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Poly[caesium [[μ6-carbido-dodeca­kis-μ2-chloro-hexa­zircon­ium]-tri-μ2-chloro]], Cs[(Zr6C)Cl15], crystallizes in the ortho­rhom­bic space group Pmma. The structure is built up of two symmetry-independent [(Zr6C)Cli12Cla6/2] cluster units (where `inner' and `outer' ligands are denoted by i and a, respectively), which are three-dimensionally connected to form a cluster network through all six halogen atoms on the exo positions of each octa­hedral (Zr6C) metal unit, forming Cla–a bridges. The caesium cations are distributed in several voids within the cluster network. 16 of the 23 independent atoms lie on crystallographic special positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105043076/fa1155sup1.cif
Contains datablocks h4-Cs[(Zr6C)Cl15], I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105043076/fa1155Isup2.hkl
Contains datablock I

Comment top

In the present paper, we describe the structure of the cluster compound Cs[(Zr6C)Cl15], which was prepared using Al4C3 as carbon source and reactor grade (extreme low Hf content) Zr powder and ZrCl4 [for reviews on Zr cluster chemistry see Corbett (1992, 1995, 1996, 2000)]. Being a member of the K[(Zr6C)Cl15] structure type (Ziebarth & Corbett, 1987), this compound crystallizes in the orthorhombic space group Pmma. This structure type is based on two symmetry-independent anionic cluster units, [(Zr6C)Cl12iCl6/2a] [where `inner' and `outer' ligands are denoted by i and a, respectively (Schäfer & von Schnering, 1964)] (Fig. 1), sharing the outer ligands with neighboring units, forming two different types of cluster chains. One linear chain runs along the c axis, where all cluster units are connected by linear chlorine bridges, and the other type is built up of bent chlorine bridges [Zr2—Cl3a—Zr2 = 137.7 (1)°] forming a zigzag chain of clusters along the a axis (Fig. 2). Additional bent chlorine bridges [Zr1—Cl1a—Zr3 = 132.84 (6)°] interconnect the two groups of chains leading to a three-dimensional cluster network. Within the cluster network the Cs cations are distributed on serveral sites. The title compound is structurally comparable to the boron-centered zirconium cluster compound CsK[(Zr6B)Cl15], in which the potassium site is fully occupied and the caesium cation is distributed on two sites (Ziebarth & Corbett, 1987). Contrary to CsK[(Zr6B)Cl15] the cation distribution within the cluster network in the title phase is different. Apparently the size of the cavities plays an important role. Whereas in CsK[(Zr6B)Cl15] the Wyckhoff site 4k is completely occupied by potassium, in Cs[(Zr6C)Cl15] the occupation is rather small (0.08). This site is surrounded by 10 Cl atoms with Cs3—Cl distances as short as 3.297 (6) Å, compared with the sum of the ionic (Shannon) radii of Cs and Cl of 3.55 Å (Shannon, 1976). Therefore, we can assume that this site is too small to accommodate more than marginal numbers of Cs cations.

The two remaining cation sites are filled with caesium ions as in CsK[(Zr6B)Cl15]. For both sites the Cs atoms had to be refined on split positions (Cs1/Cs2 and Cs4/Cs5). Both sites have longer distances to the surrounding Cl atoms [3.42 (1) and 3.46 (1) Å, respectively]; therefore, size restrictions are much less pronounced. The Cs4/Cs5 site is especially interesting, because the Cs atoms are disordered along a channel running down the [001] direction (Fig. 3). This might be understood as a structural hint for the possibility that this phase could be an acceptable ionic conductor. Conductivity measurements are being planned.

The coordination polyhedron of Cs3 can be described as an irregular twofold capped tetragonal prism, whereas the other two coordination environments are rather irregular. The coordination environment of each Zr atom consists of a tetragonal pyramidal arrangement of Cl atoms, a square arrangement of Zr atoms and one additional C atom.

Experimental top

Cs[(Zr6C)Cl15] is conventionally prepared from appropriate mixtures of CsCl, ZrCl4, elemental Zr and Al4C3, which are enclosed in welded niobium (or tantalum) ampoules, which in turn are sealed in evacuated silica ampoules. Reactions are carried out by heating the enclosed ampoules at 1123 K for two to three weeks. The air- and moisture-sensitive compound was obtained as dark red crystals.

Refinement top

During structure refinement, it quickly became obvious that the Cs cation is distributed on several disordered positions. As in the CsK[(Zr6B)Cl15] structure (Ziebarth & Corbett, 1987) the Wyckoff sites 4k, 2f and 2c are involved. Unconstrained refinements of all five positions (two sites split into two positions) including variations of the occupational factors indicated the site 2f to be fully occupied, which accounts for one-half of a Cs atom per formula unit. The refinement of this atom was carried out using a split position (Cs1 and Cs2), with the sum of the site occupation factors being fixed to full occupation (occupation factors are given in the deposited CIF). Using a restrained occupation for atoms Cs3, Cs4 and Cs5, the total Cs content per formula unit refines to Cs1.00 (7)[(Zr6C)Cl15]. The two independent interstitial C atoms were refined isotropically. All the other atoms were refined using anisotropic displacement parameters.

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998 or? 2001); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The independent cluster components of the title phase, with the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (*) x, y, z − 1; (#) 1/2 − x, y, z − 1.]
[Figure 2] Fig. 2. A view of the structure of the title phase down [010], showing the two independent cluster chain types. C atoms are shown as white circles, zirconium as regulary dotted circles, and outer Cl atoms as irregularly dotted circles. Inner halides and Cs atoms have been omitted for clarity.
[Figure 3] Fig. 3. Disordered Cs4 and Cs5 atoms located between cluster chains, viewed down [001] (Cs atoms are represented by displacement ellipsoids with 50% probability, Cl atoms as irregulary dotted circles, Zr atoms as regularly dotted circles and C atoms as shaded circles).
Poly[caesium [[µ4-carbido-dodecakis-µ2-chloro-hexazirconium]-tri-µ2-chloro]] top
Crystal data top
Cs[Zr6CCl15]F(000) = 2224
Mr = 1223.99Dx = 3.274 Mg m3
Orthorhombic, PmmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2a 2aCell parameters from 42 reflections
a = 18.513 (2) Åθ = 2.9–19.9°
b = 13.916 (1) ŵ = 5.47 mm1
c = 9.6383 (7) ÅT = 293 K
V = 2483.1 (4) Å3Irregular block, dark red
Z = 40.52 × 0.43 × 0.40 mm
Data collection top
Siemens P4
diffractometer
2627 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.033
Graphite monochromatorθmax = 28.0°, θmin = 2.1°
ω scansh = 124
Absorption correction: ψ scan
(Farrugia, 1999)
k = 181
Tmin = 0.047, Tmax = 0.112l = 121
4087 measured reflections2 standard reflections every 98 reflections
3223 independent reflections intensity decay: 0.0%
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)] = 0.046 w = 1/[σ2(Fo2) + (0.0687P)2 + 15.1304P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.128(Δ/σ)max = 0.001
S = 1.08Δρmax = 2.00 e Å3
3223 reflectionsΔρmin = 1.62 e Å3
141 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00071 (11)
Crystal data top
Cs[Zr6CCl15]V = 2483.1 (4) Å3
Mr = 1223.99Z = 4
Orthorhombic, PmmaMo Kα radiation
a = 18.513 (2) ŵ = 5.47 mm1
b = 13.916 (1) ÅT = 293 K
c = 9.6383 (7) Å0.52 × 0.43 × 0.40 mm
Data collection top
Siemens P4
diffractometer
2627 reflections with I > 2σ(I)
Absorption correction: ψ scan
(Farrugia, 1999)
Rint = 0.033
Tmin = 0.047, Tmax = 0.1122 standard reflections every 98 reflections
4087 measured reflections intensity decay: 0.0%
3223 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.128 w = 1/[σ2(Fo2) + (0.0687P)2 + 15.1304P]
where P = (Fo2 + 2Fc2)/3
S = 1.08Δρmax = 2.00 e Å3
3223 reflectionsΔρmin = 1.62 e Å3
141 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cs10.25000.50001.034 (1)0.060 (2)0.66 (7)
Cs20.25000.50001.071 (5)0.044 (5)0.34 (7)
Cs30.25000.2513 (5)0.6600 (7)0.025 (1)0.08
Cs40.012 (1)0.00000.534 (4)0.06 (2)0.27 (3)
Cs50.037 (2)0.00000.405 (4)0.038 (3)0.15 (3)
Zr10.47113 (3)0.38426 (4)0.34092 (6)0.0168 (2)
Zr20.61535 (4)0.50000.42067 (9)0.0164 (2)
Zr30.33744 (3)0.11620 (4)0.14316 (6)0.0161 (2)
Zr40.25000.00000.3755 (1)0.0142 (2)
Zr50.25000.00000.9088 (1)0.0168 (2)
Cl10.43813 (9)0.2512 (1)0.1532 (2)0.0289 (4)
Cl20.25000.00000.6421 (3)0.0415 (9)
Cl30.75000.50000.3207 (3)0.0257 (6)
Cl40.50000.2457 (2)0.50000.0262 (5)
Cl50.4367 (1)0.50000.1488 (2)0.0252 (4)
Cl60.59655 (8)0.3724 (1)0.2367 (2)0.0268 (3)
Cl70.34025 (7)0.3748 (1)0.4114 (2)0.0243 (3)
Cl80.25000.2560 (2)0.1398 (3)0.0254 (5)
Cl90.4426 (1)0.00000.1452 (3)0.0309 (5)
Cl100.34499 (8)0.1276 (1)0.40434 (16)0.0244 (3)
Cl110.15255 (9)0.1271 (1)0.8832 (2)0.0283 (3)
C10.50000.50000.50000.009 (2)*
C20.25000.00000.140 (1)0.011 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.076 (5)0.054 (4)0.049 (3)0.0000.0000.000
Cs20.033 (3)0.020 (3)0.079 (11)0.0000.0000.000
Cs30.023 (3)0.023 (3)0.030 (4)0.0000.0000.003 (3)
Cs40.06 (2)0.0191 (12)0.09 (3)0.0000.06 (2)0.000
Cs50.033 (6)0.036 (4)0.045 (8)0.0000.029 (5)0.000
Zr10.0102 (3)0.0169 (3)0.0232 (3)0.00108 (18)0.00091 (19)0.0020 (2)
Zr20.0084 (3)0.0176 (4)0.0233 (4)0.0000.0003 (3)0.000
Zr30.0134 (3)0.0166 (3)0.0182 (3)0.00228 (19)0.00087 (19)0.0001 (2)
Zr40.0132 (5)0.0168 (5)0.0127 (5)0.0000.0000.000
Zr50.0194 (5)0.0183 (5)0.0129 (5)0.0000.0000.000
Cl10.0268 (7)0.0291 (8)0.0310 (9)0.0142 (6)0.0072 (6)0.0090 (6)
Cl20.063 (2)0.050 (2)0.0120 (14)0.0000.0000.000
Cl30.0089 (11)0.0362 (17)0.0318 (16)0.0000.0000.000
Cl40.0233 (10)0.0182 (10)0.0370 (12)0.0000.0060 (8)0.000
Cl50.0233 (10)0.0281 (11)0.0242 (10)0.0000.0058 (8)0.000
Cl60.0155 (6)0.0300 (8)0.0348 (8)0.0015 (5)0.0038 (6)0.0114 (7)
Cl70.0112 (5)0.0267 (7)0.0350 (8)0.0049 (5)0.0005 (5)0.0082 (6)
Cl80.0224 (9)0.0169 (9)0.0370 (12)0.0000.0000.0002 (9)
Cl90.0128 (9)0.0265 (11)0.0534 (15)0.0000.0057 (9)0.000
Cl100.0255 (7)0.0262 (7)0.0215 (7)0.0083 (6)0.0039 (5)0.0022 (6)
Cl110.0326 (8)0.0298 (8)0.0225 (7)0.0109 (6)0.0068 (6)0.0026 (6)
Geometric parameters (Å, º) top
Zr—C(average)2.278 (2)Zr3—Cl12.6486 (16)
Zr—Zr(average)3.221 (1)Zr4—Cl102.5146 (14)
Zr—Cla(average)2.643 (2)Zr4—Cl22.569 (3)
Zr—Cli(average)2.527 (2)Zr5—Cl11iv2.5388 (15)
Zr1—Zr1i3.221 (1)Zr5—Cl22.571 (3)
Zr1—Zr1ii3.248 (1)Cs1—Cl3iii3.415 (13)
Zr1—Zr2iii3.2307 (9)Cs1—Cl8ix3.547 (4)
Zr1—Zr23.2115 (9)Cs1—Cl5vii3.630 (5)
Zr3—Zr3iv3.234 (1)Cs2—Cl8ix3.461 (10)
Zr3—Zr3v3.237 (1)Cs2—Cl5vii3.537 (11)
Zr3—Zr43.2014 (9)Cs2—Cl3iii3.77 (5)
Zr3—Zr5vi3.215 (1)Cs2—Cl7x4.08 (4)
Zr1—C12.2871 (6)Cs3—Cl11v3.297 (6)
Zr2—C12.2682 (7)Cs3—Cl73.389 (6)
Zr3—C22.2883 (6)Cs3—Cl6ii3.449 (4)
Zr4—C22.27 (1)Cs3—Cl3iii3.466 (7)
Zr5—C2vii2.23 (1)Cs3—Cl103.483 (6)
Zr1—Cl72.5197 (15)Cs3—Cl23.502 (7)
Zr1—Cl42.5206 (17)Cs4—Cl9xi3.35 (3)
Zr1—Cl52.5353 (18)Cs4—Cl10v3.422 (10)
Zr1—Cl62.5354 (15)Cs4—Cl4xii3.442 (5)
Zr1—Cl12.6602 (17)Cs4—Cl10xiii3.616 (16)
Zr2—Cl7iii2.5164 (16)Cs4—Cl9xii3.84 (3)
Zr2—Cl62.5339 (17)Cs5—Cl9xii3.054 (19)
Zr2—Cl32.6726 (14)Cs5—Cl10xi3.362 (12)
Zr3—Cl11viii2.5172 (17)Cs5—Cl4xi3.605 (13)
Zr3—Cl102.5262 (16)Cs5—Cl11xiv3.93 (4)
Zr3—Cl92.5306 (17)Cs5—Cl2xiv3.97 (3)
Zr3—Cl82.5306 (17)Cs5—Cl10v3.97 (2)
Zr2xv—Cl3—Zr2137.7 (1)Cl8ix—Cs1—Cl8vii146.5 (4)
Zr1—Cl1—Zr3132.84 (6)Cl8ix—Cs2—Cl3iii101.1 (8)
Zr4—Cl2—Zr5180.0Cl8ix—Cs2—Cl5vii87.7 (3)
Cl5—Zr1—Cl183.54 (5)Cl8ix—Cs2—Cl7x54.9 (5)
Cl5—Zr1—Cl688.99 (7)Cl8ix—Cs2—Cl8vii157.8 (16)
Cl5—Zr1—Zr1i50.56 (3)Cl8—Zr3—Cl184.57 (5)
Cl5—Zr1—Zr293.74 (5)Cl8—Zr3—Zr3iv140.22 (3)
C1—Zr1—Zr1ii44.767 (15)Cl8—Zr3—Zr494.23 (5)
C1—Zr1—Zr2iii44.593 (15)Cl8—Zr3—Zr5vi93.18 (5)
Cl1—Zr1—Zr1i134.10 (4)Cl9xi—Cs4—Cl10v129.3 (11)
Cl1—Zr1—Zr2134.65 (4)Cl9xi—Cs4—Cl4xii93.6 (4)
C1—Zr1—Cl1179.22 (5)Cl9xi—Cs4—Cl9xii170.1 (11)
C1—Zr1—Cl595.79 (4)Cl9xi—Cs4—Zr4131.7 (11)
C1—Zr1—Cl695.60 (4)Cl9xii—Cs5—Cl10xi145.1 (6)
C1—Zr1—Cl794.64 (4)Cl9xii—Cs5—Cl11xvi74.4 (7)
Cl4—Zr1—Cl186.01 (5)Cl9xii—Cs5—Cl2xiv118.3 (12)
Cl4—Zr1—Cl5169.55 (5)Cl9xii—Cs5—Cl4xi95.7 (2)
Cl4—Zr1—Cl689.82 (4)Cl2xiv—Cs5—Cl10v152.7 (4)
Cl4—Zr1—Zr1i139.89 (3)Cl9—Zr3—Cl184.94 (5)
Cl4—Zr1—Zr293.54 (3)Cl9—Zr3—Cl8169.49 (5)
Cl6—Zr1—Cl183.99 (5)Cl9—Zr3—Zr3v140.28 (3)
Cl6—Zr1—Zr1i93.74 (4)Cl9—Zr3—Zr493.47 (5)
Cl6—Zr1—Zr250.67 (4)Cl9—Zr3—Zr5vi94.10 (5)
Cl6i—Zr2—Cl382.86 (6)Cl10v—Cs3—Cl1060.65 (13)
Cl6—Zr2—Cl6i89.01 (8)Cl10v—Cs3—Cl258.08 (12)
Cl6—Zr2—Zr150.71 (4)Cl10v—Cs3—Zr2iii123.91 (18)
Cl3—Zr2—Zr1i133.56 (6)Cl10—Cs3—Zr589.56 (14)
C1—Zr2—Cl3178.56 (8)Cl10v—Cs4—Cl10xi117.8 (3)
C1—Zr2—Cl696.12 (4)Cl10v—Cs4—Cl4xii122.1 (3)
C1—Zr2—Cl7iii95.20 (4)Cl10xiii—Cs4—Cl9xii110.4 (10)
C1—Zr2—Zr145.410 (16)Cl10xiii—Cs4—Zr4149.6 (2)
C2—Zr3—Cl1178.7 (3)Cl10xi—Cs5—Cl10v110.3 (6)
C2—Zr3—Cl1095.6 (3)Cl10xi—Cs5—Cl11xiv105.7 (8)
C2—Zr3—Cl11viii94.6 (3)Cl10xiii—Cs5—Cl4xi119.1 (5)
C2—Zr3—Cl895.19 (4)Cl10—Zr3—Cl183.13 (5)
C2—Zr3—Cl995.32 (4)Cl10—Zr3—Cl890.00 (7)
C2—Zr3—Zr3v44.977 (15)Cl10—Zr3—Cl989.41 (7)
C2—Zr3—Zr445.2 (3)Cl10—Zr3—Zr3v93.17 (4)
C2—Zr3—Zr5vi43.8 (3)Cl10—Zr3—Zr450.41 (4)
C2—Zr4—Cl1096.35 (4)Cl10—Zr3—Zr5vi139.43 (4)
C2—Zr4—Cs3128.10 (9)Cl10—Zr4—Cl10xii167.30 (9)
C2—Zr4—Zr3xii45.618 (17)Cl10—Zr4—Cl283.65 (4)
C2vii—Zr5—Cl11iv95.57 (4)Cl10—Zr4—Zr3xii141.97 (5)
C2vii—Zr5—Cs3124.43 (10)Cl11v—Cs3—Cl10v118.6 (2)
C2vii—Zr5—Zr3vii45.364 (17)Cl11v—Cs3—Cl1166.36 (14)
Cl1—Zr3—Zr3v134.73 (4)Cl11v—Cs3—Cl260.57 (12)
Cl1—Zr3—Zr4133.54 (4)Cl11v—Cs3—Cl3iii119.24 (19)
Cl1—Zr3—Zr5vi137.44 (4)Cl11v—Cs3—Cl6xi121.2 (2)
Cl2—Zr4—Zr3134.382 (17)Cl11v—Cs3—Cl7117.21 (4)
Cl2—Zr5—Zr3vii134.636 (17)Cl11v—Cs3—Zr2iii102.76 (8)
Cl3iii—Cs1—Cl5ix107.8 (2)Cl11v—Cs3—Zr536.75 (8)
Cl3iii—Cs1—Cl8ix106.8 (2)Cl11xiv—Cs5—Cl10v133.4 (6)
Cl3iii—Cs2—Cl7x143.7 (4)Cl11xiv—Cs5—Cl11xvi53.5 (6)
Cl3iii—Cs3—Cl10122.11 (18)Cl11xiv—Cs5—Cl2xiv51.5 (5)
Cl3iii—Cs3—Cl2179.8 (2)Cl11viii—Zr3—Cl186.64 (5)
Cl3iii—Cs3—Zr5142.5 (2)Cl11viii—Zr3—Cl10169.76 (5)
Cl4xi—Cs4—Cl10xiii116.6 (6)Cl11viii—Zr3—Cl889.30 (7)
Cl4xii—Cs4—Cl4xi166.9 (14)Cl11viii—Zr3—Cl989.42 (8)
Cl4xii—Cs4—Cl9xii85.5 (6)Cl11viii—Zr3—Zr3iv93.46 (4)
Cl4xi—Cs5—Cl10v53.6 (3)Cl11viii—Zr3—Zr5vi50.81 (4)
Cl4xii—Cs5—Cl11xvi135.2 (9)Cl11iv—Zr5—Cl11v168.85 (9)
Cl4xii—Cs5—Cl2xiv102.6 (4)Cl11iv—Zr5—Cl284.43 (4)
Cl4xi—Cs5—Cl4xii143.1 (13)Cl11iv—Zr5—Cs3121.32 (7)
Cl5vii—Cs1—Cl5ix144.4 (4)Zr1ii—Cl4—Zr180.21 (7)
Cl5vii—Cs2—Cl3iii102.3 (8)Zr1i—Cl5—Cs1vi117.57 (15)
Cl5vii—Cs2—Cl5ix155.4 (16)Zr1i—Cl5—Zr178.88 (7)
Cl5vii—Cs2—Cl7ix103.2 (10)Zr1i—Zr1—Zr1ii90.0
Cl6ii—Cs3—Cl10v149.48 (18)Zr1i—Zr1—Zr2iii60.097 (12)
Cl6ii—Cs3—Cl2120.13 (12)Zr1—Zr2—Zr1i60.20 (2)
Cl6ii—Cs3—Cl3iii59.79 (11)Zr2—C1—Zr1ii90.34 (2)
Cl6ii—Cs3—Cl6xi110.9 (2)Zr2—Cl6—Zr178.62 (5)
Cl7x—Cs2—Cl7ix48.4 (5)Zr2iii—Cl7—Zr179.81 (4)
Cl7—Cs3—Cl1060.09 (10)Zr2—Zr1—Zr1i59.899 (12)
Cl7—Cs3—Cl2118.12 (19)Zr2—Zr1—Zr1ii60.02 (2)
Cl7—Cs3—Cl3iii62.08 (12)Zr2—Zr1—Zr2iii89.52 (2)
Cl7—Cs3—Cl6xi111.25 (18)Zr3xii—C2—Zr3178.3 (5)
Cl7—Cs3—Cl7v59.07 (13)Zr3xvii—Cl11—Zr578.98 (5)
Cl7—Zr1—Cl185.76 (5)Zr3v—Cl8—Zr379.53 (7)
Cl7—Zr1—Cl490.00 (4)Zr3iv—Cl9—Zr379.43 (6)
Cl7—Zr1—Cl589.33 (7)Zr3iv—Zr3—Zr3v90.0
Cl7—Zr1—Cl6169.74 (6)Zr3xii—Zr4—Zr3iv60.75 (3)
Cl7—Zr1—Zr1i93.00 (4)Zr3vii—Zr5—Zr3xviii60.39 (3)
Cl7—Zr1—Zr2139.57 (4)Zr4—C2—Zr3xii89.2 (3)
Cl7iii—Zr2—Cl385.83 (6)Zr4—Cl10—Zr378.85 (5)
Cl7iii—Zr2—Cl6168.65 (6)Zr4—Zr3—Zr3iv59.662 (13)
Cl7iii—Zr2—Cl7ii87.64 (8)Zr4—Zr3—Zr5vi89.02 (2)
Cl7iii—Zr2—Zr1140.61 (4)Zr5vi—C2—Zr3xii90.8 (3)
Cl10xi—Cs5—Cl2xiv54.3 (3)Zr5vi—Zr3—Zr3iv59.807 (13)
Cl8ix—Cs1—Cl5vii84.94 (11)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1; (iii) x+1, y+1, z+1; (iv) x, y, z; (v) x+1/2, y, z; (vi) x, y, z1; (vii) x, y, z+1; (viii) x+1/2, y, z1; (ix) x+1/2, y+1, z+1; (x) x, y+1, z+1; (xi) x1/2, y, z+1; (xii) x+1/2, y, z; (xiii) x1/2, y, z+1; (xiv) x, y, z+1; (xv) x+3/2, y+1, z; (xvi) x, y, z+1; (xvii) x+1/2, y, z+1; (xviii) x, y, z+1.

Experimental details

Crystal data
Chemical formulaCs[Zr6CCl15]
Mr1223.99
Crystal system, space groupOrthorhombic, Pmma
Temperature (K)293
a, b, c (Å)18.513 (2), 13.916 (1), 9.6383 (7)
V3)2483.1 (4)
Z4
Radiation typeMo Kα
µ (mm1)5.47
Crystal size (mm)0.52 × 0.43 × 0.40
Data collection
DiffractometerSiemens P4
diffractometer
Absorption correctionψ scan
(Farrugia, 1999)
Tmin, Tmax0.047, 0.112
No. of measured, independent and
observed [I > 2σ(I)] reflections
4087, 3223, 2627
Rint0.033
(sin θ/λ)max1)0.660
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.128, 1.08
No. of reflections3223
No. of parameters141
w = 1/[σ2(Fo2) + (0.0687P)2 + 15.1304P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.00, 1.62

Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1998 or? 2001), SHELXL97.

Selected geometric parameters (Å, º) top
Zr—C(average)2.278 (2)Zr—Cla(average)2.643 (2)
Zr—Zr(average)3.221 (1)Zr—Cli(average)2.527 (2)
Zr2i—Cl3—Zr2137.7 (1)Zr4—Cl2—Zr5180.0
Zr1—Cl1—Zr3132.84 (6)
Symmetry code: (i) x+3/2, y+1, z.
 

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