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Logo of actae2this articlesearchopen accesssubmitActa Crystallographica Section E: Crystallographic CommunicationsActa Crystallographica Section E: Crystallographic Communications
 
Acta Crystallogr E Crystallogr Commun. 2017 December 1; 73(Pt 12): 1903–1907.
Published online 2017 November 21. doi:  10.1107/S2056989017016310
PMCID: PMC5730249

Deca­chloro­cyclo­penta­silanes coordinated by pairs of chloride anions, with different cations, but the same solvent mol­ecules

Abstract

We have determined the crystal structures of two deca­chloro­cyclo­penta­silanes, namely bis­(tetra-n-butyl­ammonium) dichloride deca­chloro­cyclo­penta­silane di­chloro­methane disolvate, 2C16H36N+·2Cl·Si5Cl10·2CH2Cl2, (I), and bis­(tetra­ethyl­ammonium) dichloride deca­chloro­cyclo­penta­silane di­chloro­methane disolvate, 2C8H20N+·2Cl·Si5Cl10·2CH2Cl2, (II), both of which crystallize with discrete cations, anions, and solvent mol­ecules. In (I), the complete deca­chloro­cyclo­penta­silane ring is generated by a crystallographic twofold rotation axis. In (II), one cation is located on a general position and the other two are disordered about centres of inversion. These are the first structures featuring the structural motif of a five-membered cyclo­penta­silane ring coordinated from both sides by a chloride ion. The extended structures of (I) and (II) feature numerous C—H(...)Cl inter­actions. In (II), the N atoms are located on centres of inversion and as a result, the ethyl­ene chains are disordered over equally occupied orientations.

Keywords: crystal structure, deca­chloro­cyclo­penta­silanes, inverse-sandwich complex, C—H(...)Cl contacts

Chemical context  

The title compounds are the first known halide diadducts of the long-known perchlorinated cyclo­penta­silane Si5Cl10 (Hengge & Kovar, 1977  ). Their structures can be seen as inverse-sandwich complexes, in which two chloride ions lie above and below the planar five-membered silicon ring.

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Object name is e-73-01903-scheme1.jpg

In the recent years, new and facile synthetic protocols for the Cl diadduct [Si6Cl14]2– of dodeca­chloro­cyclo­hexa­silane have been developed. It can either be prepared through the chloride-induced disproportionation of Si2Cl6, which leads directly to [Si6Cl14]2– (Tillmann et al., 2012  , 2014  ; Tillmann, Moxter et al., 2015  ), or the Lewis acidic uncomplexed Si6Cl12 can be used as the starting material. In the latter case, mere addition of soluble chloride salts [R 4N]Cl (R = nBu or Et) leads to the formation of [Si6Cl14]2– (Dai et al., 2010  ). Given this background, it was of inter­est to investigate the Lewis acidity and ability of Si5Cl10 to bind Cl ions.

Structural commentary  

Bis(tetra-n-butyl­ammonium) dichloride deca­chloro­cyclo­penta­silane di­chloro­methane disolvate, 2C16H36N+·2Cl·Si5Cl10·2CH2Cl2, (I), crystallizes with discrete cations, anions, and solvent mol­ecules (Fig. 1  ). The five-membered deca­chloro­cyclo­penta­silane ring is located on a twofold rotation axis. The Si—Cl bond lengths range from 2.081 (3) Å for Si2—Cl21 to 2.100 (3) Å for Si2—Cl22. The Si—Si bond lengths do not vary markedly: they range from 2.339 (3) Å (Si1—Si2) to 2.347 (3) Å (Si2—Si3).

Figure 1
Perspective view of (I) with displacement ellipsoids drawn at the 50% probability level. For clarity, H atoms are omitted and only the symmetry independent mol­ecules are labelled. Atoms without labels are generated by the symmetry operator − ...

The almost planar ring (r.m.s. deviation 0.002 Å) is coord­inated by two chloride anions located above and below the ring. The distances of the chloride ions to the Si atoms [Cl1(...)Si1 2.907 (3), Cl1(...)Si2 2.914 (3), Cl1(...)Si3 2.930 (3) Å,] show that the chloride ions are located almost exactly above the centroid of the ring [distance Cl1(...)Cg = 2.1434 (16) Å].

Bis(tetra­ethyl­ammonium) dichloride deca­chloro­cyclo­penta­silane di­chloro­methane disolvate, 2C8H20N+·2Cl·Si5Cl10·2CH2Cl2, (II), crystallizes as (I) with discrete cations, anions, and solvent mol­ecules (Fig. 2  ). The Si—Cl bonds again lie in a quite narrow range [2.0805 (9) Å (Si1—Cl12) to 2.1102 (8) Å (Si2—Cl22)] and the Si—Si bond lengths are also very similar [2.3386 (8) Å (Si1—Si2) to 2.3473 (7) Å (Si4—Si5)].

Figure 2
Perspective view of (II) with displacement ellipsoids drawn at the 50% probability level. For clarity, H atoms are omitted and only one of the two disordered sites of the tetra­ethyl­ammonium cations are shown.

The five-membered deca­chloro­cyclo­penta­silane ring is almost planar (r.m.s. deviation = 0.017 Å) and coordinated by two chloride anions located above and below the ring with a Cl(...)Cg distance of 2.1781 (5) Å for Cl1 and 2.1237 (5) Å for Cl2. The Cl(...)Si distances range from 2.9381 (7) Å (Cl1(...)Si5) to 2.9645 (7) Å (Cl1(...)Si2) and from 2.8759 (8) Å (Cl2(...)Si2) to 2.9510 (7) Å (Cl2(...)Si5). Since the Cl(...)Si distances have a broader range for Cl2, it can be said that this ion is slightly displaced from a position directly over the ring centroid.

It is inter­esting to note that (I) and (II) have – apart from the different cations – the same mol­ecular stoichiometry, i.e. one Si5Cl10 ring coordinated by two chloride anions, two cations and two solvent di­chloro­methane mol­ecules. However, since (I) has twofold rotation symmetry, there are only half of the chemical entities in the asymmetric unit.

Supra­molecular features  

The components of (I) and (II) are linked by a plethora of C—H(...)Cl contacts (Tables 1  and 2  , respectively); in particular the chloride ions are surrounded by C—H groups. For an example, see Fig. 3  . As a result of the disorder of the N2 and N3 cations in (II), a plot showing the coordination of the Cl ions looks extremely crowded and is therefore omitted.

Figure 3
Perspective view of (I) showing the environment of the Cl anion. The contact to the centre of the five-membered ring is drawn as an open dashed bond. H(...)Cl contacts less than 3.5 Å are drawn as dashed lines.
Table 1
Hydrogen-bond geometry (Å, °) for (I)
Table 2
Hydrogen-bond geometry (Å, °) for (II)

Database survey  

The present structures are the first examples of a deca­chloro­cyclo­penta­silane ring coordinated by two anions. There are only two structures of a deca­chloro­cyclo­penta­silane ring in the CSD (Version 5.38 of November 2016 plus three updates; Groom et al., 2016  ), namely deca­chloro­cyclo­penta­silane 4-methyl­benzo­nitrile solvate (refcode ELAFON; Dai et al., 2010  ) and deca­chloro­cyclo­penta­silane aceto­nitrile solvate (ELAFIH; Dai et al., 2010  ). In both of them, the deca­chloro­cyclo­penta­silane ring is almost planar (0.017 Å for ELAFON and 0.001 Å for ELAFIH) and shows almost no variation in the Si—Si (2.358–2.368 Å for ELAFON and 2.342–2.349 Å for ELAFIH) and Si—Cl (2.030–2.059 Å for ELAFON and 2.034– 2.038 Å for ELAFIH) bond lengths.

The distance of the N atom to the centroid of the ring is 2.152 and 2.196 Å for ELAFON and 2.234 Å for ELAFIH. This difference could be due to the steric demand of the benzene ring in ELAFIH. The N(...)Cg distances are in the same range as the Cl(...)Cg distances in (I) and (II).

Mean values of the structural parameters of the four compared structures and dichloride dodeca­chloro­cyclo­hexa­silanes (Tillmann, Lerner & Bolte, 2015  ) are compiled in Table 3  . It is remarkable that the Si—Si and Si—Cl bond lengths do not vary significantly between the five and six-membered Si rings, but the Cl(...)Cg distance in the dodeca­chloro­cyclo­hexa­silanes is significantly shorter than for deca­chloro­cyclo­penta­silane. This might be due to the fact that the Cl ligands form a narrower cone in five- compared to six-membered rings.

Table 3
Mean values (Å) of Si—Si, Si—Cl bond lengths and Cl/N(...)Cg contacts in the title compounds and related structures

Synthesis and crystallization  

The addition of a solution of [R 4N]Cl (R = nBu or Et) in CH2Cl2 at 195 K to a solution of Si5Cl10 in CH2Cl2 furnished the Cl diadducts [R 4N]2[Si5Cl12] (R = nBu or Et) (Fig. 4  ). Crystals of [R 4N]2[Si5Cl12] (R = nBu or Et) could be harvested after storage of the reaction solution for one week at 195 K in 89% and 93% yield, respectively. Both adducts are stable in the solid phase under inert conditions. However, in solution a rapid transformation of [nBu4N]2[Si5Cl12] to [nBu4N]2[Si6Cl14] and [nBu4N]2[Si7Cl16] (Fig. 5  ) can be observed via 29Si NMR spectroscopy (for the NMR spectrum see Fig. S1 in the Supporting information), while [Et4N]2[Si5Cl12] is not soluble. For comparison, a 29Si CP/MAS NMR spectrum of single crystals of [nBu4N]2[Si5Cl12] was recorded (Fig. S2 in the Supporting information).

Figure 4
Synthesis of [R 4N]2[Si5Cl12] (R = nBu or Et).
Figure 5
Transformation of [nBu4N]2[Si5Cl12] (I) to [nBu4N]2[Si6Cl14] (R = R′ = Cl) and [nBu4N]2[Si7Cl16] (R = Cl; R′ = SiCl3).

Refinement details  

Crystal data, data collection and structure refinement details are summarized in Table 4  . H atoms were refined using a riding model, with Cmeth­yl—H = 0.98 Å or Cmethyl­ene—H = 0.99 Å and with U iso(H) = 1.5U eq(Cmeth­yl) or 1.2U eq(C).

Table 4
Experimental details

The Cl atoms of the di­chloro­methane solvent mol­ecule in (I) have rather large displacement ellipsoids, but since no valid disorder model for splitting this mol­ecule could be found, refinement with enlarged ADPs was preferred. In (II), atoms N2 and N3 are located on centres of inversion. As a result, the ethyl­ene chains are disordered over equally occupied orientations.

Supplementary Material

Crystal structure: contains datablock(s) I, II, global. DOI: 10.1107/S2056989017016310/hb7717sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989017016310/hb7717Isup2.hkl

Structure factors: contains datablock(s) II. DOI: 10.1107/S2056989017016310/hb7717IIsup3.hkl

Fig. S1. 29Si NMR spectra. DOI: 10.1107/S2056989017016310/hb7717sup4.pdf

Fig. S2. 29Si CP/MAS NMR spectrum. DOI: 10.1107/S2056989017016310/hb7717sup5.pdf

CCDC references: 1585194, 1585193

Additional supporting information: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors wish to thank Johanna Becker-Baldus for the recording of the 29Si CP/MAS NMR spectrum.

supplementary crystallographic information

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Crystal data

2C16H36N+·2Cl·Si5Cl10·2CH2Cl2F(000) = 2544
Mr = 1220.61Dx = 1.341 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 20.9091 (15) ÅCell parameters from 30920 reflections
b = 15.7423 (7) Åθ = 3.3–25.8°
c = 19.8734 (16) ŵ = 0.85 mm1
β = 112.451 (6)°T = 173 K
V = 6045.7 (7) Å3Needle, colourless
Z = 40.27 × 0.16 × 0.12 mm

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Data collection

Stoe IPDS II two-circle diffractometer4428 reflections with I > 2σ(I)
Radiation source: Genix 3D IµS microfocus X-ray sourceRint = 0.060
ω scansθmax = 25.8°, θmin = 3.3°
Absorption correction: multi-scan (X-AREA; Stoe & Cie, 2001)h = −25→25
Tmin = 0.543, Tmax = 1.000k = −18→19
32650 measured reflectionsl = −24→24
5699 independent reflections

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Refinement

Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.103H-atom parameters constrained
wR(F2) = 0.199w = 1/[σ2(Fo2) + (0.0209P)2 + 98.7944P] where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max < 0.001
5699 reflectionsΔρmax = 1.50 e Å3
258 parametersΔρmin = −1.46 e Å3

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Cl10.44920 (9)0.65838 (13)0.63371 (9)0.0392 (4)
Si10.55353 (9)0.75962 (13)0.74394 (10)0.0312 (4)
Si20.58692 (10)0.61853 (14)0.73977 (10)0.0329 (4)
Si30.50000.53144 (19)0.75000.0368 (7)
Cl110.55030 (11)0.83349 (15)0.65484 (12)0.0536 (5)
Cl120.62942 (10)0.82642 (15)0.82814 (12)0.0535 (6)
Cl210.60720 (11)0.58866 (16)0.64782 (11)0.0534 (6)
Cl220.68493 (9)0.59548 (15)0.82099 (11)0.0499 (5)
Cl310.46207 (13)0.44593 (15)0.66352 (15)0.0667 (7)
N10.3868 (3)0.7205 (4)0.4082 (3)0.0278 (12)
C10.4614 (3)0.6993 (5)0.4564 (4)0.0309 (15)
H1A0.46680.63680.45780.037*
H1B0.46990.71850.50650.037*
C20.5172 (4)0.7380 (5)0.4335 (4)0.0373 (17)
H2A0.51020.71880.38380.045*
H2B0.51350.80080.43290.045*
C30.5881 (4)0.7115 (6)0.4859 (4)0.047 (2)
H3A0.58940.64890.49130.056*
H3B0.59690.73670.53430.056*
C40.6455 (4)0.7395 (6)0.4601 (6)0.060 (3)
H4A0.69050.72100.49560.090*
H4B0.63750.71370.41270.090*
H4C0.64500.80150.45570.090*
C50.3758 (4)0.8156 (5)0.3999 (4)0.0351 (16)
H5A0.32580.82650.37280.042*
H5B0.40070.83740.37000.042*
C60.3994 (4)0.8659 (5)0.4706 (4)0.0440 (19)
H6A0.37440.84570.50100.053*
H6B0.44950.85680.49810.053*
C70.3852 (4)0.9597 (5)0.4545 (5)0.055 (2)
H7A0.33480.96850.42880.066*
H7B0.40820.97870.42190.066*
C80.4110 (5)1.0135 (6)0.5234 (6)0.078 (3)
H8A0.40081.07340.51040.116*
H8B0.38770.99570.55540.116*
H8C0.46111.00590.54850.116*
C90.3385 (3)0.6853 (5)0.4418 (4)0.0303 (15)
H9A0.29100.70450.41200.036*
H9B0.35130.71070.49080.036*
C100.3372 (4)0.5894 (5)0.4494 (4)0.0396 (17)
H10A0.32730.56230.40150.047*
H10B0.38300.56930.48350.047*
C110.2824 (4)0.5642 (5)0.4778 (4)0.044 (2)
H11A0.23640.58150.44200.053*
H11B0.29060.59510.52370.053*
C120.2818 (4)0.4698 (6)0.4915 (5)0.059 (2)
H12A0.24550.45670.50970.088*
H12B0.27270.43890.44590.088*
H12C0.32680.45250.52760.088*
C130.3714 (4)0.6817 (5)0.3333 (3)0.0348 (16)
H13A0.40260.70850.31250.042*
H13B0.38340.62060.34000.042*
C140.2978 (4)0.6896 (6)0.2779 (4)0.0412 (18)
H14A0.28390.75010.27110.049*
H14B0.26570.65890.29530.049*
C150.2940 (4)0.6515 (7)0.2051 (4)0.057 (2)
H15A0.32940.67890.19070.068*
H15B0.30490.59010.21180.068*
C160.2249 (5)0.6627 (9)0.1459 (5)0.083 (4)
H16A0.22510.63750.10090.124*
H16B0.18980.63460.15940.124*
H16C0.21430.72340.13830.124*
C1L0.1235 (8)0.4569 (8)0.2807 (9)0.110 (5)
H1L10.13170.48570.32750.132*
H1L20.09040.49240.24160.132*
Cl1L0.19998 (18)0.4539 (3)0.2681 (2)0.1200 (15)
Cl2L0.0881 (5)0.3685 (5)0.2810 (5)0.294 (6)

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cl10.0321 (9)0.0584 (12)0.0230 (8)−0.0037 (9)0.0059 (7)−0.0024 (8)
Si10.0233 (9)0.0364 (11)0.0327 (10)−0.0031 (8)0.0092 (8)−0.0029 (8)
Si20.0281 (9)0.0417 (12)0.0302 (10)0.0050 (9)0.0124 (8)−0.0018 (9)
Si30.0373 (15)0.0330 (16)0.0421 (16)0.0000.0174 (13)0.000
Cl110.0498 (11)0.0575 (14)0.0576 (13)−0.0087 (10)0.0251 (10)0.0109 (11)
Cl120.0345 (10)0.0572 (14)0.0600 (13)−0.0137 (9)0.0082 (9)−0.0193 (11)
Cl210.0526 (12)0.0739 (15)0.0441 (11)0.0101 (11)0.0302 (10)−0.0056 (10)
Cl220.0276 (9)0.0708 (15)0.0470 (11)0.0139 (9)0.0095 (8)0.0056 (10)
Cl310.0663 (15)0.0501 (13)0.0859 (18)−0.0109 (12)0.0315 (13)−0.0313 (13)
N10.027 (3)0.032 (3)0.028 (3)0.003 (2)0.014 (2)0.002 (2)
C10.025 (3)0.036 (4)0.030 (4)0.002 (3)0.009 (3)0.000 (3)
C20.044 (4)0.035 (4)0.039 (4)−0.006 (3)0.023 (3)−0.005 (3)
C30.030 (4)0.065 (6)0.045 (4)−0.006 (4)0.014 (3)−0.011 (4)
C40.045 (5)0.054 (6)0.096 (7)−0.011 (4)0.043 (5)−0.018 (5)
C50.032 (4)0.035 (4)0.040 (4)0.009 (3)0.015 (3)0.003 (3)
C60.052 (5)0.039 (4)0.046 (4)0.001 (4)0.024 (4)−0.007 (4)
C70.042 (5)0.038 (5)0.082 (7)0.005 (4)0.020 (4)−0.012 (4)
C80.063 (6)0.052 (6)0.116 (9)−0.004 (5)0.033 (6)−0.034 (6)
C90.024 (3)0.042 (4)0.025 (3)0.000 (3)0.010 (3)0.003 (3)
C100.039 (4)0.043 (4)0.041 (4)−0.002 (4)0.019 (3)0.003 (4)
C110.028 (4)0.057 (5)0.049 (5)0.001 (4)0.016 (3)0.016 (4)
C120.043 (5)0.059 (6)0.079 (7)−0.005 (4)0.027 (5)0.019 (5)
C130.040 (4)0.043 (4)0.025 (3)0.004 (3)0.017 (3)−0.002 (3)
C140.036 (4)0.055 (5)0.030 (4)−0.003 (4)0.010 (3)−0.005 (3)
C150.044 (5)0.082 (7)0.045 (5)0.005 (5)0.018 (4)−0.005 (5)
C160.056 (6)0.150 (12)0.035 (5)0.004 (7)0.009 (4)−0.019 (6)
C1L0.143 (13)0.077 (9)0.149 (13)0.017 (9)0.100 (11)−0.003 (9)
Cl1L0.087 (2)0.168 (4)0.114 (3)−0.022 (2)0.048 (2)−0.065 (3)
Cl2L0.471 (12)0.237 (7)0.350 (10)−0.225 (8)0.355 (10)−0.183 (7)

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Geometric parameters (Å, º)

Si1—Cl122.097 (3)C7—H7A0.9900
Si1—Cl112.098 (3)C7—H7B0.9900
Si1—Si22.339 (3)C8—H8A0.9800
Si1—Si1i2.341 (4)C8—H8B0.9800
Si2—Cl212.081 (3)C8—H8C0.9800
Si2—Cl222.100 (3)C9—C101.519 (10)
Si2—Si32.347 (3)C9—H9A0.9900
Si3—Cl312.086 (3)C9—H9B0.9900
Si3—Cl31i2.086 (3)C10—C111.509 (9)
Si3—Si2i2.347 (3)C10—H10A0.9900
N1—C91.513 (8)C10—H10B0.9900
N1—C51.515 (9)C11—C121.513 (12)
N1—C11.523 (8)C11—H11A0.9900
N1—C131.525 (8)C11—H11B0.9900
C1—C21.531 (9)C12—H12A0.9800
C1—H1A0.9900C12—H12B0.9800
C1—H1B0.9900C12—H12C0.9800
C2—C31.510 (10)C13—C141.518 (10)
C2—H2A0.9900C13—H13A0.9900
C2—H2B0.9900C13—H13B0.9900
C3—C41.538 (10)C14—C151.539 (10)
C3—H3A0.9900C14—H14A0.9900
C3—H3B0.9900C14—H14B0.9900
C4—H4A0.9800C15—C161.485 (12)
C4—H4B0.9800C15—H15A0.9900
C4—H4C0.9800C15—H15B0.9900
C5—C61.521 (10)C16—H16A0.9800
C5—H5A0.9900C16—H16B0.9800
C5—H5B0.9900C16—H16C0.9800
C6—C71.516 (11)C1L—Cl2L1.578 (14)
C6—H6A0.9900C1L—Cl1L1.711 (13)
C6—H6B0.9900C1L—H1L10.9900
C7—C81.522 (13)C1L—H1L20.9900
Cl12—Si1—Cl1199.57 (12)C6—C7—H7B109.2
Cl12—Si1—Si2111.06 (11)C8—C7—H7B109.2
Cl11—Si1—Si2114.22 (11)H7A—C7—H7B107.9
Cl12—Si1—Si1i112.32 (12)C7—C8—H8A109.5
Cl11—Si1—Si1i111.28 (12)C7—C8—H8B109.5
Si2—Si1—Si1i108.28 (6)H8A—C8—H8B109.5
Cl21—Si2—Cl2299.76 (11)C7—C8—H8C109.5
Cl21—Si2—Si1114.16 (12)H8A—C8—H8C109.5
Cl22—Si2—Si1110.71 (12)H8B—C8—H8C109.5
Cl21—Si2—Si3111.61 (12)N1—C9—C10116.6 (6)
Cl22—Si2—Si3113.15 (11)N1—C9—H9A108.1
Si1—Si2—Si3107.47 (10)C10—C9—H9A108.1
Cl31—Si3—Cl31i99.6 (2)N1—C9—H9B108.1
Cl31—Si3—Si2111.65 (9)C10—C9—H9B108.1
Cl31i—Si3—Si2112.64 (9)H9A—C9—H9B107.3
Cl31—Si3—Si2i112.64 (9)C11—C10—C9110.0 (6)
Cl31i—Si3—Si2i111.65 (9)C11—C10—H10A109.7
Si2—Si3—Si2i108.50 (16)C9—C10—H10A109.7
C9—N1—C5108.1 (5)C11—C10—H10B109.7
C9—N1—C1109.8 (5)C9—C10—H10B109.7
C5—N1—C1111.2 (5)H10A—C10—H10B108.2
C9—N1—C13110.9 (5)C10—C11—C12112.6 (7)
C5—N1—C13108.8 (5)C10—C11—H11A109.1
C1—N1—C13108.0 (5)C12—C11—H11A109.1
N1—C1—C2116.1 (6)C10—C11—H11B109.1
N1—C1—H1A108.3C12—C11—H11B109.1
C2—C1—H1A108.3H11A—C11—H11B107.8
N1—C1—H1B108.3C11—C12—H12A109.5
C2—C1—H1B108.3C11—C12—H12B109.5
H1A—C1—H1B107.4H12A—C12—H12B109.5
C3—C2—C1110.1 (6)C11—C12—H12C109.5
C3—C2—H2A109.6H12A—C12—H12C109.5
C1—C2—H2A109.6H12B—C12—H12C109.5
C3—C2—H2B109.6C14—C13—N1116.9 (6)
C1—C2—H2B109.6C14—C13—H13A108.1
H2A—C2—H2B108.1N1—C13—H13A108.1
C2—C3—C4112.1 (7)C14—C13—H13B108.1
C2—C3—H3A109.2N1—C13—H13B108.1
C4—C3—H3A109.2H13A—C13—H13B107.3
C2—C3—H3B109.2C13—C14—C15108.9 (6)
C4—C3—H3B109.2C13—C14—H14A109.9
H3A—C3—H3B107.9C15—C14—H14A109.9
C3—C4—H4A109.5C13—C14—H14B109.9
C3—C4—H4B109.5C15—C14—H14B109.9
H4A—C4—H4B109.5H14A—C14—H14B108.3
C3—C4—H4C109.5C16—C15—C14112.5 (7)
H4A—C4—H4C109.5C16—C15—H15A109.1
H4B—C4—H4C109.5C14—C15—H15A109.1
N1—C5—C6115.6 (6)C16—C15—H15B109.1
N1—C5—H5A108.4C14—C15—H15B109.1
C6—C5—H5A108.4H15A—C15—H15B107.8
N1—C5—H5B108.4C15—C16—H16A109.5
C6—C5—H5B108.4C15—C16—H16B109.5
H5A—C5—H5B107.4H16A—C16—H16B109.5
C7—C6—C5110.1 (7)C15—C16—H16C109.5
C7—C6—H6A109.6H16A—C16—H16C109.5
C5—C6—H6A109.6H16B—C16—H16C109.5
C7—C6—H6B109.6Cl2L—C1L—Cl1L116.2 (8)
C5—C6—H6B109.6Cl2L—C1L—H1L1108.2
H6A—C6—H6B108.2Cl1L—C1L—H1L1108.2
C6—C7—C8112.3 (8)Cl2L—C1L—H1L2108.2
C6—C7—H7A109.2Cl1L—C1L—H1L2108.2
C8—C7—H7A109.2H1L1—C1L—H1L2107.4
C9—N1—C1—C2−174.3 (6)C5—N1—C9—C10175.4 (6)
C5—N1—C1—C2−54.8 (7)C1—N1—C9—C10−63.2 (7)
C13—N1—C1—C264.6 (7)C13—N1—C9—C1056.1 (8)
N1—C1—C2—C3−179.8 (6)N1—C9—C10—C11−175.2 (6)
C1—C2—C3—C4172.9 (7)C9—C10—C11—C12−176.1 (7)
C9—N1—C5—C668.4 (7)C9—N1—C13—C1455.2 (8)
C1—N1—C5—C6−52.2 (7)C5—N1—C13—C14−63.6 (8)
C13—N1—C5—C6−171.0 (6)C1—N1—C13—C14175.6 (6)
N1—C5—C6—C7−179.9 (6)N1—C13—C14—C15176.8 (7)
C5—C6—C7—C8−177.3 (7)C13—C14—C15—C16−175.4 (9)

Symmetry code: (i) −x+1, y, −z+3/2.

Bis(tetra-n-butylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (I)   Hydrogen-bond geometry (Å, º)

D—H···AD—HH···AD···AD—H···A
C1—H1B···Cl10.992.883.686 (7)139
C2—H2A···Cl31ii0.992.893.596 (8)129
C5—H5A···Cl22iii0.992.993.945 (7)163
C9—H9B···Cl10.992.913.652 (7)132
C1L—H1L1···Cl12iii0.992.963.528 (13)119

Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x−1/2, −y+3/2, z−1/2.

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Crystal data

2C8H20N+·2Cl·Si5Cl10·2CH2Cl2Z = 2
Mr = 996.20F(000) = 1016
Triclinic, P1Dx = 1.525 Mg m3
a = 10.3596 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.9612 (5) ÅCell parameters from 153722 reflections
c = 16.0205 (6) Åθ = 3.3–30.8°
α = 89.959 (3)°µ = 1.17 mm1
β = 72.484 (3)°T = 173 K
γ = 79.534 (3)°Block, colourless
V = 2169.29 (15) Å30.23 × 0.23 × 0.20 mm

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Data collection

Stoe IPDS II two-circle diffractometer11976 reflections with I > 2σ(I)
ω scansRint = 0.043
Absorption correction: multi-scan (X-AREA; Stoe & Cie, 2001)θmax = 30.5°, θmin = 3.4°
Tmin = 0.408, Tmax = 1.000h = −14→14
62962 measured reflectionsk = −19→19
13044 independent reflectionsl = −22→22

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Refinement

Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.048H-atom parameters constrained
wR(F2) = 0.131w = 1/[σ2(Fo2) + (0.0683P)2 + 1.6519P] where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
13044 reflectionsΔρmax = 0.87 e Å3
409 parametersΔρmin = −0.84 e Å3

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Cl10.68362 (5)0.71247 (4)0.37887 (3)0.03357 (10)
Cl20.55394 (6)0.71721 (4)0.14756 (3)0.03425 (11)
Si10.79603 (6)0.63165 (4)0.19539 (4)0.03316 (12)
Si20.74595 (6)0.80223 (4)0.20699 (4)0.02939 (11)
Si30.51729 (5)0.85241 (4)0.29623 (3)0.02570 (10)
Si40.42527 (5)0.71172 (4)0.33588 (3)0.02431 (10)
Si50.59853 (6)0.57465 (4)0.27696 (4)0.02724 (11)
Cl110.97197 (6)0.57714 (6)0.23162 (6)0.0628 (2)
Cl120.86579 (9)0.57414 (5)0.06642 (4)0.0632 (2)
Cl210.88627 (7)0.86092 (6)0.25209 (5)0.05179 (16)
Cl220.78501 (6)0.86177 (4)0.08273 (4)0.04303 (13)
Cl310.49581 (7)0.94164 (4)0.40573 (4)0.04399 (13)
Cl320.39997 (6)0.94686 (4)0.23306 (4)0.04020 (12)
Cl410.33929 (5)0.71094 (4)0.47227 (3)0.03436 (10)
Cl420.24659 (5)0.71209 (4)0.29964 (4)0.03703 (11)
Cl510.63586 (6)0.47736 (4)0.36927 (4)0.04057 (12)
Cl520.53223 (8)0.48498 (4)0.20041 (4)0.04831 (15)
N10.27041 (18)0.79721 (13)−0.00541 (11)0.0299 (3)
C10.2204 (4)0.7299 (2)0.06657 (18)0.0551 (7)
H1A0.12380.72620.07170.066*
H1B0.22060.75900.12280.066*
C20.3050 (4)0.62647 (19)0.0530 (2)0.0551 (7)
H2A0.26560.58820.10240.083*
H2B0.30340.5959−0.00160.083*
H2C0.40040.62880.04970.083*
C30.2867 (3)0.7533 (2)−0.09498 (16)0.0438 (5)
H3A0.36410.6966−0.10890.053*
H3B0.31260.8021−0.13870.053*
C40.1610 (4)0.7201 (3)−0.1052 (3)0.0648 (9)
H4A0.18160.6928−0.16510.097*
H4B0.13570.6701−0.06360.097*
H4C0.08420.7759−0.09340.097*
C50.1640 (3)0.89268 (19)0.0117 (2)0.0470 (6)
H5A0.18630.9314−0.04070.056*
H5B0.07210.87670.01920.056*
C60.1555 (3)0.9554 (2)0.0910 (2)0.0545 (7)
H6A0.08521.01450.09670.082*
H6B0.13060.91870.14380.082*
H6C0.24510.97360.08370.082*
C70.4085 (3)0.81784 (18)−0.00349 (18)0.0412 (5)
H7A0.39800.84240.05660.049*
H7B0.47560.7554−0.01550.049*
C80.4683 (3)0.8892 (2)−0.0662 (2)0.0517 (6)
H8A0.55680.8970−0.05940.078*
H8B0.48260.8651−0.12640.078*
H8C0.40480.9523−0.05400.078*
N20.00000.50000.50000.0260 (4)
C21−0.0005 (4)0.6091 (3)0.5117 (3)0.0331 (8)0.5
H21A−0.08550.64830.50400.040*0.5
H21B0.08000.62700.46750.040*0.5
C21'0.0128 (5)0.5139 (3)0.5909 (3)0.0350 (8)0.5
H21C0.10130.47550.59410.042*0.5
H21D−0.06330.49120.63520.042*0.5
C220.0063 (3)0.6300 (3)0.6105 (2)0.0638 (9)
H22A0.00610.69940.61970.096*0.5
H22B−0.07400.61220.65360.096*0.5
H22C0.09080.59100.61730.096*0.5
H22D0.01440.64030.66900.096*0.5
H22E0.08230.65180.56650.096*0.5
H22F−0.08180.66750.60750.096*0.5
C230.1319 (4)0.4394 (3)0.5085 (3)0.0294 (7)0.5
H23A0.12850.36930.50400.035*0.5
H23B0.14110.45440.56660.035*0.5
C23'0.1182 (4)0.5289 (3)0.4300 (3)0.0321 (7)0.5
H23C0.11960.59860.43980.039*0.5
H23D0.10630.51970.37170.039*0.5
C240.2624 (2)0.4624 (2)0.4327 (2)0.0533 (7)
H24A0.34710.42280.43890.080*0.5
H24B0.25380.44670.37530.080*0.5
H24C0.26620.53170.43770.080*0.5
H24D0.33910.48130.38710.080*0.5
H24E0.27430.47230.49030.080*0.5
H24F0.26100.39350.42240.080*0.5
N30.00001.00000.50000.0324 (5)
C31−0.0124 (7)1.0998 (4)0.5376 (4)0.0522 (13)0.5
H31A−0.05991.10320.60150.063*0.5
H31B−0.06841.14770.51060.063*0.5
C31'0.1452 (5)1.0189 (5)0.4881 (4)0.0509 (13)0.5
H31C0.20031.00760.42550.061*0.5
H31D0.19100.97290.52210.061*0.5
C320.1392 (6)1.1271 (4)0.5199 (3)0.0956 (17)
H32A0.12941.19300.54500.143*0.5
H32B0.19411.08030.54740.143*0.5
H32C0.18551.12460.45660.143*0.5
H32D0.23301.13790.51180.143*0.5
H32E0.09511.17270.48560.143*0.5
H32F0.08571.13800.58210.143*0.5
C33−0.0905 (5)1.0176 (4)0.5927 (3)0.0412 (10)0.5
H33A−0.18501.00920.59670.049*0.5
H33B−0.09521.08510.61400.049*0.5
C33'0.0691 (5)0.9243 (4)0.5529 (3)0.0459 (11)0.5
H33C0.16290.93500.54790.055*0.5
H33D0.07650.85720.52960.055*0.5
C34−0.0250 (4)0.9384 (3)0.6531 (2)0.0724 (11)
H34A−0.08330.94900.71440.109*0.5
H34B−0.02120.87190.63180.109*0.5
H34C0.06830.94750.64900.109*0.5
H34D0.01620.89160.68790.109*0.5
H34E−0.03141.00500.67560.109*0.5
H34F−0.11750.92740.65740.109*0.5
C1L0.1880 (4)0.3162 (2)0.1144 (2)0.0565 (7)
H1L10.23300.29600.05160.068*
H1L20.09970.36110.12000.068*
Cl1A0.29537 (8)0.37721 (5)0.15334 (6)0.05663 (17)
Cl1B0.15522 (9)0.21224 (6)0.17452 (6)0.05883 (18)
C2L0.4865 (4)0.7900 (3)0.6208 (2)0.0642 (8)
H2L10.52010.82280.56570.077*
H2L20.48310.72220.60500.077*
Cl2A0.60192 (10)0.78831 (6)0.68194 (6)0.0634 (2)
Cl2B0.32076 (10)0.85079 (10)0.67916 (6)0.0828 (3)

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cl10.0361 (2)0.0429 (3)0.0274 (2)−0.01369 (19)−0.01464 (17)0.00581 (17)
Cl20.0424 (3)0.0357 (2)0.0271 (2)−0.00201 (19)−0.01742 (18)−0.00062 (16)
Si10.0284 (2)0.0311 (3)0.0307 (3)0.0042 (2)−0.0012 (2)0.0051 (2)
Si20.0258 (2)0.0307 (3)0.0279 (2)−0.00452 (19)−0.00314 (19)0.00405 (19)
Si30.0266 (2)0.0229 (2)0.0245 (2)−0.00328 (17)−0.00405 (18)−0.00117 (17)
Si40.0239 (2)0.0234 (2)0.0246 (2)−0.00303 (17)−0.00662 (17)−0.00054 (16)
Si50.0287 (2)0.0228 (2)0.0295 (2)−0.00127 (18)−0.00988 (19)−0.00119 (18)
Cl110.0288 (3)0.0663 (4)0.0855 (5)0.0061 (3)−0.0147 (3)0.0272 (4)
Cl120.0766 (5)0.0475 (3)0.0344 (3)0.0162 (3)0.0127 (3)−0.0050 (2)
Cl210.0423 (3)0.0669 (4)0.0530 (3)−0.0301 (3)−0.0132 (3)0.0083 (3)
Cl220.0427 (3)0.0432 (3)0.0342 (2)−0.0043 (2)−0.0008 (2)0.0144 (2)
Cl310.0582 (3)0.0344 (2)0.0360 (3)−0.0095 (2)−0.0090 (2)−0.0121 (2)
Cl320.0410 (3)0.0302 (2)0.0445 (3)0.00368 (19)−0.0119 (2)0.00648 (19)
Cl410.0336 (2)0.0416 (3)0.0253 (2)−0.01096 (19)−0.00306 (17)0.00253 (17)
Cl420.0285 (2)0.0429 (3)0.0433 (3)−0.00619 (18)−0.01663 (19)0.0021 (2)
Cl510.0404 (3)0.0343 (2)0.0516 (3)−0.0089 (2)−0.0198 (2)0.0174 (2)
Cl520.0629 (4)0.0337 (3)0.0529 (3)−0.0081 (2)−0.0251 (3)−0.0133 (2)
N10.0310 (8)0.0304 (8)0.0275 (7)−0.0052 (6)−0.0080 (6)0.0030 (6)
C10.0746 (19)0.0423 (13)0.0395 (12)−0.0160 (13)−0.0016 (12)0.0076 (10)
C20.085 (2)0.0343 (12)0.0522 (15)−0.0151 (13)−0.0287 (15)0.0117 (10)
C30.0530 (14)0.0456 (12)0.0365 (11)−0.0105 (10)−0.0187 (10)−0.0010 (9)
C40.069 (2)0.0598 (18)0.087 (2)−0.0171 (15)−0.0524 (19)−0.0019 (16)
C50.0357 (11)0.0378 (12)0.0634 (16)−0.0041 (9)−0.0110 (11)0.0002 (11)
C60.0512 (15)0.0407 (13)0.0554 (15)−0.0079 (11)0.0070 (12)−0.0096 (11)
C70.0378 (11)0.0392 (11)0.0498 (13)−0.0028 (9)−0.0208 (10)0.0006 (9)
C80.0378 (12)0.0480 (14)0.0643 (17)−0.0150 (10)−0.0042 (11)−0.0017 (12)
N20.0230 (9)0.0267 (10)0.0268 (10)−0.0036 (8)−0.0063 (8)0.0051 (8)
C210.0329 (18)0.0228 (16)0.040 (2)−0.0042 (14)−0.0058 (16)0.0055 (14)
C21'0.0330 (19)0.043 (2)0.0293 (17)−0.0049 (16)−0.0108 (15)0.0050 (15)
C220.0471 (15)0.073 (2)0.0663 (19)−0.0141 (14)−0.0078 (13)−0.0342 (16)
C230.0252 (16)0.0297 (17)0.0327 (17)−0.0030 (13)−0.0095 (14)0.0056 (14)
C23'0.0275 (17)0.0336 (18)0.0322 (18)−0.0082 (14)−0.0031 (14)0.0067 (14)
C240.0240 (9)0.0589 (16)0.0671 (17)−0.0074 (10)0.0005 (10)−0.0163 (13)
N30.0243 (10)0.0345 (12)0.0329 (11)0.0000 (9)−0.0037 (9)−0.0037 (9)
C310.072 (4)0.037 (2)0.040 (2)−0.006 (2)−0.009 (2)−0.0055 (19)
C31'0.030 (2)0.081 (4)0.043 (3)−0.015 (2)−0.0107 (18)0.013 (2)
C320.146 (4)0.103 (3)0.080 (3)−0.084 (3)−0.061 (3)0.023 (2)
C330.034 (2)0.049 (2)0.0292 (18)0.0039 (18)0.0004 (16)−0.0031 (17)
C33'0.033 (2)0.055 (3)0.045 (2)0.0018 (19)−0.0118 (19)0.009 (2)
C340.083 (2)0.110 (3)0.0381 (14)−0.048 (2)−0.0207 (15)0.0216 (16)
C1L0.0620 (17)0.0570 (16)0.0647 (18)−0.0176 (14)−0.0369 (15)0.0150 (13)
Cl1A0.0500 (3)0.0452 (3)0.0797 (5)−0.0104 (3)−0.0265 (3)0.0018 (3)
Cl1B0.0613 (4)0.0527 (4)0.0685 (5)−0.0195 (3)−0.0237 (4)0.0092 (3)
C2L0.0639 (19)0.078 (2)0.0503 (16)0.0043 (16)−0.0266 (14)−0.0118 (15)
Cl2A0.0746 (5)0.0622 (4)0.0588 (4)0.0015 (4)−0.0367 (4)−0.0093 (3)
Cl2B0.0612 (5)0.1170 (9)0.0576 (5)0.0084 (5)−0.0143 (4)0.0110 (5)

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Geometric parameters (Å, º)

Si1—Cl122.0805 (9)C22—H22B0.9800
Si1—Cl112.0906 (9)C22—H22C0.9800
Si1—Si22.3386 (8)C22—H22D0.9800
Si1—Si52.3469 (8)C22—H22E0.9800
Si2—Cl212.0910 (8)C22—H22F0.9800
Si2—Cl222.1102 (8)C23—C241.604 (5)
Si2—Si32.3465 (7)C23—H23A0.9900
Si3—Cl312.0849 (7)C23—H23B0.9900
Si3—Cl322.0967 (8)C23'—C241.622 (5)
Si3—Si42.3419 (7)C23'—H23C0.9900
Si4—Cl412.0977 (7)C23'—H23D0.9900
Si4—Cl422.0993 (7)C24—H24A0.9800
Si4—Si52.3473 (7)C24—H24B0.9800
Si5—Cl512.0814 (7)C24—H24C0.9800
Si5—Cl522.0890 (8)C24—H24D0.9800
N1—C31.510 (3)C24—H24E0.9800
N1—C11.516 (3)C24—H24F0.9800
N1—C71.519 (3)N3—C31ii1.487 (5)
N1—C51.533 (3)N3—C311.487 (5)
C1—C21.526 (4)N3—C33ii1.491 (4)
C1—H1A0.9900N3—C331.491 (4)
C1—H1B0.9900N3—C31'ii1.530 (5)
C2—H2A0.9800N3—C31'1.530 (5)
C2—H2B0.9800N3—C33'ii1.561 (5)
C2—H2C0.9800N3—C33'1.561 (5)
C3—C41.511 (4)C31—C321.625 (8)
C3—H3A0.9900C31—H31A0.9900
C3—H3B0.9900C31—H31B0.9900
C4—H4A0.9800C31'—C321.579 (8)
C4—H4B0.9800C31'—H31C0.9900
C4—H4C0.9800C31'—H31D0.9900
C5—C61.514 (4)C32—H32A0.9800
C5—H5A0.9900C32—H32B0.9800
C5—H5B0.9900C32—H32C0.9800
C6—H6A0.9800C32—H32D0.9800
C6—H6B0.9800C32—H32E0.9800
C6—H6C0.9800C32—H32F0.9800
C7—C81.495 (4)C33—C341.656 (6)
C7—H7A0.9900C33—H33A0.9900
C7—H7B0.9900C33—H33B0.9900
C8—H8A0.9800C33'—C341.599 (6)
C8—H8B0.9800C33'—H33C0.9900
C8—H8C0.9800C33'—H33D0.9900
N2—C23'i1.508 (4)C34—H34A0.9800
N2—C23'1.508 (4)C34—H34B0.9800
N2—C23i1.514 (4)C34—H34C0.9800
N2—C231.514 (4)C34—H34D0.9800
N2—C21'i1.517 (4)C34—H34E0.9800
N2—C21'1.517 (4)C34—H34F0.9800
N2—C211.533 (4)C1L—Cl1A1.765 (3)
N2—C21i1.533 (4)C1L—Cl1B1.769 (3)
C21—C221.633 (6)C1L—H1L10.9900
C21—H21A0.9900C1L—H1L20.9900
C21—H21B0.9900C2L—Cl2B1.746 (4)
C21'—C221.636 (6)C2L—Cl2A1.757 (3)
C21'—H21C0.9900C2L—H2L10.9900
C21'—H21D0.9900C2L—H2L20.9900
C22—H22A0.9800
Cl12—Si1—Cl1198.50 (4)C21—C22—H22A109.5
Cl12—Si1—Si2113.28 (3)C21—C22—H22B109.5
Cl11—Si1—Si2111.32 (4)H22A—C22—H22B109.5
Cl12—Si1—Si5111.49 (4)C21—C22—H22C109.5
Cl11—Si1—Si5113.90 (4)H22A—C22—H22C109.5
Si2—Si1—Si5108.23 (3)H22B—C22—H22C109.5
Cl21—Si2—Cl2298.77 (4)C21'—C22—H22D109.5
Cl21—Si2—Si1112.27 (4)C21'—C22—H22E109.5
Cl22—Si2—Si1111.72 (3)H22D—C22—H22E109.5
Cl21—Si2—Si3112.69 (3)C21'—C22—H22F109.5
Cl22—Si2—Si3113.01 (3)H22D—C22—H22F109.5
Si1—Si2—Si3108.26 (3)H22E—C22—H22F109.5
Cl31—Si3—Cl32100.07 (3)N2—C23—C24110.3 (3)
Cl31—Si3—Si4111.69 (3)N2—C23—H23A109.6
Cl32—Si3—Si4111.61 (3)C24—C23—H23A109.6
Cl31—Si3—Si2114.12 (3)N2—C23—H23B109.6
Cl32—Si3—Si2111.88 (3)C24—C23—H23B109.6
Si4—Si3—Si2107.47 (3)H23A—C23—H23B108.1
Cl41—Si4—Cl4298.87 (3)N2—C23'—C24109.6 (3)
Cl41—Si4—Si3111.22 (3)N2—C23'—H23C109.7
Cl42—Si4—Si3112.22 (3)C24—C23'—H23C109.7
Cl41—Si4—Si5112.75 (3)N2—C23'—H23D109.7
Cl42—Si4—Si5113.01 (3)C24—C23'—H23D109.7
Si3—Si4—Si5108.60 (3)H23C—C23'—H23D108.2
Cl51—Si5—Cl5299.88 (3)C23—C24—H24A109.5
Cl51—Si5—Si1113.02 (3)C23—C24—H24B109.5
Cl52—Si5—Si1112.15 (3)H24A—C24—H24B109.5
Cl51—Si5—Si4114.27 (3)C23—C24—H24C109.5
Cl52—Si5—Si4110.11 (3)H24A—C24—H24C109.5
Si1—Si5—Si4107.38 (3)H24B—C24—H24C109.5
C3—N1—C1111.90 (19)C23'—C24—H24D109.5
C3—N1—C7108.98 (18)C23'—C24—H24E109.5
C1—N1—C7109.2 (2)H24D—C24—H24E109.5
C3—N1—C5108.79 (19)C23'—C24—H24F109.5
C1—N1—C5108.2 (2)H24D—C24—H24F109.5
C7—N1—C5109.76 (17)H24E—C24—H24F109.5
N1—C1—C2115.0 (2)C31ii—N3—C31180.0 (4)
N1—C1—H1A108.5C31ii—N3—C33ii66.3 (3)
C2—C1—H1A108.5C31—N3—C33ii113.7 (3)
N1—C1—H1B108.5C31ii—N3—C33113.7 (3)
C2—C1—H1B108.5C31—N3—C3366.3 (3)
H1A—C1—H1B107.5C33ii—N3—C33180.0
C1—C2—H2A109.5C31'ii—N3—C31'180.0 (7)
C1—C2—H2B109.5C31'ii—N3—C33'ii72.4 (3)
H2A—C2—H2B109.5C31'—N3—C33'ii107.6 (3)
C1—C2—H2C109.5C31'ii—N3—C33'107.6 (3)
H2A—C2—H2C109.5C31'—N3—C33'72.4 (3)
H2B—C2—H2C109.5C33'ii—N3—C33'180.0 (3)
N1—C3—C4115.5 (2)N3—C31—C32110.4 (4)
N1—C3—H3A108.4N3—C31—H31A109.6
C4—C3—H3A108.4C32—C31—H31A109.6
N1—C3—H3B108.4N3—C31—H31B109.6
C4—C3—H3B108.4C32—C31—H31B109.6
H3A—C3—H3B107.5H31A—C31—H31B108.1
C3—C4—H4A109.5N3—C31'—C32110.7 (4)
C3—C4—H4B109.5N3—C31'—H31C109.5
H4A—C4—H4B109.5C32—C31'—H31C109.5
C3—C4—H4C109.5N3—C31'—H31D109.5
H4A—C4—H4C109.5C32—C31'—H31D109.5
H4B—C4—H4C109.5H31C—C31'—H31D108.1
C6—C5—N1115.2 (2)C31—C32—H32A109.5
C6—C5—H5A108.5C31—C32—H32B109.5
N1—C5—H5A108.5H32A—C32—H32B109.5
C6—C5—H5B108.5C31—C32—H32C109.5
N1—C5—H5B108.5H32A—C32—H32C109.5
H5A—C5—H5B107.5H32B—C32—H32C109.5
C5—C6—H6A109.5C31'—C32—H32D109.5
C5—C6—H6B109.5C31'—C32—H32E109.5
H6A—C6—H6B109.5H32D—C32—H32E109.5
C5—C6—H6C109.5C31'—C32—H32F109.5
H6A—C6—H6C109.5H32D—C32—H32F109.5
H6B—C6—H6C109.5H32E—C32—H32F109.5
C8—C7—N1116.3 (2)N3—C33—C34108.3 (3)
C8—C7—H7A108.2N3—C33—H33A110.0
N1—C7—H7A108.2C34—C33—H33A110.0
C8—C7—H7B108.2N3—C33—H33B110.0
N1—C7—H7B108.2C34—C33—H33B110.0
H7A—C7—H7B107.4H33A—C33—H33B108.4
C7—C8—H8A109.5N3—C33'—C34107.8 (3)
C7—C8—H8B109.5N3—C33'—H33C110.1
H8A—C8—H8B109.5C34—C33'—H33C110.1
C7—C8—H8C109.5N3—C33'—H33D110.1
H8A—C8—H8C109.5C34—C33'—H33D110.1
H8B—C8—H8C109.5H33C—C33'—H33D108.5
C23'i—N2—C23'180.0C33—C34—H34A109.5
C23i—N2—C23180.0 (3)C33—C34—H34B109.5
C23'i—N2—C21'i111.7 (2)H34A—C34—H34B109.5
C23'—N2—C21'i68.3 (2)C33—C34—H34C109.5
C23'i—N2—C21'68.3 (2)H34A—C34—H34C109.5
C23'—N2—C21'111.7 (2)H34B—C34—H34C109.5
C21'i—N2—C21'180.0C33'—C34—H34D109.5
C23i—N2—C2169.5 (2)C33'—C34—H34E109.5
C23—N2—C21110.5 (2)H34D—C34—H34E109.5
C23i—N2—C21i110.5 (2)C33'—C34—H34F109.5
C23—N2—C21i69.5 (2)H34D—C34—H34F109.5
C21—N2—C21i180.0 (4)H34E—C34—H34F109.5
N2—C21—C22107.8 (3)Cl1A—C1L—Cl1B110.64 (16)
N2—C21—H21A110.2Cl1A—C1L—H1L1109.5
C22—C21—H21A110.2Cl1B—C1L—H1L1109.5
N2—C21—H21B110.2Cl1A—C1L—H1L2109.5
C22—C21—H21B110.2Cl1B—C1L—H1L2109.5
H21A—C21—H21B108.5H1L1—C1L—H1L2108.1
N2—C21'—C22108.4 (3)Cl2B—C2L—Cl2A111.70 (18)
N2—C21'—H21C110.0Cl2B—C2L—H2L1109.3
C22—C21'—H21C110.0Cl2A—C2L—H2L1109.3
N2—C21'—H21D110.0Cl2B—C2L—H2L2109.3
C22—C21'—H21D110.0Cl2A—C2L—H2L2109.3
H21C—C21'—H21D108.4H2L1—C2L—H2L2107.9
C3—N1—C1—C252.6 (3)C23'i—N2—C21'—C22−117.4 (3)
C7—N1—C1—C2−68.1 (3)C23'—N2—C21'—C2262.6 (3)
C5—N1—C1—C2172.4 (3)C21—N2—C23—C24−62.3 (3)
C1—N1—C3—C453.9 (3)C21i—N2—C23—C24117.7 (3)
C7—N1—C3—C4174.8 (2)C21'i—N2—C23'—C24−119.9 (3)
C5—N1—C3—C4−65.6 (3)C21'—N2—C23'—C2460.1 (3)
C3—N1—C5—C6−168.9 (2)C33ii—N3—C31—C32−49.5 (5)
C1—N1—C5—C669.3 (3)C33—N3—C31—C32130.5 (5)
C7—N1—C5—C6−49.8 (3)C33'ii—N3—C31'—C3257.8 (4)
C3—N1—C7—C861.8 (3)C33'—N3—C31'—C32−122.2 (4)
C1—N1—C7—C8−175.7 (2)C31ii—N3—C33—C3460.0 (5)
C5—N1—C7—C8−57.2 (3)C31—N3—C33—C34−120.0 (5)
C23i—N2—C21—C22118.2 (3)C31'ii—N3—C33'—C34−58.6 (5)
C23—N2—C21—C22−61.8 (3)C31'—N3—C33'—C34121.4 (5)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y+2, −z+1.

Bis(tetraethylammonium) dichloride decachlorocyclopentasilane dichloromethane disolvate (II)   Hydrogen-bond geometry (Å, º)

D—H···AD—HH···AD···AD—H···A
C1—H1B···Cl420.992.993.829 (3)144
C2—H2C···Cl20.982.953.753 (3)139
C3—H3A···Cl52iii0.992.793.643 (3)144
C3—H3B···Cl2Biv0.992.983.804 (3)142
C5—H5B···Cl22v0.992.893.850 (3)165
C6—H6B···Cl21v0.982.863.630 (3)136
C7—H7A···Cl20.992.863.394 (2)115
C22—H22C···Cl51vi0.982.893.847 (4)165
C22—H22E···Cl410.982.903.859 (3)165
C23—H23B···Cl1vi0.992.983.465 (4)111
C23′—H23C···Cl420.992.873.497 (4)122
C24—H24C···Cl410.982.843.793 (3)164
C24—H24E···Cl51vi0.982.813.771 (3)165
C24—H24F···Cl2Avi0.982.923.778 (3)147
C31′—H31C···Cl310.992.953.434 (5)111
C32—H32F···Cl21vii0.982.763.584 (4)142
C33—H33A···Cl32ii0.992.943.515 (4)118
C33′—H33D···Cl410.992.983.630 (5)124
C34—H34A···Cl1Bi0.982.933.556 (3)123
C34—H34C···Cl2B0.982.893.716 (4)142
C34—H34A···Cl1Bi0.982.933.556 (3)123
C1L—H1L1···Cl12iii0.992.903.421 (3)114
C2L—H2L2···Cl410.992.963.465 (3)113

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y+2, −z+1; (iii) −x+1, −y+1, −z; (iv) x, y, z−1; (v) x−1, y, z; (vi) −x+1, −y+1, −z+1; (vii) −x+1, −y+2, −z+1.

References

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Articles from Acta Crystallographica Section E: Crystallographic Communications are provided here courtesy of International Union of Crystallography