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The title compound, hexa-μ-chloro-1:2κ4Cl;2:3κ4Cl;3:4κ4Cl-hexachloro-1κ2Cl,2κCl,3κCl,4κ2Cl-hexakis­(diethyl­amine)-1κ2N,2κN,3κN,4κ2N-tetraindium(III), [(InCl3)4(Et2NH)6] or [In4Cl12(C4H11N)6], lies about an inversion centre and consists of four octahedrally coordinated In centres linked by bridging Cl atoms to form three four-membered In2Cl2 rings.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100010362/de1146sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100010362/de1146Isup2.hkl
Contains datablock I

CCDC reference: 153868

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[In4Cl12(C4H11N)6]Z = 1
Mr = 1323.64F(000) = 652
Triclinic, P1Dx = 1.820 Mg m3
a = 10.962 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.407 (2) ÅCell parameters from 8192 reflections
c = 11.674 (2) Åθ = 1.9–25.0°
α = 95.46 (3)°µ = 2.57 mm1
β = 109.57 (3)°T = 133 K
γ = 114.20 (3)°Block, colourless
V = 1207.8 (4) Å30.3 × 0.3 × 0.1 mm
Data collection top
Stoe-Siemens-Huber four-circle
diffractometer
5291 independent reflections
Radiation source: fine-focus sealed tube4871 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Detector resolution: 8.192 pixels/mm pixels mm-1θmax = 27.1°, θmin = 1.9°
φ and ω scansh = 1412
Absorption correction: semi-empirical (using intensity measurements)
(SADABS; Sheldrick, 1999)
k = 1414
Tmin = 0.512, Tmax = 0.783l = 014
45298 measured reflections
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.054H atoms treated by a mixture of independent and constrained refinement
S = 1.14 w = 1/[σ2(Fo2) + (0.0293P)2 + 0.4598P]
where P = (Fo2 + 2Fc2)/3
5291 reflections(Δ/σ)max = 0.001
223 parametersΔρmax = 0.58 e Å3
3 restraintsΔρmin = 1.08 e Å3
Special details top

Experimental. Intensities were measured with a Siemens CCD area detector

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
In10.16254 (2)0.17520 (2)0.26727 (1)0.01588 (5)
In20.09422 (2)0.42290 (1)0.12313 (1)0.01431 (5)
Cl10.15375 (6)0.21661 (5)0.03551 (5)0.0180 (1)
Cl20.09098 (6)0.41004 (5)0.33569 (5)0.0180 (1)
Cl30.37922 (7)0.03459 (6)0.15741 (6)0.0279 (1)
Cl40.12865 (7)0.19437 (6)0.48348 (5)0.0271 (1)
Cl50.22419 (7)0.29472 (6)0.13154 (6)0.0227 (1)
Cl60.05579 (6)0.44214 (5)0.10137 (5)0.0169 (1)
N10.2675 (2)0.3108 (2)0.2337 (2)0.0178 (4)
H10.232 (3)0.350 (2)0.182 (2)0.021*
C10.2138 (3)0.4232 (2)0.3454 (2)0.0266 (5)
H110.10530.47260.38100.032*
H120.24220.38580.41110.032*
C20.2742 (3)0.5203 (3)0.3138 (3)0.0320 (6)
H210.25610.55030.24240.048*
H220.22540.59750.38730.048*
H230.38000.47570.29130.048*
C30.4310 (3)0.2349 (2)0.1691 (2)0.0245 (5)
H310.45970.16130.09720.029*
H320.46910.29500.13480.029*
C40.5005 (3)0.1773 (3)0.2570 (3)0.0382 (7)
H410.44860.13330.30480.057*
H420.60390.11200.20720.057*
H430.49390.24930.31560.057*
N20.0003 (2)0.1031 (2)0.2658 (2)0.0181 (4)
H20.054 (3)0.163 (2)0.237 (2)0.022*
C50.1007 (3)0.1161 (2)0.3956 (2)0.0225 (5)
H510.04770.04170.42640.027*
H520.12650.20050.45280.027*
C60.2404 (3)0.1151 (3)0.4029 (3)0.0387 (7)
H610.21620.03070.34870.058*
H620.30090.12450.49030.058*
H630.29490.18960.37430.058*
C70.0581 (3)0.0279 (2)0.1726 (2)0.0259 (5)
H710.02210.02840.15170.031*
H720.13580.03510.09380.031*
C80.1206 (3)0.1487 (3)0.2196 (3)0.0339 (6)
H810.04060.15280.28620.051*
H820.17310.22980.14960.051*
H830.18860.14160.25360.051*
N30.2885 (2)0.6302 (2)0.2043 (2)0.0164 (4)
H30.270 (3)0.675 (2)0.148 (2)0.020*
C90.3011 (3)0.7068 (2)0.3231 (2)0.0200 (5)
H910.35800.68590.39630.024*
H920.20170.67760.32090.024*
C100.3748 (3)0.8562 (2)0.3411 (2)0.0281 (5)
H1010.47470.88640.34660.042*
H1020.37890.90120.41910.042*
H1030.31860.87770.26930.042*
C110.4325 (3)0.6367 (2)0.2198 (2)0.0217 (5)
H1110.44720.57190.26610.026*
H1120.51260.72700.27130.026*
C120.4415 (3)0.6067 (2)0.0953 (2)0.0252 (5)
H1210.36760.51470.04680.038*
H1220.53950.61730.11050.038*
H1230.42340.66840.04770.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
In10.01848 (9)0.01507 (8)0.01782 (9)0.00917 (7)0.00935 (7)0.00713 (6)
In20.01696 (8)0.01360 (8)0.01490 (8)0.00792 (6)0.00782 (6)0.00637 (6)
Cl10.0198 (3)0.0152 (2)0.0162 (2)0.0060 (2)0.0069 (2)0.0049 (2)
Cl20.0213 (3)0.0169 (2)0.0144 (2)0.0071 (2)0.0078 (2)0.0057 (2)
Cl30.0241 (3)0.0175 (3)0.0363 (3)0.0054 (2)0.0118 (3)0.0056 (2)
Cl40.0361 (3)0.0374 (3)0.0221 (3)0.0239 (3)0.0175 (3)0.0163 (3)
Cl50.0279 (3)0.0219 (3)0.0297 (3)0.0173 (2)0.0165 (2)0.0125 (2)
Cl60.0219 (3)0.0187 (2)0.0162 (2)0.0125 (2)0.0102 (2)0.0073 (2)
N10.020 (1)0.0195 (9)0.0186 (9)0.0111 (8)0.0103 (8)0.0071 (8)
C10.034 (1)0.027 (1)0.023 (1)0.021 (1)0.009 (1)0.003 (1)
C20.042 (2)0.028 (1)0.032 (1)0.024 (1)0.014 (1)0.006 (1)
C30.021 (1)0.024 (1)0.029 (1)0.012 (1)0.008 (1)0.009 (1)
C40.033 (2)0.038 (2)0.061 (2)0.020 (1)0.032 (2)0.025 (1)
N20.025 (1)0.0164 (9)0.0194 (9)0.0124 (8)0.0125 (8)0.0094 (8)
C50.024 (1)0.025 (1)0.021 (1)0.015 (1)0.007 (1)0.0081 (9)
C60.033 (2)0.055 (2)0.042 (2)0.030 (2)0.017 (1)0.025 (2)
C70.037 (1)0.023 (1)0.025 (1)0.019 (1)0.015 (1)0.006 (1)
C80.042 (2)0.022 (1)0.037 (2)0.018 (1)0.012 (1)0.008 (1)
N30.0169 (9)0.0163 (9)0.0172 (9)0.0078 (8)0.0078 (8)0.0064 (7)
C90.024 (1)0.017 (1)0.018 (1)0.0079 (9)0.0105 (9)0.0024 (9)
C100.033 (1)0.017 (1)0.032 (1)0.008 (1)0.016 (1)0.003 (1)
C110.0179 (1)0.024 (1)0.023 (1)0.011 (1)0.007 (1)0.0053 (9)
C120.0229 (1)0.026 (1)0.031 (1)0.012 (1)0.016 (1)0.009 (1)
Geometric parameters (Å, º) top
In1—N22.256 (2)N1—C31.493 (3)
In1—N12.267 (2)N1—C11.498 (3)
In1—Cl32.394 (2)C1—C21.522 (3)
In1—Cl42.3994 (8)C3—C41.519 (4)
In1—Cl22.746 (2)N2—C51.496 (3)
In1—Cl12.8165 (8)N2—C71.505 (3)
In2—N32.263 (2)C5—C61.510 (3)
In2—Cl52.4122 (8)C7—C81.514 (4)
In2—Cl22.5109 (7)N3—C111.497 (3)
In2—Cl12.531 (2)N3—C91.499 (3)
In2—Cl62.5573 (8)C9—C101.513 (3)
In2—Cl6i2.6474 (8)C11—C121.506 (3)
Cl6—In2i2.6474 (8)
N2—In1—N1155.12 (7)Cl1—In2—Cl689.54 (5)
N2—In1—Cl396.92 (6)N3—In2—Cl6i82.61 (5)
N1—In1—Cl398.42 (6)Cl5—In2—Cl6i177.08 (2)
N2—In1—Cl499.63 (6)Cl2—In2—Cl6i88.95 (3)
N1—In1—Cl495.84 (6)Cl1—In2—Cl6i85.42 (3)
Cl3—In1—Cl4103.04 (5)Cl6—In2—Cl6i81.33 (3)
N2—In1—Cl277.64 (5)In2—Cl1—In197.88 (4)
N1—In1—Cl282.72 (5)In2—Cl2—In1100.24 (5)
Cl3—In1—Cl2165.53 (2)In2—Cl6—In2i98.67 (3)
Cl4—In1—Cl291.14 (5)C3—N1—C1112.8 (2)
N2—In1—Cl181.63 (5)C3—N1—In1112.6 (1)
N1—In1—Cl178.90 (5)C1—N1—In1115.5 (1)
Cl3—In1—Cl190.04 (4)N1—C1—C2113.3 (2)
Cl4—In1—Cl1166.54 (2)N1—C3—C4112.5 (2)
Cl2—In1—Cl175.97 (4)C5—N2—C7113.7 (2)
N3—In2—Cl598.95 (5)C5—N2—In1112.6 (1)
N3—In2—Cl292.15 (6)C7—N2—In1117.0 (2)
Cl5—In2—Cl293.45 (3)N2—C5—C6113.9 (2)
N3—In2—Cl1167.85 (5)N2—C7—C8113.9 (2)
Cl5—In2—Cl193.10 (3)C11—N3—C9110.9 (2)
Cl2—In2—Cl185.54 (4)C11—N3—In2115.1 (1)
N3—In2—Cl690.70 (6)C9—N3—In2113.5 (1)
Cl5—In2—Cl696.15 (3)N3—C9—C10112.8 (2)
Cl2—In2—Cl6169.43 (2)N3—C11—C12112.6 (2)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···Cl10.88 (2)2.75 (2)3.258 (2)118 (2)
N2—H2···Cl50.88 (2)2.62 (2)3.476 (2)167 (2)
N2—H2···Cl20.88 (2)2.76 (2)3.158 (2)110 (2)
N1—H1···Cl6i0.88 (2)2.85 (2)3.685 (2)158 (2)
N3—H3···Cl1i0.89 (2)2.78 (2)3.653 (2)168 (2)
Symmetry code: (i) x, y+1, z.
 

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