C0.9600
C19—H19C0.9600C60—H60A0.9594
C20—H20A0.9600C60—H60B0.9616
C20—H20B0.9600C60—H60C0.9585
O1—Ti1—O4103.85 (9)C11—C15—Ti272.47 (16)
O1—Ti1—Cl1102.67 (7)C20—C15—Ti2120.5 (2)
O4—Ti1—Cl1105.01 (7)C11—C16—H16A109.5
O1—Ti1—C592.82 (11)C11—C16—H16B109.5
O4—Ti1—C5101.87 (11)H16A—C16—H16B109.5
Cl1—Ti1—C5144.51 (9)C11—C16—H16C109.5
O1—Ti1—C1125.50 (11)H16A—C16—H16C109.5
O4—Ti1—C183.22 (10)H16B—C16—H16C109.5
Cl1—Ti1—C1128.01 (9)C12—C17—H17A109.5
C5—Ti1—C134.35 (12)C12—C17—H17B109.5
O1—Ti1—C487.43 (10)H17A—C17—H17B109.5
O4—Ti1—C4136.09 (11)C12—C17—H17C109.5
Cl1—Ti1—C4113.75 (10)H17A—C17—H17C109.5
C5—Ti1—C434.49 (12)H17B—C17—H17C109.5
C1—Ti1—C457.05 (12)C13—C18—H18A109.5
O1—Ti1—C2144.42 (11)C13—C18—H18B109.5
O4—Ti1—C2100.59 (11)H18A—C18—H18B109.5
Cl1—Ti1—C295.44 (9)C13—C18—H18C109.5
C5—Ti1—C256.78 (11)H18A—C18—H18C109.5
C1—Ti1—C233.67 (11)H18B—C18—H18C109.5
C4—Ti1—C257.14 (12)C14—C19—H19A109.5
O1—Ti1—C3115.67 (12)C14—C19—H19B109.5
O4—Ti1—C3135.02 (11)H19A—C19—H19B109.5
Cl1—Ti1—C387.08 (8)C14—C19—H19C109.5
C5—Ti1—C357.46 (11)H19A—C19—H19C109.5
C1—Ti1—C356.98 (11)H19B—C19—H19C109.5
C4—Ti1—C334.74 (12)C15—C20—H20A109.5
C2—Ti1—C334.50 (12)C15—C20—H20B109.5
O5—Ti2—O1104.75 (8)H20A—C20—H20B109.5
O5—Ti2—O2102.48 (8)C15—C20—H20C109.5
O1—Ti2—O2102.69 (9)H20A—C20—H20C109.5
O5—Ti2—C11118.18 (10)H20B—C20—H20C109.5
O1—Ti2—C11132.72 (10)C25—C21—C22108.0 (3)
O2—Ti2—C1187.22 (9)C25—C21—C26127.1 (4)
O5—Ti2—C12144.35 (10)C22—C21—C26124.9 (4)
O1—Ti2—C1298.13 (10)C25—C21—Ti372.23 (16)
O2—Ti2—C1298.64 (9)C22—C21—Ti372.05 (16)
C11—Ti2—C1234.67 (11)C26—C21—Ti3122.0 (2)
O5—Ti2—C1587.75 (10)C23—C22—C21107.7 (3)
O1—Ti2—C15140.47 (9)C23—C22—C27125.9 (3)
O2—Ti2—C15111.08 (10)C21—C22—C27126.4 (3)
C11—Ti2—C1534.78 (11)C23—C22—Ti372.47 (16)
C12—Ti2—C1557.75 (11)C21—C22—Ti373.21 (16)
O5—Ti2—C1489.39 (9)C27—C22—Ti3119.6 (2)
O1—Ti2—C14106.97 (10)C22—C23—C24107.9 (3)
O2—Ti2—C14143.97 (9)C22—C23—C28125.8 (3)
C11—Ti2—C1457.57 (10)C24—C23—C28126.3 (3)
C12—Ti2—C1457.57 (10)C22—C23—Ti373.13 (17)
C15—Ti2—C1434.61 (10)C24—C23—Ti372.26 (16)
O5—Ti2—C13120.71 (9)C28—C23—Ti3121.1 (2)
O1—Ti2—C1384.78 (9)C25—C24—C23108.2 (3)
O2—Ti2—C13132.88 (9)C25—C24—C29125.7 (3)
C11—Ti2—C1357.36 (10)C23—C24—C29126.1 (3)
C12—Ti2—C1334.61 (10)C25—C24—Ti373.32 (17)
C15—Ti2—C1357.30 (10)C23—C24—Ti372.92 (16)
C14—Ti2—C1334.30 (10)C29—C24—Ti3120.9 (2)
O5—Ti3—O4100.31 (8)C21—C25—C24108.2 (3)
O5—Ti3—O3101.47 (8)C21—C25—C30126.0 (4)
O4—Ti3—O3107.16 (10)C24—C25—C30125.7 (4)
O5—Ti3—C2492.05 (9)C21—C25—Ti373.63 (17)
O4—Ti3—C24138.09 (10)C24—C25—Ti372.22 (17)
O3—Ti3—C24109.32 (11)C30—C25—Ti3121.6 (2)
O5—Ti3—C23121.66 (10)C21—C26—H26A109.5
O4—Ti3—C23133.54 (10)C21—C26—H26B109.5
O3—Ti3—C2384.64 (9)H26A—C26—H26B109.5
C24—Ti3—C2334.82 (10)C21—C26—H26C109.5
O5—Ti3—C2593.98 (10)H26A—C26—H26C109.5
O4—Ti3—C25104.28 (11)H26B—C26—H26C109.5
O3—Ti3—C25141.58 (10)C22—C27—H27A109.5
C24—Ti3—C2534.46 (11)C22—C27—H27B109.5
C23—Ti3—C2557.53 (10)H27A—C27—H27B109.5
O5—Ti3—C22148.76 (9)C22—C27—H27C109.5
O4—Ti3—C2299.14 (10)H27A—C27—H27C109.5
O3—Ti3—C2295.81 (10)H27B—C27—H27C109.5
C24—Ti3—C2257.49 (10)C23—C28—H28A109.5
C23—Ti3—C2234.40 (11)C23—C28—H28B109.5
C25—Ti3—C2257.47 (10)H28A—C28—H28B109.5
O5—Ti3—C21124.77 (10)C23—C28—H28C109.5
O4—Ti3—C2183.62 (10)H28A—C28—H28C109.5
O3—Ti3—C21130.23 (10)H28B—C28—H28C109.5
C24—Ti3—C2157.06 (11)C24—C29—H29A109.5
C23—Ti3—C2157.29 (11)C24—C29—H29B109.5
C25—Ti3—C2134.15 (12)H29A—C29—H29B109.5
C22—Ti3—C2134.74 (11)C24—C29—H29C109.5
O7—Ti4—O6104.44 (8)H29A—C29—H29C109.5
O7—Ti4—Cl2101.01 (7)H29B—C29—H29C109.5
O6—Ti4—Cl2104.93 (8)C25—C30—H30A109.5
O7—Ti4—C3596.95 (10)C25—C30—H30B109.5
O6—Ti4—C3598.25 (11)H30A—C30—H30B109.5
Cl2—Ti4—C35145.89 (8)C25—C30—H30C109.5
O7—Ti4—C3485.48 (10)H30A—C30—H30C109.5
O6—Ti4—C34133.19 (11)H30B—C30—H30C109.5
Cl2—Ti4—C34118.08 (10)C32—C31—C35108.0 (3)
C35—Ti4—C3434.99 (12)C32—C31—C36125.8 (4)
O7—Ti4—C31131.43 (11)C35—C31—C36126.2 (3)
O6—Ti4—C3184.86 (10)C32—C31—Ti473.98 (17)
Cl2—Ti4—C31122.84 (9)C35—C31—Ti470.46 (16)
C35—Ti4—C3134.70 (12)C36—C31—Ti4121.0 (2)
C34—Ti4—C3157.29 (11)C31—C32—C33108.1 (3)
O7—Ti4—C33109.57 (12)C31—C32—C37126.1 (4)
O6—Ti4—C33139.84 (11)C33—C32—C37125.8 (4)
Cl2—Ti4—C3389.08 (9)C31—C32—Ti472.06 (17)
C35—Ti4—C3357.48 (11)C33—C32—Ti472.49 (18)
C34—Ti4—C3334.27 (13)C37—C32—Ti4122.4 (3)
C31—Ti4—C3356.67 (12)C32—C33—C34108.3 (3)
O7—Ti4—C32141.61 (12)C32—C33—C38126.1 (4)
O6—Ti4—C32106.95 (12)C34—C33—C38125.5 (4)
Cl2—Ti4—C3291.75 (9)C32—C33—Ti473.6 (2)
C35—Ti4—C3257.26 (11)C34—C33—Ti471.76 (18)
C34—Ti4—C3256.85 (12)C38—C33—Ti4124.1 (3)
C31—Ti4—C3233.96 (12)C33—C34—C35107.6 (3)
C33—Ti4—C3233.93 (13)C33—C34—C39127.3 (4)
O10—Ti5—O6101.37 (9)C35—C34—C39125.0 (4)
O10—Ti5—O9101.04 (9)C33—C34—Ti474.0 (2)
O6—Ti5—O9106.37 (10)C35—C34—Ti471.02 (18)
O10—Ti5—C4391.21 (10)C39—C34—Ti4120.2 (2)
O6—Ti5—C43140.16 (12)C31—C35—C34107.8 (3)
O9—Ti5—C43108.03 (13)C31—C35—C40126.8 (4)
O10—Ti5—C42120.76 (12)C34—C35—C40125.3 (4)
O6—Ti5—C42133.80 (12)C31—C35—Ti474.84 (18)
O9—Ti5—C4284.67 (11)C34—C35—Ti473.99 (18)
C43—Ti5—C4234.26 (13)C40—C35—Ti4118.6 (2)
O10—Ti5—C41147.28 (10)C31—C36—H36A109.5
O6—Ti5—C4199.57 (11)C31—C36—H36B109.5
O9—Ti5—C4196.81 (11)H36A—C36—H36B109.5
C43—Ti5—C4157.04 (12)C31—C36—H36C109.5
C42—Ti5—C4134.25 (13)H36A—C36—H36C109.5
O10—Ti5—C4492.74 (10)H36B—C36—H36C109.5
O6—Ti5—C44106.14 (12)C32—C37—H37A109.5
O9—Ti5—C44141.20 (12)C32—C37—H37B109.5
C43—Ti5—C4434.91 (13)H37A—C37—H37B109.5
C42—Ti5—C4457.42 (13)C32—C37—H37C109.5
C41—Ti5—C4457.20 (12)H37A—C37—H37C109.5
O10—Ti5—C45123.77 (11)H37B—C37—H37C109.5
O6—Ti5—C4584.93 (11)C33—C38—H38A109.5
O9—Ti5—C45130.99 (11)C33—C38—H38B109.5
C43—Ti5—C4557.27 (13)H38A—C38—H38B109.5
C42—Ti5—C4557.12 (13)C33—C38—H38C109.5
C41—Ti5—C4534.41 (12)H38A—C38—H38C109.5
C44—Ti5—C4534.27 (12)H38B—C38—H38C109.5
O10—Ti6—O7103.94 (8)C34—C39—H39A109.5
O10—Ti6—O8102.86 (8)C34—C39—H39B109.5
O7—Ti6—O8102.65 (8)H39A—C39—H39B109.5
O10—Ti6—C52129.27 (11)C34—C39—H39C109.5
O7—Ti6—C52122.51 (11)H39A—C39—H39C109.5
O8—Ti6—C5286.88 (9)H39B—C39—H39C109.5
O10—Ti6—C5394.75 (10)C35—C40—H40A109.5
O7—Ti6—C53145.20 (9)C35—C40—H40B109.5
O8—Ti6—C53101.40 (10)H40A—C40—H40B109.5
C52—Ti6—C5334.99 (12)C35—C40—H40C109.5
O10—Ti6—C51140.76 (10)H40A—C40—H40C109.5
O7—Ti6—C5190.54 (10)H40B—C40—H40C109.5
O8—Ti6—C51109.31 (11)C42—C41—C45108.3 (3)
C52—Ti6—C5135.16 (12)C42—C41—C46126.7 (4)
C53—Ti6—C5157.71 (11)C45—C41—C46125.0 (4)
O10—Ti6—C55108.70 (11)C42—C41—Ti572.25 (18)
O7—Ti6—C5589.25 (10)C45—C41—Ti573.72 (18)
O8—Ti6—C55142.40 (10)C46—C41—Ti5119.4 (2)
C52—Ti6—C5557.36 (11)C43—C42—C41108.5 (3)
C53—Ti6—C5556.71 (11)C43—C42—C47125.6 (4)
C51—Ti6—C5534.10 (12)C41—C42—C47125.9 (4)
O10—Ti6—C5484.87 (10)C43—C42—Ti572.65 (19)
O7—Ti6—C54118.13 (10)C41—C42—Ti573.49 (19)
O8—Ti6—C54135.45 (10)C47—C42—Ti5119.8 (3)
C52—Ti6—C5457.10 (10)C42—C43—C44108.3 (3)
C53—Ti6—C5434.09 (11)C42—C43—C48126.4 (4)
C51—Ti6—C5456.44 (11)C44—C43—C48125.3 (4)
C55—Ti6—C5433.39 (12)C42—C43—Ti573.09 (19)
O8—Ti7—O9106.42 (8)C44—C43—Ti573.50 (19)
O8—Ti7—O2115.35 (9)C48—C43—Ti5119.8 (2)
O9—Ti7—O2107.32 (9)C45—C44—C43107.3 (3)
O8—Ti7—O3107.61 (9)C45—C44—C49126.0 (4)
O9—Ti7—O3114.14 (10)C43—C44—C49126.7 (4)
O2—Ti7—O3106.26 (8)C45—C44—Ti573.66 (18)
Ti1—O1—Ti2128.44 (10)C43—C44—Ti571.59 (19)
Ti7—O2—Ti2130.26 (10)C49—C44—Ti5120.5 (2)
Ti7—O3—Ti3128.29 (10)C44—C45—C41107.6 (3)
Ti1—O4—Ti3135.88 (10)C44—C45—C50126.9 (4)
Ti3—O5—Ti2121.26 (10)C41—C45—C50125.5 (4)
Ti4—O6—Ti5134.14 (10)C44—C45—Ti572.07 (18)
Ti4—O7—Ti6128.83 (10)C41—C45—Ti571.88 (18)
Ti7—O8—Ti6130.63 (10)C50—C45—Ti5122.3 (3)
Ti7—O9—Ti5128.90 (11)C41—C46—H46A109.5
Ti5—O10—Ti6121.44 (10)C41—C46—H46B109.5
C2—C1—C5108.9 (3)H46A—C46—H46B109.5
C2—C1—C6125.4 (4)C41—C46—H46C109.5
C5—C1—C6125.8 (4)H46A—C46—H46C109.5
C2—C1—Ti174.61 (19)H46B—C46—H46C109.5
C5—C1—Ti171.57 (18)C42—C47—H47A109.5
C6—C1—Ti1119.3 (2)C42—C47—H47B109.5
C1—C2—C3108.4 (3)H47A—C47—H47B109.5
C1—C2—C7127.6 (4)C42—C47—H47C109.5
C3—C2—C7124.0 (4)H47A—C47—H47C109.5
C1—C2—Ti171.72 (18)H47B—C47—H47C109.5
C3—C2—Ti172.91 (18)C43—C48—H48A109.5
C7—C2—Ti1121.5 (3)C43—C48—H48B109.5
C4—C3—C2106.3 (3)H48A—C48—H48B109.5
C4—C3—C8127.1 (4)C43—C48—H48C109.5
C2—C3—C8126.5 (4)H48A—C48—H48C109.5
C4—C3—Ti171.20 (18)H48B—C48—H48C109.5
C2—C3—Ti172.59 (18)C44—C49—H49A109.5
C8—C3—Ti1125.0 (3)C44—C49—H49B109.5
C5—C4—C3107.8 (3)H49A—C49—H49B109.5
C5—C4—C9125.8 (4)C44—C49—H49C109.5
C3—C4—C9126.4 (4)H49A—C49—H49C109.5
C5—C4—Ti171.37 (19)H49B—C49—H49C109.5
C3—C4—Ti174.05 (19)C45—C50—H50A109.5
C9—C4—Ti1120.7 (3)C45—C50—H50B109.5
C1—C5—C4108.7 (3)H50A—C50—H50B109.5
C1—C5—C10125.7 (4)C45—C50—H50C109.5
C4—C5—C10125.5 (4)H50A—C50—H50C109.5
C1—C5—Ti174.08 (19)H50B—C50—H50C109.5
C4—C5—Ti174.14 (19)C55—C51—C52107.6 (3)
C10—C5—Ti1119.8 (2)C55—C51—C56126.0 (4)
C1—C6—H6A109.5C52—C51—C56126.3 (4)
C1—C6—H6B109.5C55—C51—Ti673.77 (18)
H6A—C6—H6B109.5C52—C51—Ti672.05 (17)
C1—C6—H6C109.5C56—C51—Ti6121.0 (2)
H6A—C6—H6C109.5C53—C52—C51106.6 (3)
H6B—C6—H6C109.5C53—C52—C57126.6 (4)
C2—C7—H7A109.5C51—C52—C57126.8 (4)
C2—C7—H7B109.5C53—C52—Ti672.70 (16)
H7A—C7—H7B109.5C51—C52—Ti672.79 (16)
C2—C7—H7C109.5C57—C52—Ti6120.9 (2)
H7A—C7—H7C109.5C54—C53—C52107.7 (3)
H7B—C7—H7C109.5C54—C53—C58126.2 (4)
C3—C8—H8A109.5C52—C53—C58126.1 (3)
C3—C8—H8B109.5C54—C53—Ti674.33 (16)
H8A—C8—H8B109.5C52—C53—Ti672.31 (16)
C3—C8—H8C109.5C58—C53—Ti6117.9 (2)
H8A—C8—H8C109.5C55—C54—C53109.1 (3)
H8B—C8—H8C109.5C55—C54—C59126.1 (4)
C4—C9—H9A109.5C53—C54—C59124.8 (4)
C4—C9—H9B109.5C55—C54—Ti672.92 (17)
H9A—C9—H9B109.5C53—C54—Ti671.59 (15)
C4—C9—H9C109.5C59—C54—Ti6121.8 (2)
H9A—C9—H9C109.5C54—C55—C51108.9 (3)
H9B—C9—H9C109.5C54—C55—C60125.1 (4)
C5—C10—H10A109.5C51—C55—C60126.0 (4)
C5—C10—H10B109.5C54—C55—Ti673.69 (17)
H10A—C10—H10B109.5C51—C55—Ti672.13 (17)
C5—C10—H10C109.5C60—C55—Ti6120.7 (2)
H10A—C10—H10C109.5C51—C56—H56A109.5
H10B—C10—H10C109.5C51—C56—H56B109.5
C12—C11—C15108.1 (3)H56A—C56—H56B109.5
C12—C11—C16126.7 (3)C51—C56—H56C109.5
C15—C11—C16125.2 (3)H56A—C56—H56C109.5
C12—C11—Ti272.67 (16)H56B—C56—H56C109.5
C15—C11—Ti272.76 (16)C52—C57—H57A109.5
C16—C11—Ti2121.6 (2)C52—C57—H57B109.5
C11—C12—C13107.9 (3)H57A—C57—H57B109.5
C11—C12—C17125.8 (3)C52—C57—H57C109.5
C13—C12—C17126.3 (3)H57A—C57—H57C109.5
C11—C12—Ti272.66 (16)H57B—C57—H57C109.5
C13—C12—Ti273.79 (15)C53—C58—H58A109.5
C17—C12—Ti2118.3 (2)C53—C58—H58B109.5
C14—C13—C12108.1 (3)H58A—C58—H58B109.5
C14—C13—C18126.0 (3)C53—C58—H58C109.5
C12—C13—C18125.8 (3)H58A—C58—H58C109.5
C14—C13—Ti272.43 (15)H58B—C58—H58C109.5
C12—C13—Ti271.60 (15)C54—C59—H59A109.5
C18—C13—Ti2121.3 (2)C54—C59—H59B109.5
C13—C14—C15108.0 (3)H59A—C59—H59B109.5
C13—C14—C19126.5 (3)C54—C59—H59C109.5
C15—C14—C19125.5 (3)H59A—C59—H59C109.5
C13—C14—Ti273.28 (16)H59B—C59—H59C109.5
C15—C14—Ti272.16 (16)C55—C60—H60A109.5
C19—C14—Ti2120.4 (2)C55—C60—H60B109.3
C14—C15—C11107.9 (3)H60A—C60—H60B109.4
C14—C15—C20125.9 (3)C55—C60—H60C109.5
C11—C15—C20126.2 (3)H60A—C60—H60C109.7
C14—C15—Ti273.23 (16)H60B—C60—H60C109.5

Experimental details

Crystal data
Chemical formula[Ti6(C10H15)6Cl2O10]
Mr1377.52
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)11.4724 (14), 29.713 (4), 19.495 (2)
β (°) 92.090 (2)
V3)6641.0 (14)
Z4
Radiation typeMo Kα
µ (mm1)0.93
Crystal size (mm)0.28 × 0.26 × 0.10
Data collection
DiffractometerBruker CCD area detector
diffractometer
Absorption correctionMulti-scan
(SHELXTL; Bruker, 1997)
Tmin, Tmax0.781, 0.917
No. of measured, independent and
observed [I > 2σ(I)] reflections
37338, 13061, 10417
Rint0.026
(sin θ/λ)max1)0.618
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.121, 1.02
No. of reflections13061
No. of parameters741
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.44, 0.24

Computer programs: SMART (Bruker, 1998), SMART, SAINT-NT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Ti1—O11.8049 (18)Ti4—C312.379 (3)
Ti1—O41.8073 (19)Ti5—O101.8334 (18)
Ti1—Cl12.2919 (9)Ti5—O61.844 (2)
Ti2—O51.8401 (18)Ti5—O91.8485 (19)
Ti2—O11.8461 (19)Ti6—O101.8374 (18)
Ti2—O21.8492 (18)Ti6—O71.8389 (18)
Ti3—O51.8331 (17)Ti6—O81.8572 (17)
Ti3—O41.844 (2)Ti7—O81.8091 (18)
Ti3—O31.8454 (19)Ti7—O91.811 (2)
Ti4—O71.8095 (18)Ti7—O21.8157 (18)
Ti4—O61.814 (2)Ti7—O31.8167 (19)
Ti4—Cl22.2914 (10)
O1—Ti1—O4103.85 (9)O6—Ti4—C3598.25 (11)
O1—Ti1—Cl1102.67 (7)Cl2—Ti4—C31122.84 (9)
O1—Ti2—O2102.69 (9)O2—Ti7—O3106.26 (8)
O7—Ti4—O6104.44 (8)Ti7—O3—Ti3128.29 (10)
O7—Ti4—Cl2101.01 (7)Ti3—O5—Ti2121.26 (10)
O6—Ti4—Cl2104.93 (8)
 

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