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The structure of the salt of the di-μ-chloro-bis­[tetra­chloro­zirconate(IV)] anion and the N,N′-iso­propyl-N-(tri­methyl­silyl)benzamidinium cation, (C16H29N2Si)2[Zr2Cl10]·2CH2Cl2, is reported. The anion lies about an inversion centre and shows a substantially octahedral coordination around Zr, while the structure of the cation is unequivocally assigned as that of a benzamidinium ion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103010035/na1614sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103010035/na1614Isup2.hkl
Contains datablock I

CCDC reference: 214380

Comment top

Mono(amidinate) complexes of group IV transition metals (Ti, Zr), when activated by methylaluminoxane (MAO), are active in Ziegler–Natta polymerization of ethylene, propylene and styrene (Flores, Chien & Rausch, 1995a, 1995b).

While trying to isolate, from the CH2Cl2 solution of the reaction products, the mono(amidinate) complex {C6H5—C[N—CH(CH3)2]2}ZrCl3, prepared as reported by Fenske et al. (1988) according to Scheme 1, we obtained, a crystalline compound as a by-product. 1H NMR (CD2Cl2 at room temperature): δ 0.07 (s, 9H), 1.33 (d, 6H), 1.69 (d, 6H), 3.51 (m, 1H), 4.18 (m, 1H), 6.59 (s, 1H), 7.2–8 (m, 5H). The singlet at δ 0.07 (chemical shift from TMS), which is unequivocally attributable to a trimethyl silyl group, and the wide singlet at δ 6.59 suggest that an unexpected compound was isolated, probably as a result of partial hydrolysis of ZrCl4, due to contamination of the reaction solvent with H2O traces. A similar behaviour of ZrCl4 has been reported for reaction with 1,3,5-trimethoxybenzene (Coles et al., 1999).

Crystal structure analysis of the new compound has shown that it corresponds to the chemical formula reported in Scheme 2.

An ORTEP-3 (Farrugia, 1997) diagram is shown in Fig. 1 (a partially disordered solvent molecule, CH2Cl2, is also present in the crystallographically independent unit), and selected bond lengths and angles are reported in Table 1.

The di-µ-chloro-bis[tetrachlorozirconate(IV)] anion (Zr2Cl102−) is dimeric through bridging Cl atoms across crystallographic inversion centres, and the coordination around the metal atom is substantially octahedral. As expected, the Zr—Cl bond distances are longer (ca 0.2 Å) in the case of bridging Cl atoms.

The cation is at variance with the case reported in the literature (Coles et al., 1999), in which protonation and cation formation were only inferred. In the present case, the location of the H atom is certain; in fact, it was clearly identified in a difference Fourier map as bonded to atom N2, so that the cation can be indivituated as an amidinium ion. The two C—N bond distances are equivalent, as reported in a similar amidinium cation (Schmidt & Arnold, 2002), and the N—Si bond length is considerably longer than, for example, the value reported for N,N-dimethyl-(trimethylsilyl)amine (1.72 Å; Blake et al., 1986). The latter observation suggests little evidence? of pπ–dπ bond contributions between N and Si atoms in the present case, so that the double bond is? delocalized over the N1—C1—N2 system only (delocalization toward the phenyl ring can be excluded since the plane of the ring forms a dihedral angle of 72.8 (3)° with the C1/N1/N2 plane). Actually, the formation of the three centered pπ–pπ conjugated system is probably the reason why protonation occurs on N2 instead of N1.

Experimental top

Single crystals were obtained by cooling from CH2Cl2 solution at 253 K. The crystal used in the analysis was sealed in a Lindemann capillary under a nitrogen atmosphere.

Refinement top

Reflections corresponding to systematic absences were not collected. All H atoms were positioned stereochemically, with the exception of the H atoms bonded to atoms N2 and C10, which were found from a difference Fourier synthesis. All H atoms were refined as riding, with Uiso values equal to Ueq of the carrier atom. The disorder of the CH2Cl2 solvent molecule has been modeled without constraints on the basis of three partially superimposed sites (A, B and C) with occupancy factors 0.4, 0.4 and 1/5, respectively. Seemingly, site B is obtained from site A by rotation around the Cl6A—C17A bond, and site C from site A by rotation around the Cl7A—C17A bond. Furthermore, if the solvent molecule and its nearest centrosymmetrically related molecule are considered, some of the possible relative orientations are not allowed because of the close contacts between Cl atoms.

Computing details top

Data collection: MACH3/PC & CAD-4-PC (Nonius, 1996); cell refinement: CELLFIT (Centore, 2002); data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of the cation and anion of (I), with displacement ellipsoids shown at the 30% probability level. One of the three positions of the solvent molecule is also shown.
Bis[N,N'-diisopropyl-N-(trimethylsilyl)benzamidinium] di-µ-chloro-bis[tetrachlorozirconate(IV)] dichloromethane disolvate top
Crystal data top
(C16H29N2Si)2[Zr2Cl10]·2CH2Cl2F(000) = 2560
Mr = 1261.80Dx = 1.463 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ac 2abCell parameters from 25 reflections
a = 19.61 (5) Åθ = 28.2–29.4°
b = 17.350 (2) ŵ = 1.09 mm1
c = 16.832 (2) ÅT = 293 K
V = 5727 (15) Å3Prism, white
Z = 40.60 × 0.50 × 0.30 mm
Data collection top
Enraf Nonius MACH3
diffractometer
4109 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 28.0°, θmin = 2.0°
non–profiled ω/2θ scansh = 025
Absorption correction: ϕ scan
North et al. (1968). The number of ψ scan sets used was 3. Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied.
k = 022
Tmin = 0.503, Tmax = 0.721l = 022
6872 measured reflections1 standard reflections every 126 min
6872 independent reflections intensity decay: none
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)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.147H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0624P)2 + 7.0008P]
where P = (Fo2 + 2Fc2)/3
6872 reflections(Δ/σ)max = 0.002
261 parametersΔρmax = 0.67 e Å3
0 restraintsΔρmin = 0.55 e Å3
Crystal data top
(C16H29N2Si)2[Zr2Cl10]·2CH2Cl2V = 5727 (15) Å3
Mr = 1261.80Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 19.61 (5) ŵ = 1.09 mm1
b = 17.350 (2) ÅT = 293 K
c = 16.832 (2) Å0.60 × 0.50 × 0.30 mm
Data collection top
Enraf Nonius MACH3
diffractometer
4109 reflections with I > 2σ(I)
Absorption correction: ϕ scan
North et al. (1968). The number of ψ scan sets used was 3. Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied.
Rint = 0.000
Tmin = 0.503, Tmax = 0.7211 standard reflections every 126 min
6872 measured reflections intensity decay: none
6872 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.147H-atom parameters constrained
S = 1.02Δρmax = 0.67 e Å3
6872 reflectionsΔρmin = 0.55 e Å3
261 parameters
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. ******DISORDER OF THE SOLVENT MOLECULE****** The disorder of the CH2Cl2solvent molecule has been modeled on the basis of three partially superimposed sites (A, B, C) with occupancy factors 0.4, 0.4 and 0.2 respectively. Seemingly, site B is obtained from A by rotation around the bond CL6A—C17A, and site C from site A by rotation around the bond CL7A—C17A. Furthermore, if the molecule and its nearest centrosymmetrically related one are considered, not all the possible orientations of the three sites are allowed, but B—B, B—C and C—B are forbidden since they give too close contacts between CL atoms.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr10.96881 (2)0.54489 (2)0.10439 (3)0.03928 (12)
Si10.68405 (7)0.31647 (8)0.32674 (9)0.0538 (3)
Cl10.85645 (6)0.56518 (8)0.15514 (9)0.0617 (3)
Cl20.97332 (6)0.66989 (7)0.04251 (8)0.0585 (3)
Cl31.08104 (5)0.51165 (7)0.02703 (7)0.0470 (3)
Cl40.97128 (7)0.41410 (7)0.15402 (8)0.0605 (3)
Cl51.03420 (7)0.58774 (9)0.21637 (8)0.0689 (4)
Cl6A0.8717 (3)0.4551 (3)0.3642 (3)0.196 (2)0.40
Cl6B0.8717 (3)0.4551 (3)0.3642 (3)0.196 (2)0.40
Cl7A0.9820 (3)0.3630 (4)0.3818 (4)0.200 (3)0.40
Cl7C0.9820 (3)0.3630 (4)0.3818 (4)0.200 (3)0.20
Cl80.9965 (7)0.4607 (8)0.4376 (8)0.243 (5)*0.40
Cl90.9561 (10)0.5285 (12)0.4243 (13)0.184 (7)*0.20
N10.75165 (17)0.2529 (2)0.2899 (2)0.0427 (8)
N20.82984 (19)0.2069 (2)0.1969 (2)0.0496 (9)
H20.85440.19430.23650.050*
C10.7767 (2)0.2503 (2)0.2168 (3)0.0418 (10)
C20.7461 (2)0.2976 (2)0.1533 (3)0.0402 (9)
C30.7802 (2)0.3618 (3)0.1248 (3)0.0514 (12)
H30.82260.37510.14550.051*
C40.7513 (3)0.4059 (3)0.0660 (3)0.0605 (13)
H40.77450.44860.04650.060*
C50.6884 (3)0.3872 (3)0.0358 (3)0.0641 (14)
H50.66820.41820.00260.064*
C60.6553 (3)0.3222 (3)0.0628 (3)0.0612 (14)
H60.61340.30860.04110.061*
C70.6833 (2)0.2774 (3)0.1214 (3)0.0504 (11)
H70.66050.23380.13950.050*
C80.7742 (2)0.1966 (3)0.3524 (3)0.0509 (11)
H80.74180.20300.39620.051*
C90.7673 (3)0.1129 (3)0.3270 (3)0.0650 (14)
H9A0.72240.10430.30620.065*
H9B0.80050.10160.28680.065*
H9C0.77460.08000.37210.065*
C100.8431 (3)0.2166 (4)0.3870 (3)0.0705 (16)
H10A0.84070.26370.41090.070*
H10B0.85520.17800.42710.070*
H10C0.87920.22000.34950.070*
C110.8519 (2)0.1865 (3)0.1151 (3)0.0510 (12)
H110.82360.21470.07700.051*
C120.8405 (3)0.1010 (3)0.1039 (4)0.0715 (16)
H12A0.79320.08920.11210.071*
H12B0.85340.08660.05090.071*
H12C0.86770.07290.14150.071*
C130.9247 (3)0.2092 (3)0.1035 (3)0.0714 (16)
H13A0.92910.26400.10930.071*
H13B0.95260.18380.14230.071*
H13C0.93920.19440.05120.071*
C140.6716 (3)0.4056 (3)0.2697 (4)0.0797 (19)
H14A0.65740.39310.21670.080*
H14B0.63720.43660.29480.080*
H14C0.71360.43390.26770.080*
C150.6081 (3)0.2556 (4)0.3301 (4)0.088 (2)
H15A0.61750.21020.36080.088*
H15B0.57130.28360.35410.088*
H15C0.59550.24090.27700.088*
C160.7107 (3)0.3478 (3)0.4273 (3)0.0772 (17)
H16A0.71830.30340.46010.077*
H16B0.75200.37720.42350.077*
H16C0.67550.37910.45040.077*
C17A0.9568 (10)0.4600 (11)0.3580 (6)0.256 (10)0.40
C17B0.9568 (10)0.4600 (11)0.3580 (6)0.256 (10)0.40
C17C0.9568 (10)0.4600 (11)0.3580 (6)0.256 (10)0.20
H17A0.97150.47410.30500.256*0.40
H18A0.97550.49640.39590.256*0.40
H17B0.96920.50540.32770.256*0.40
H18B0.97220.41540.32830.256*0.40
H17C0.91140.45690.33530.256*0.20
H18C0.98680.47690.31570.256*0.20
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0370 (2)0.0354 (2)0.0455 (2)0.00041 (17)0.00024 (19)0.00417 (18)
Si10.0500 (7)0.0499 (8)0.0613 (9)0.0133 (6)0.0114 (6)0.0051 (7)
Cl10.0468 (6)0.0572 (7)0.0811 (9)0.0039 (5)0.0207 (6)0.0070 (7)
Cl20.0621 (7)0.0390 (6)0.0745 (8)0.0052 (5)0.0088 (7)0.0079 (6)
Cl30.0309 (5)0.0580 (7)0.0521 (6)0.0032 (5)0.0044 (5)0.0111 (5)
Cl40.0674 (8)0.0406 (6)0.0734 (8)0.0017 (6)0.0021 (7)0.0068 (6)
Cl50.0750 (9)0.0797 (9)0.0521 (7)0.0276 (7)0.0112 (7)0.0079 (7)
Cl6A0.160 (3)0.257 (6)0.172 (4)0.051 (4)0.027 (3)0.054 (4)
Cl6B0.160 (3)0.257 (6)0.172 (4)0.051 (4)0.027 (3)0.054 (4)
Cl7A0.154 (4)0.206 (6)0.239 (7)0.014 (4)0.009 (4)0.115 (6)
Cl7C0.154 (4)0.206 (6)0.239 (7)0.014 (4)0.009 (4)0.115 (6)
N10.0402 (18)0.0426 (19)0.045 (2)0.0060 (16)0.0027 (17)0.0024 (17)
N20.048 (2)0.060 (2)0.041 (2)0.0168 (18)0.0011 (17)0.0001 (19)
C10.039 (2)0.037 (2)0.050 (3)0.0016 (18)0.000 (2)0.005 (2)
C20.039 (2)0.033 (2)0.049 (2)0.0043 (17)0.003 (2)0.0002 (19)
C30.043 (2)0.049 (3)0.062 (3)0.007 (2)0.003 (2)0.001 (2)
C40.070 (3)0.040 (3)0.072 (3)0.002 (2)0.009 (3)0.011 (3)
C50.077 (4)0.054 (3)0.061 (3)0.013 (3)0.011 (3)0.008 (3)
C60.056 (3)0.050 (3)0.077 (4)0.002 (2)0.018 (3)0.002 (3)
C70.047 (3)0.039 (2)0.065 (3)0.004 (2)0.005 (2)0.001 (2)
C80.055 (3)0.055 (3)0.043 (3)0.013 (2)0.002 (2)0.001 (2)
C90.079 (4)0.052 (3)0.065 (3)0.005 (3)0.003 (3)0.009 (3)
C100.068 (4)0.077 (4)0.066 (4)0.020 (3)0.012 (3)0.009 (3)
C110.053 (3)0.057 (3)0.043 (3)0.017 (2)0.007 (2)0.002 (2)
C120.073 (4)0.068 (4)0.073 (4)0.006 (3)0.009 (3)0.025 (3)
C130.078 (4)0.065 (3)0.072 (4)0.005 (3)0.027 (3)0.004 (3)
C140.097 (4)0.059 (3)0.084 (4)0.034 (3)0.017 (4)0.009 (3)
C150.050 (3)0.096 (5)0.117 (6)0.003 (3)0.019 (3)0.009 (4)
C160.092 (4)0.070 (4)0.070 (4)0.023 (3)0.014 (3)0.017 (3)
C17A0.35 (2)0.34 (2)0.072 (6)0.240 (19)0.003 (9)0.021 (9)
C17B0.35 (2)0.34 (2)0.072 (6)0.240 (19)0.003 (9)0.021 (9)
C17C0.35 (2)0.34 (2)0.072 (6)0.240 (19)0.003 (9)0.021 (9)
Geometric parameters (Å, º) top
Zr1—Cl12.389 (5)C8—C91.519 (7)
Zr1—Cl22.408 (6)C8—H80.9800
Zr1—Cl32.622 (5)C9—H9A0.9600
Zr1—Cl3i2.610 (7)C9—H9B0.9600
Zr1—Cl42.419 (6)C9—H9C0.9600
Zr1—Cl52.398 (6)C10—H10A0.9128
Si1—C151.827 (7)C10—H10B0.9801
Si1—N11.833 (4)C10—H10C0.9494
Si1—C141.837 (6)C11—C131.493 (8)
Si1—C161.853 (6)C11—C121.512 (7)
Cl3—Zr1i2.610 (7)C11—H110.9800
Cl6A—C17A1.674 (18)C12—H12A0.9600
Cl7A—C17A1.80 (2)C12—H12B0.9600
Cl8—C17A1.550 (18)C12—H12C0.9600
Cl9—C17A1.63 (2)C13—H13A0.9600
N1—C11.325 (5)C13—H13B0.9600
N1—C81.503 (6)C13—H13C0.9600
N2—C11.329 (6)C14—H14A0.9600
N2—C111.485 (6)C14—H14B0.9600
N2—H20.8502C14—H14C0.9600
C1—C21.474 (6)C15—H15A0.9600
C2—C31.385 (6)C15—H15B0.9600
C2—C71.389 (7)C15—H15C0.9600
C3—C41.373 (7)C16—H16A0.9600
C3—H30.9300C16—H16B0.9600
C4—C51.373 (8)C16—H16C0.9600
C4—H40.9300C17A—H17A0.9700
C5—C61.378 (7)C17A—H18A0.9699
C5—H50.9300C17A—H17B0.9700
C6—C71.371 (7)C17A—H18B0.9700
C6—H60.9300C17A—H17C0.9701
C7—H70.9300C17A—H18C0.9701
C8—C101.512 (8)
Cl1—Zr1—Cl599.58 (5)C8—C10—H10A109.3
Cl1—Zr1—Cl293.20 (5)C8—C10—H10B109.0
Cl5—Zr1—Cl292.36 (5)H10A—C10—H10B108.7
Cl1—Zr1—Cl491.91 (5)C8—C10—H10C115.1
Cl5—Zr1—Cl490.50 (5)H10A—C10—H10C105.9
Cl2—Zr1—Cl4173.66 (5)H10B—C10—H10C108.7
Cl1—Zr1—Cl3i90.74 (11)N2—C11—C13109.7 (4)
Cl5—Zr1—Cl3i169.46 (5)N2—C11—C12107.8 (4)
Cl2—Zr1—Cl3i89.17 (5)C13—C11—C12112.5 (4)
Cl4—Zr1—Cl3i87.00 (4)N2—C11—H11108.9
Cl1—Zr1—Cl3169.82 (5)C13—C11—H11108.9
Cl5—Zr1—Cl390.56 (4)C12—C11—H11108.9
Cl2—Zr1—Cl387.28 (4)C11—C12—H12A109.5
Cl4—Zr1—Cl387.04 (4)C11—C12—H12B109.5
Cl3i—Zr1—Cl379.09 (12)H12A—C12—H12B109.5
C15—Si1—N1104.6 (3)C11—C12—H12C109.5
C15—Si1—C14113.2 (3)H12A—C12—H12C109.5
N1—Si1—C14115.2 (2)H12B—C12—H12C109.5
C15—Si1—C16111.8 (3)C11—C13—H13A109.5
N1—Si1—C16106.4 (2)C11—C13—H13B109.5
C14—Si1—C16105.5 (3)H13A—C13—H13B109.5
Zr1i—Cl3—Zr1100.91 (12)C11—C13—H13C109.5
C1—N1—C8121.2 (4)H13A—C13—H13C109.5
C1—N1—Si1127.1 (3)H13B—C13—H13C109.5
C8—N1—Si1111.5 (3)Si1—C14—H14A109.5
C1—N2—C11126.6 (4)Si1—C14—H14B109.5
C1—N2—H2113.1H14A—C14—H14B109.5
C11—N2—H2120.0Si1—C14—H14C109.5
N1—C1—N2122.9 (4)H14A—C14—H14C109.5
N1—C1—C2120.2 (4)H14B—C14—H14C109.5
N2—C1—C2116.9 (4)Si1—C15—H15A109.5
C3—C2—C7119.8 (4)Si1—C15—H15B109.5
C3—C2—C1120.2 (4)H15A—C15—H15B109.5
C7—C2—C1120.0 (4)Si1—C15—H15C109.5
C4—C3—C2119.9 (5)H15A—C15—H15C109.5
C4—C3—H3120.1H15B—C15—H15C109.5
C2—C3—H3120.1Si1—C16—H16A109.5
C5—C4—C3120.4 (5)Si1—C16—H16B109.5
C5—C4—H4119.8H16A—C16—H16B109.5
C3—C4—H4119.8Si1—C16—H16C109.5
C4—C5—C6119.6 (5)H16A—C16—H16C109.5
C4—C5—H5120.2H16B—C16—H16C109.5
C6—C5—H5120.2Cl8—C17A—Cl6A116.6 (10)
C7—C6—C5120.8 (5)Cl9—C17A—Cl7A122.2 (11)
C7—C6—H6119.6Cl6A—C17A—Cl7A102.3 (7)
C5—C6—H6119.6Cl6A—C17A—H17A111.5
C6—C7—C2119.4 (4)Cl7A—C17A—H17A111.1
C6—C7—H7120.3Cl6A—C17A—H18A111.7
C2—C7—H7120.3Cl7A—C17A—H18A111.0
N1—C8—C10112.6 (4)H17A—C17A—H18A109.1
N1—C8—C9113.5 (4)Cl8—C17A—H17B108.7
C10—C8—C9114.0 (4)Cl6A—C17A—H17B109.0
N1—C8—H8105.2Cl8—C17A—H18B107.2
C10—C8—H8105.2Cl6A—C17A—H18B107.7
C9—C8—H8105.2H17B—C17A—H18B107.4
C8—C9—H9A109.5Cl9—C17A—H17C107.6
C8—C9—H9B109.5Cl7A—C17A—H17C106.8
H9A—C9—H9B109.5Cl9—C17A—H18C106.7
C8—C9—H9C109.5Cl7A—C17A—H18C106.2
H9A—C9—H9C109.5H17C—C17A—H18C106.5
H9B—C9—H9C109.5
Cl1—Zr1—Cl3—Zr1i3.2 (3)C7—C2—C3—C41.0 (7)
Cl5—Zr1—Cl3—Zr1i177.98 (5)C1—C2—C3—C4179.6 (4)
Cl2—Zr1—Cl3—Zr1i89.68 (5)C2—C3—C4—C50.8 (8)
Cl4—Zr1—Cl3—Zr1i87.51 (5)C3—C4—C5—C62.4 (8)
Cl3i—Zr1—Cl3—Zr1i0.0C4—C5—C6—C72.2 (9)
C17A—Cl7A—Cl8—Cl920.0 (14)C5—C6—C7—C20.4 (8)
Cl7A—Cl8—Cl9—C17A19.0 (12)C3—C2—C7—C61.2 (7)
C17A—Cl8—Cl9—Cl6A36.5 (7)C1—C2—C7—C6179.5 (4)
Cl7A—Cl8—Cl9—Cl6A17.5 (15)C1—N1—C8—C1078.0 (5)
C17A—Cl6A—Cl9—Cl845.8 (11)Si1—N1—C8—C10106.0 (4)
C15—Si1—N1—C1101.8 (4)C1—N1—C8—C953.4 (6)
C14—Si1—N1—C123.1 (5)Si1—N1—C8—C9122.6 (4)
C16—Si1—N1—C1139.7 (4)C1—N2—C11—C13124.9 (5)
C15—Si1—N1—C873.9 (4)C1—N2—C11—C12112.2 (5)
C14—Si1—N1—C8161.2 (3)Cl7A—Cl8—C17A—Cl9161.8 (12)
C16—Si1—N1—C844.6 (4)Cl9—Cl8—C17A—Cl6A67.2 (16)
C8—N1—C1—N210.7 (7)Cl7A—Cl8—C17A—Cl6A94.7 (11)
Si1—N1—C1—N2174.0 (3)Cl9—Cl8—C17A—Cl7A161.8 (12)
C8—N1—C1—C2170.2 (4)Cl6A—Cl9—C17A—Cl8124.5 (11)
Si1—N1—C1—C25.1 (6)Cl8—Cl9—C17A—Cl6A124.5 (11)
C11—N2—C1—N1165.4 (4)Cl8—Cl9—C17A—Cl7A20.4 (14)
C11—N2—C1—C215.4 (7)Cl6A—Cl9—C17A—Cl7A104.1 (10)
N1—C1—C2—C3107.1 (5)Cl9—Cl6A—C17A—Cl847.9 (11)
N2—C1—C2—C372.1 (6)Cl9—Cl6A—C17A—Cl7A122.8 (11)
N1—C1—C2—C773.6 (6)Cl8—Cl7A—C17A—Cl917.2 (12)
N2—C1—C2—C7107.2 (5)Cl8—Cl7A—C17A—Cl6A114.2 (10)
Symmetry code: (i) x+2, y1, z.

Experimental details

Crystal data
Chemical formula(C16H29N2Si)2[Zr2Cl10]·2CH2Cl2
Mr1261.80
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)293
a, b, c (Å)19.61 (5), 17.350 (2), 16.832 (2)
V3)5727 (15)
Z4
Radiation typeMo Kα
µ (mm1)1.09
Crystal size (mm)0.60 × 0.50 × 0.30
Data collection
DiffractometerEnraf Nonius MACH3
diffractometer
Absorption correctionϕ scan
North et al. (1968). The number of ψ scan sets used was 3. Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied.
Tmin, Tmax0.503, 0.721
No. of measured, independent and
observed [I > 2σ(I)] reflections
6872, 6872, 4109
Rint0.000
(sin θ/λ)max1)0.660
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.147, 1.02
No. of reflections6872
No. of parameters261
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.67, 0.55

Computer programs: MACH3/PC & CAD-4-PC (Nonius, 1996), CELLFIT (Centore, 2002), XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX publication routines (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Zr1—Cl12.389 (5)Zr1—Cl52.398 (6)
Zr1—Cl22.408 (6)Si1—N11.833 (4)
Zr1—Cl32.622 (5)N1—C11.325 (5)
Zr1—Cl3i2.610 (7)N2—C11.329 (6)
Zr1—Cl42.419 (6)C1—C21.474 (6)
Cl1—Zr1—Cl599.58 (5)Cl3i—Zr1—Cl379.09 (12)
Cl5—Zr1—Cl3i169.46 (5)Zr1i—Cl3—Zr1100.91 (12)
Cl1—Zr1—Cl3169.82 (5)
N2—C1—C2—C372.1 (6)N1—C1—C2—C773.6 (6)
Symmetry code: (i) x+2, y1, z.
 

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