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The title complex, [Ti(C5H5)(C2H6N)2Cl], exhibits two nearly planar dimethylamide groups oriented approximately perpendicular to each other. The Ti[rightwards arrow]cyclopentadienyl centroid vector lies nearly in the plane of one of the dimethylamide groups. Long-range contacts between Ti-Cl and cyclopentadienyl H-C groups give rise to geometric ordering in the extended solid.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110023176/sf3132sup1.cif
Contains datablocks global, 1a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110023176/sf31321asup2.hkl
Contains datablock 1a

CCDC reference: 786803

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SMART (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2005); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Chlorido(η5-cyclopentadienyl)bis(dimethylamido)titanium top
Crystal data top
[Ti(C5H5)(C2H6N)2Cl]F(000) = 496
Mr = 236.60Dx = 1.351 Mg m3
Monoclinic, P21/nMelting point: 336 K
Hall symbol: -P 2ynMo Kα radiation, λ = 0.71073 Å
a = 9.3621 (9) ÅCell parameters from 9781 reflections
b = 11.0618 (10) Åθ = 2.5–25.4°
c = 11.5907 (11) ŵ = 0.93 mm1
β = 104.259 (1)°T = 100 K
V = 1163.37 (19) Å3Block, dark red
Z = 40.20 × 0.20 × 0.20 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2133 independent reflections
Radiation source: fine-focus sealed tube1960 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
φ and ω scansθmax = 25.4°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1111
Tmin = 0.837, Tmax = 0.837k = 1313
14937 measured reflectionsl = 1313
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0284P)2 + 0.6046P]
where P = (Fo2 + 2Fc2)/3
2133 reflections(Δ/σ)max < 0.001
122 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.25 e Å3
Special details top

Experimental. Data were collected on a single parallelepiped. The crystal was mounted on a Cryoloop with Paratone-N oil. The crystal-to-detector distance was 60 mm and exposure time was 10 s per frame using a scan width of 0.5°.

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
Ti10.21237 (3)0.33216 (3)0.47002 (2)0.01448 (10)
Cl10.32843 (4)0.45489 (4)0.63118 (4)0.02238 (12)
N10.05397 (14)0.24969 (13)0.51023 (12)0.0188 (3)
N20.35083 (15)0.20437 (13)0.48327 (12)0.0180 (3)
C10.02702 (19)0.43809 (17)0.32309 (15)0.0259 (4)
H1A0.07580.45600.32870.031*
C20.07278 (19)0.33411 (16)0.27054 (15)0.0229 (4)
H2A0.00720.26760.22950.027*
C30.22210 (19)0.35011 (17)0.27068 (15)0.0247 (4)
H3A0.28020.29710.22920.030*
C40.2699 (2)0.46095 (17)0.32627 (16)0.0276 (4)
H4A0.36760.50000.33120.033*
C50.1480 (2)0.51503 (17)0.35797 (16)0.0296 (4)
H5A0.14640.59780.39230.036*
C60.1004 (2)0.20015 (17)0.63148 (15)0.0255 (4)
H6A0.08480.11250.62890.038*
H6B0.04210.23740.68160.038*
H6C0.20510.21760.66470.038*
C70.09587 (19)0.21187 (18)0.45330 (16)0.0265 (4)
H7A0.15940.22540.50780.040*
H7B0.09630.12580.43330.040*
H7C0.13280.25900.38050.040*
C80.32302 (19)0.07510 (15)0.48449 (16)0.0237 (4)
H8A0.38860.03890.55510.036*
H8B0.34150.03810.41270.036*
H8C0.22020.06120.48640.036*
C90.49634 (18)0.22941 (17)0.46392 (15)0.0233 (4)
H9A0.57220.19340.52850.035*
H9B0.51140.31700.46260.035*
H9C0.50310.19460.38770.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.01332 (16)0.01598 (17)0.01359 (16)0.00148 (11)0.00225 (11)0.00040 (11)
Cl10.0195 (2)0.0246 (2)0.0216 (2)0.00071 (16)0.00208 (16)0.00661 (16)
N10.0170 (7)0.0210 (7)0.0179 (7)0.0004 (6)0.0035 (5)0.0002 (6)
N20.0178 (7)0.0194 (7)0.0165 (7)0.0025 (6)0.0038 (5)0.0003 (6)
C10.0220 (9)0.0341 (10)0.0197 (9)0.0114 (8)0.0015 (7)0.0091 (8)
C20.0210 (9)0.0323 (10)0.0129 (8)0.0013 (7)0.0005 (7)0.0015 (7)
C30.0225 (9)0.0377 (11)0.0140 (8)0.0075 (8)0.0049 (7)0.0064 (7)
C40.0247 (9)0.0335 (10)0.0228 (9)0.0041 (8)0.0028 (7)0.0121 (8)
C50.0400 (11)0.0210 (9)0.0254 (9)0.0071 (8)0.0034 (8)0.0088 (8)
C60.0267 (9)0.0292 (10)0.0220 (9)0.0008 (8)0.0084 (7)0.0048 (8)
C70.0201 (9)0.0322 (10)0.0277 (10)0.0073 (8)0.0064 (7)0.0038 (8)
C80.0267 (9)0.0189 (9)0.0247 (9)0.0036 (7)0.0049 (7)0.0029 (7)
C90.0172 (8)0.0313 (10)0.0216 (9)0.0062 (7)0.0054 (7)0.0037 (7)
Geometric parameters (Å, º) top
Ti1—N11.8945 (14)C3—C41.406 (3)
Ti1—N21.8984 (14)C3—H3A1.0000
Ti1—C32.3430 (17)C4—C51.415 (3)
Ti1—Cl12.3480 (5)C4—H4A1.0000
Ti1—C42.3534 (17)C5—H5A1.0000
Ti1—C22.3592 (17)C6—H6A0.9800
Ti1—C52.3993 (18)C6—H6B0.9800
Ti1—C12.4143 (16)C6—H6C0.9800
N1—C71.457 (2)C7—H7A0.9800
N1—C61.471 (2)C7—H7B0.9800
N2—C81.454 (2)C7—H7C0.9800
N2—C91.461 (2)C8—H8A0.9800
C1—C51.395 (3)C8—H8B0.9800
C1—C21.416 (3)C8—H8C0.9800
C1—H1A1.0000C9—H9A0.9800
C2—C31.409 (2)C9—H9B0.9800
C2—H2A1.0000C9—H9C0.9800
N1—Ti1—N2100.48 (6)C1—C2—H2A125.9
N1—Ti1—C3120.42 (6)Ti1—C2—H2A125.9
N2—Ti1—C387.21 (6)C4—C3—C2108.30 (16)
N1—Ti1—Cl1108.64 (4)C4—C3—Ti172.98 (10)
N2—Ti1—Cl1101.14 (4)C2—C3—Ti173.20 (9)
C3—Ti1—Cl1127.79 (5)C4—C3—H3A125.6
N1—Ti1—C4142.68 (6)C2—C3—H3A125.6
N2—Ti1—C4103.72 (6)Ti1—C3—H3A125.6
C3—Ti1—C434.84 (7)C3—C4—C5107.55 (16)
Cl1—Ti1—C494.10 (5)C3—C4—Ti172.18 (10)
N1—Ti1—C288.12 (6)C5—C4—Ti174.46 (10)
N2—Ti1—C2106.77 (6)C3—C4—H4A125.9
C3—Ti1—C234.86 (6)C5—C4—H4A125.9
Cl1—Ti1—C2144.14 (5)Ti1—C4—H4A125.9
C4—Ti1—C257.91 (6)C1—C5—C4108.43 (17)
N1—Ti1—C5115.58 (6)C1—C5—Ti173.75 (10)
N2—Ti1—C5138.33 (6)C4—C5—Ti170.92 (10)
C3—Ti1—C557.34 (7)C1—C5—H5A125.7
Cl1—Ti1—C587.04 (5)C4—C5—H5A125.7
C4—Ti1—C534.62 (7)Ti1—C5—H5A125.7
C2—Ti1—C557.12 (6)N1—C6—H6A109.5
N1—Ti1—C186.39 (6)N1—C6—H6B109.5
N2—Ti1—C1140.92 (6)H6A—C6—H6B109.5
C3—Ti1—C157.25 (6)N1—C6—H6C109.5
Cl1—Ti1—C1113.07 (5)H6A—C6—H6C109.5
C4—Ti1—C157.10 (6)H6B—C6—H6C109.5
C2—Ti1—C134.50 (6)N1—C7—H7A109.5
C5—Ti1—C133.69 (6)N1—C7—H7B109.5
C7—N1—C6110.52 (13)H7A—C7—H7B109.5
C7—N1—Ti1138.73 (11)N1—C7—H7C109.5
C6—N1—Ti1110.47 (10)H7A—C7—H7C109.5
C8—N2—C9111.34 (14)H7B—C7—H7C109.5
C8—N2—Ti1127.78 (11)N2—C8—H8A109.5
C9—N2—Ti1119.37 (11)N2—C8—H8B109.5
C5—C1—C2108.07 (16)H8A—C8—H8B109.5
C5—C1—Ti172.57 (10)N2—C8—H8C109.5
C2—C1—Ti170.62 (9)H8A—C8—H8C109.5
C5—C1—H1A125.9H8B—C8—H8C109.5
C2—C1—H1A125.9N2—C9—H9A109.5
Ti1—C1—H1A125.9N2—C9—H9B109.5
C3—C2—C1107.62 (16)H9A—C9—H9B109.5
C3—C2—Ti171.94 (9)N2—C9—H9C109.5
C1—C2—Ti174.88 (10)H9A—C9—H9C109.5
C3—C2—H2A125.9H9B—C9—H9C109.5
Mean structural parameters for CpTiClx(NR2)3-x complexes (Å, °) top
Complex(2)(3)(1a)(1b)(4)
Ti—C2.3142.3452.3742.3782.377
Ti—N1.8641.8961.8991.897/2.055
Ti—Cl2.2242.2982.3482.308
Cl—Ti—Cl102.9103.4
Cl—Ti—N106.1104.9104.2
N—Ti—N100.599.5102.6
 

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