Twinned caesium cerium(IV) penta­fluoride

Grzechnik, A.; Underwood, C.C.; Kolis, J.W.

doi:10.1107/S1600536814003286

inorganic compounds

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ISSN: 2056-9890

Volume 70| Part 3| March 2014| Pages i12-i13

doi:10.1107/S1600536814003286

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Twinned caesium cerium(IV) pentafluoride

Andrzej Grzechnik,^a ^* Christopher C. Underwood ^b and Joseph W. Kolis ^b

^aInstitute of Crystallography, RWTH Aachen University, Jägerstr. 17-19, 52066 Aachen, Germany, and ^bDepartment of Chemistry, Clemson University, Clemson SC 29634, USA
^*Correspondence e-mail: grzechnik@xtal.rwth-aachen.de

(Received 28 January 2014; accepted 13 February 2014; online 19 February 2014)

Single-crystals of CsCeF₅ were synthesized hydrothermally. The crystal under investigation was twinned by pseudo-merohedry with a twofold rotation around the c axis as an additional twinning operation. The crystal structure is built of layers of distorted edge- and corner-sharing CeF₈ square-antiprisms. The Cs⁺ cations are located between the layers and exhibit coordination numbers of nine. Upon compression, CsCeF₅ undergoes an irreversible phase transition at about 1 GPa.

CCDC reference: 986654

Related literature

For background to the applications of complex cerium(IV) and thorium fluorides, see: Friese et al. (2011 ); Grzechnik et al. (2007 , 2008 , 2013a ,b ); Rouse & Weller (2009 ); Underwood (2013 ); Underwood et al. (2012 ). For related structures, see: Underwood et al. (2012). The ruby luminescence method (Mao et al., 1986 ) was used for pressure calibration. According to a recent review of twinning at high pressures (Friese & Grzechnik, 2014 ), pseudo-merohedral twinning in general is not significantly affected on compression.

Experimental

Crystal data

CsCeF₅
M_r = 368
Monoclinic, P 2₁ /c
a = 8.3125 (5) Å
b = 14.2434 (6) Å
c = 8.4507 (5) Å
β = 104.566 (5)°
V = 968.39 (9) Å³
Z = 8
Mo Kα radiation
μ = 16.80 mm⁻¹
T = 295 K
0.10 × 0.08 × 0.05 mm

Data collection

STOE IPDS 2 diffractometer
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2002 ) T_min = 0.207, T_max = 0.406
55729 measured reflections
6402 independent reflections
2543 reflections with I > 3σ(I)
R_int = 0.136

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.038
S = 1.04
6402 reflections
129 parameters
Δρ_max = 1.85 e Å⁻³
Δρ_min = −1.89 e Å⁻³

Table 1
Selected bond lengths (Å)

Ce1—F3	2.133 (6)
Ce1—F4	2.304 (5)
Ce1—F5	2.256 (6)
Ce1—F5ⁱ	2.311 (6)
Ce1—F6	2.320 (5)
Ce1—F7	2.306 (6)
Ce1—F8	2.119 (7)
Ce1—F9	2.487 (6)
Ce1—F9ⁱ	2.882 (7)
Ce2—F1	2.123 (7)
Ce2—F2	2.128 (7)
Ce2—F4ⁱⁱ	2.329 (5)
Ce2—F6	2.395 (6)
Ce2—F6ⁱⁱⁱ	3.150 (7)
Ce2—F7ⁱⁱⁱ	2.322 (6)
Ce2—F9	2.304 (6)
Ce2—F10	2.242 (5)
Ce2—F10ⁱ	2.279 (6)
Cs1—F1^iv	2.928 (8)
Cs1—F2	3.152 (6)
Cs1—F2^v	2.982 (6)
Cs1—F3^vi	3.222 (7)
Cs1—F3ⁱⁱⁱ	3.229 (7)
Cs1—F5^vi	3.099 (6)
Cs1—F8	3.095 (6)
Cs1—F8^vii	3.218 (6)
Cs1—F9	2.982 (5)
Cs2—F1^vi	2.998 (6)
Cs2—F1^viii	2.998 (7)
Cs2—F2^ix	3.042 (8)
Cs2—F3^vi	3.437 (6)
Cs2—F3ⁱⁱⁱ	2.981 (6)
Cs2—F6^vi	3.125 (6)
Cs2—F7^vii	3.140 (6)
Cs2—F8	2.980 (7)
Cs2—F10^viii	3.162 (6)
Symmetry codes: (i) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[x+1, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (iv) $[-x+2, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) -x+2, -y+1, -z+1; (vi) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vii) -x+1, -y+1, -z; (viii) $[x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ix) x-1, y, z.

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: JANA2006 (Petříček et al., 2006 ); molecular graphics: DIAMOND (Brandenburg, 2000 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 986654

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536814003286/fj2660sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814003286/fj2660Isup2.hkl

checkCIF report

Introduction top

Most of the work on structural inorganic chemistry of actinide fluorides has been primarily based on the materials that crystallize from molten alkali fluoride salts (Grzechnik et al., 2007; Grzechnik et al., 2008; Friese et al., 2011). Recently, several complex thorium fluorides have been synthesized (Underwood et al., 2012; Grzechnik et al., 2013a) and advances in the synthesis of cerium (IV) fluorides have been made (Rouse et al., 2009; Grzechnik et al., 2013b). The successful use of fluoride mineralizers in the hydrothermal crystal growth of alkali thorium fluorides suggests that additional investigations into inorganic cerium (IV) fluorides may be fruitful. The chemistry of monovalent metal cerium(IV) fluorides in hydrothermal fluids was examined by Underwood (2013) and it was found that it is considerably richer than anticipated.

We are interested in the crystal structures and stabilities of cerium (IV) fluorides as they are thought to be isostructural with the actinide fluorides (Grzechnik et al., 2013b). In the recent study by Underwood et al. (2012), three new polymorphs of CsThF₅ have been synthesized hydrothermally. The tetragonal phase (phase I, P4/nmm, Z = 2), consisting of sheets of ThF₉ tricapped trigonal prisms separated by layers of Cs atoms, is a minor product in the hydrothermal conditions. Two monoclinic polymorphs (phases II and III) are synthesized at various conditions. The phase II (P2₁/c, Z = 4) is built of chains of corner-sharing ThF₉ polyhedra, while the phase III (P2₁/c, Z = 8) is built of sheets of edge- and corner-sharing ThF₉ polyhedra. The chain structure of the phase II converts into the sheet structure of the phase III at 500°C. In this study, we examine cesium cerium(IV) pentafluoride, CsCeF₅, to see whether it is indeed isostructural with CsThF₅.

Experimental top

A series of crystals mounted on glass pins was tested on a STOE IPDS 2 diffractometer and the best one was selected for the structure determination at ambient conditions and high-pressure single-crystal x-ray studies. High-pressure data were collected in the Ahsbahs-type diamond anvil cell at room temperature at 1.2, 3.1, and 5.0 GPa. A 0.250 mm hole was drilled into a stainless steel gasket preindented to a thickness of about 0.120 mm. A 4:1 mixture of methanol and ethanol was used as a pressure medium. The ruby luminescence method (Mao et al., 1986) was used for pressure calibration.

The intensities were indexed and integrated with the software X-AREA (Stoe & Cie, 2002). Due to the pseudomerohedral twinning, some reflections in the lower θ range partly overlap. During the integration the orientation matrices of both twin individuals were used simultaneously. The overlap tolerance was set to 100%, so that all overlapped reflections were included. The faces of the crystal were optimized for each individual with the program X-SHAPE (Stoe & Cie, 2002) and an absorption correction was applied with the program Jana2006 (Petříček et al., 2006). Figures 1-3 were drawn using the program DIAMOND (Brandenburg, 2000).

Synthesis and crystallization top

All reagents for the synthesis of CsCeF₅ were of analytical grade and used as purchased. The compound in this study was prepared hydrothermally as follows: 0.20 g CeF₄ (Strem Chemical, 99.9%) was combined with five molar equivalents (0.703 g) of CsF (Alfa Aesar, 99.9%), placed into a Parr Instruments Teflon-lined autoclave and filled with 10.0 mL water. The autoclave was then heated at 250 °C for 24 h and slowly cooled at a rate of 10 °C/h to room temperature. When the reaction was complete, the content of the autoclave was filtered and the product washed with deionized water to yield a colorless material. Powder X-ray diffraction was used to characterize the bulk solid and single crystal X-ray diffraction was used to structurally characterize the new species.

Refinement top

Crystal data, data collection and structure refinement details at ambient conditions are summarized in Table 1. The diffraction pattern could be explained assuming a monoclinic lattice with a = 8.3125 (5) Å, b = 14.2434 (6) Å, c = 8.4507 (5) Å, and b = 104.566 (5)° and a two-fold rotation around the c axis as an additional twinning operation. The twinning matrix corresponds to (-1, 0, -0.4948; 0, -1, 0; 0, 0, 1). The twinning could be classified as pseudomerohedral.

The structure was solved with the program SIR97 (Altomare et al., 1999) an it was refined with the program Jana2006 (Petříček et al., 2006). The reflections from both individuals and the twinning operation were taken into account during the refinement process. The refined twin volumes of the two individuals are 0.8830 (7) and 0.1170 (7).

Results and discussion top

All the examined crystals of CsCeF₅ are pseudomerohedrally twinned and have their lattice parameters close to those for the high-temperature polymorph of CsThF₅ (phase III) (Underwood et al., 2012). We do not find any material whose single-crystal or powder x-ray intensities could be indexed with the lattices analogous to those in the phases I and II of CsThF₅. It indicates that CsCeF₅ does not exhibit any temperature-induced polymorphism within the synthesis conditions.

The analysis of the structural data in Table 2 shows that, unlike the Th atoms in the phase III of CsThF₅, the Ce atoms are eight-fold coordinated to the fluorine atoms in the distorted square antiprismatic geometry (Figure 1): the distances Ce1—F and Ce2—F are in the ranges 2.12-2.49 Å and 2.12-2.40 Å, respectively. The average Ce1—F and Ce2—F distances are the same: 2.3 (1) Å. The doublets of edge-sharing CeF₈ polyhedra share their corners to form sheets perpendicular to the b axis (Figures 2 and 3). The Cs atoms are between the sheets and are coordinated to nine fluorine atoms. The average distances Cs1—F and Cs2—F are identical: 3.1 (1) Å. Altogether, it is clear from our data that, unlike LiCeF₅ and LiThF₅ (Grzechnik et al., 2013b), CsCeF₅ and CsThF₅ are not isostructural at ambient conditions. This suggests that inorganic structural chemistries of actinide and lanthanide (IV) fluorides are not exactly analogous.

Above about 1 GPa, the single-crystal x-ray reflections in CsCeF₅ lose their intensities, become brodened and smeared, while the crystal itself is cracked into tiny pieces. The reflections can no longer be indexed with any lattice and integrated. These changes in the diffraction pattern are irreversible on decompression to atmospheric conditions. Such a behaviour suggest a pressure-induced first-order phase transition in CsCeF₅. According to a recent review of twinned structures at high pressures (Friese et al., 2014), pseudomerohedral twinning in general is not significantly affected on compression. The broadening and smearing of the reflections could thus rather be due to the collapse of the layer structure. However, the structure of the pressure-induced form of this material cannot be determined from the current single-crystal x-ray data.

Related literature top

For background to the applications of complex cerium(IV) and thorium fluorides, see: Friese et al. (2011); Grzechnik et al. (2007, 2008, 2013a,b); Rouse & Weller (2009); Underwood (2013); Underwood et al. (2012). For related structures, see: Underwood et al. (2012). The ruby luminescence method (Mao et al., 1986) was used for pressure calibration. According to a recent review of twinning at high pressures (Friese et al., 2014), twinning by pseudo-merohedry in general is not significantly affected on compression.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA (Stoe & Cie, 2002); data reduction: X-AREA (Stoe & Cie, 2002); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: JANA2006 (Petříček et al., 2006); molecular graphics: DIAMOND (Brandenburg, 2000); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. An edge-sharing doublet of distorted square antiprisms CeF₈.
	Fig. 2. Layers of CeF₈ (left) and CsF₉ (right) polyhedra viewed along the b axis.
	Fig. 3. Crystal structure in different projections. The polyhedra around the Ce atoms are drawn.

Caesium cerium(IV) pentafluoride top

Crystal data top

CsCeF₅	F(000) = 1264
M_r = 368	D_x = 5.047 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 10057 reflections
a = 8.3125 (5) Å	θ = 5.0–32.1°
b = 14.2434 (6) Å	µ = 16.80 mm⁻¹
c = 8.4507 (5) Å	T = 295 K
β = 104.566 (5)°	Irregular shape, colourless
V = 968.39 (9) Å³	0.10 × 0.08 × 0.05 mm
Z = 8

Data collection top

STOE IPDS 2 diffractometer	6402 independent reflections
Radiation source: X-ray tube	2543 reflections with I > 3σ(I)
Plane graphite monochromator	R_int = 0.136
Detector resolution: 6.67 pixels mm^-1	θ_max = 32.0°, θ_min = 4.9°
rotation method scans	h = −12→12
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2002)	k = −21→21
T_min = 0.207, T_max = 0.406	l = −12→12
55729 measured reflections

Refinement top

Refinement on F	0 constraints
R[F² > 2σ(F²)] = 0.037	Weighting scheme based on measured s.u.'s w = 1/(σ²(F) + 0.0001F²)
wR(F²) = 0.038	(Δ/σ)_max = 0.010
S = 1.04	Δρ_max = 1.85 e Å⁻³
6402 reflections	Δρ_min = −1.89 e Å⁻³
129 parameters	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
0 restraints	Extinction coefficient: 320 (20)

Crystal data top

CsCeF₅	V = 968.39 (9) Å³
M_r = 368	Z = 8
Monoclinic, P2₁/c	Mo Kα radiation
a = 8.3125 (5) Å	µ = 16.80 mm⁻¹
b = 14.2434 (6) Å	T = 295 K
c = 8.4507 (5) Å	0.10 × 0.08 × 0.05 mm
β = 104.566 (5)°

Data collection top

STOE IPDS 2 diffractometer	6402 independent reflections
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2002)	2543 reflections with I > 3σ(I)
T_min = 0.207, T_max = 0.406	R_int = 0.136
55729 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	129 parameters
wR(F²) = 0.038	0 restraints
S = 1.04	Δρ_max = 1.85 e Å⁻³
6402 reflections	Δρ_min = −1.89 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ce1	0.55769 (5)	0.74670 (6)	0.03297 (5)	0.01796 (12)
Ce2	0.98279 (5)	0.75627 (6)	0.38963 (5)	0.01810 (12)
Cs1	0.72055 (8)	0.47560 (6)	0.29747 (8)	0.0279 (2)
Cs2	0.23935 (7)	0.52409 (6)	0.21659 (8)	0.0285 (2)
F1	1.0580 (7)	0.8988 (5)	0.3904 (9)	0.031 (2)
F2	1.0275 (8)	0.6097 (5)	0.4251 (9)	0.030 (2)
F3	0.5084 (7)	0.8919 (4)	−0.0200 (8)	0.0306 (19)
F4	0.2716 (6)	0.7548 (6)	−0.0383 (6)	0.0332 (13)
F5	0.4735 (6)	0.7877 (4)	0.2572 (7)	0.0309 (17)
F6	0.8051 (7)	0.8239 (4)	0.1490 (7)	0.0286 (17)
F7	0.7769 (7)	0.6649 (4)	−0.0219 (7)	0.0280 (16)
F8	0.4839 (7)	0.6055 (5)	0.0505 (8)	0.0311 (19)
F9	0.7275 (7)	0.6849 (4)	0.2977 (8)	0.0309 (15)
F10	1.0714 (7)	0.7753 (4)	0.6611 (6)	0.032 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ce1	0.01799 (17)	0.0192 (2)	0.01669 (18)	−0.0006 (3)	0.00442 (13)	−0.0005 (3)
Ce2	0.01748 (17)	0.0193 (3)	0.01749 (18)	0.0000 (2)	0.00426 (13)	−0.0001 (3)
Cs1	0.0277 (2)	0.0267 (4)	0.0302 (3)	0.0012 (3)	0.0091 (2)	0.0004 (3)
Cs2	0.0279 (3)	0.0285 (4)	0.0285 (3)	−0.0021 (3)	0.0060 (2)	−0.0004 (2)
F1	0.026 (3)	0.031 (4)	0.035 (3)	−0.003 (2)	0.008 (2)	0.001 (3)
F2	0.033 (3)	0.016 (3)	0.041 (4)	0.006 (2)	0.010 (3)	0.001 (3)
F3	0.031 (3)	0.025 (3)	0.037 (3)	0.000 (2)	0.012 (3)	0.005 (3)
F4	0.0222 (16)	0.049 (3)	0.0287 (17)	0.006 (4)	0.0073 (15)	0.004 (5)
F5	0.022 (2)	0.040 (3)	0.031 (3)	0.007 (2)	0.008 (2)	0.005 (3)
F6	0.025 (2)	0.025 (3)	0.032 (3)	−0.003 (2)	−0.001 (2)	0.004 (2)
F7	0.022 (2)	0.029 (3)	0.034 (3)	0.003 (2)	0.010 (2)	0.003 (2)
F8	0.031 (3)	0.025 (3)	0.036 (3)	−0.004 (2)	0.006 (2)	0.005 (3)
F9	0.028 (2)	0.022 (2)	0.036 (3)	−0.002 (2)	−0.004 (2)	0.008 (3)
F10	0.030 (2)	0.050 (5)	0.016 (2)	0.001 (2)	0.0065 (18)	0.005 (2)

Geometric parameters (Å, º) top

Ce1—F3	2.133 (6)	F1—F8ⁱⁱ	3.458 (8)
Ce1—F4	2.304 (5)	F1—F10	2.865 (9)
Ce1—F5	2.256 (6)	F1—F10ⁱ	3.166 (10)
Ce1—F5ⁱ	2.311 (6)	F2—F2^v	3.445 (10)
Ce1—F6	2.320 (5)	F2—F4ⁱⁱ	2.761 (10)
Ce1—F7	2.306 (6)	F2—F6ⁱⁱⁱ	3.107 (10)
Ce1—F8	2.119 (7)	F2—F9	2.679 (8)
Ce1—F9	2.487 (6)	F2—F10	3.051 (9)
Ce1—F9ⁱ	2.882 (7)	F2—F10ⁱ	2.864 (9)
Ce2—F1	2.123 (7)	F3—F3^x	3.106 (9)
Ce2—F2	2.128 (7)	F3—F4	2.749 (10)
Ce2—F4ⁱⁱ	2.329 (5)	F3—F5	2.848 (9)
Ce2—F6	2.395 (6)	F3—F5ⁱ	3.146 (9)
Ce2—F6ⁱⁱⁱ	3.150 (7)	F3—F6	2.700 (8)
Ce2—F7ⁱⁱⁱ	2.322 (6)	F3—F9ⁱ	2.881 (10)
Ce2—F9	2.304 (6)	F4—F5	2.676 (7)
Ce2—F10	2.242 (5)	F4—F5ⁱ	2.762 (9)
Ce2—F10ⁱ	2.279 (6)	F4—F8	2.745 (10)
Cs1—F1^iv	2.928 (8)	F4—F10^xi	2.680 (6)
Cs1—F2	3.152 (6)	F4—F10^viii	2.684 (8)
Cs1—F2^v	2.982 (6)	F5—F6	3.157 (9)
Cs1—F3^vi	3.222 (7)	F5—F7ⁱⁱⁱ	2.817 (7)
Cs1—F3ⁱⁱⁱ	3.229 (7)	F5—F8	3.142 (9)
Cs1—F5^vi	3.099 (6)	F5—F8ⁱⁱⁱ	2.891 (9)
Cs1—F8	3.095 (6)	F5—F9	2.521 (8)
Cs1—F8^vii	3.218 (6)	F5—F10^viii	3.357 (8)
Cs1—F9	2.982 (5)	F6—F7	2.664 (8)
Cs2—F1^vi	2.998 (6)	F6—F7ⁱⁱⁱ	2.853 (9)
Cs2—F1^viii	2.998 (7)	F6—F9	2.514 (9)
Cs2—F2^ix	3.042 (8)	F6—F9ⁱ	2.878 (9)
Cs2—F3^vi	3.437 (6)	F6—F10ⁱ	2.607 (8)
Cs2—F3ⁱⁱⁱ	2.981 (6)	F7—F8	2.788 (9)
Cs2—F6^vi	3.125 (6)	F7—F9	2.847 (9)
Cs2—F7^vii	3.140 (6)	F7—F9ⁱ	2.598 (8)
Cs2—F8	2.980 (7)	F7—F10ⁱ	2.684 (7)
Cs2—F10^viii	3.162 (6)	F8—F8^vii	3.153 (9)
F1—F4ⁱⁱ	2.786 (10)	F8—F9	2.760 (8)
F1—F6	2.750 (8)	F9—F10ⁱ	3.390 (9)
F1—F7ⁱⁱⁱ	2.776 (9)

F3—Ce1—F4	76.4 (3)	F3ⁱⁱⁱ—F5—F6	110.5 (2)
F3—Ce1—F5	80.9 (2)	F3ⁱⁱⁱ—F5—F7ⁱⁱⁱ	82.3 (2)
F3—Ce1—F5ⁱ	90.0 (2)	F3ⁱⁱⁱ—F5—F8	69.5 (2)
F3—Ce1—F6	74.5 (2)	F3ⁱⁱⁱ—F5—F8ⁱⁱⁱ	86.3 (2)
F3—Ce1—F7	124.6 (2)	F3ⁱⁱⁱ—F5—F9	59.9 (2)
F3—Ce1—F8	153.0 (2)	F3ⁱⁱⁱ—F5—F10^viii	82.2 (2)
F3—Ce1—F9	124.6 (2)	F4—F5—F4ⁱⁱⁱ	102.0 (2)
F3—Ce1—F9ⁱ	68.3 (2)	F4—F5—F6	98.4 (2)
F4—Ce1—F5	71.86 (18)	F4—F5—F7ⁱⁱⁱ	155.1 (3)
F4—Ce1—F5ⁱ	73.51 (19)	F4—F5—F8	55.6 (2)
F4—Ce1—F6	146.4 (3)	F4—F5—F8ⁱⁱⁱ	140.2 (3)
F4—Ce1—F7	142.0 (2)	F4—F5—F9	109.4 (3)
F4—Ce1—F8	76.6 (3)	F4—F5—F10^viii	51.32 (17)
F4—Ce1—F9	124.6 (2)	F4ⁱⁱⁱ—F5—F6	158.3 (2)
F4—Ce1—F9ⁱ	117.07 (18)	F4ⁱⁱⁱ—F5—F7ⁱⁱⁱ	102.8 (2)
F5—Ce1—F5ⁱ	145.35 (18)	F4ⁱⁱⁱ—F5—F8	105.8 (3)
F5—Ce1—F6	87.2 (2)	F4ⁱⁱⁱ—F5—F8ⁱⁱⁱ	58.0 (2)
F5—Ce1—F7	136.69 (19)	F4ⁱⁱⁱ—F5—F9	114.1 (3)
F5—Ce1—F8	91.8 (2)	F4ⁱⁱⁱ—F5—F10^viii	50.83 (16)
F5—Ce1—F9	64.0 (2)	F6—F5—F7ⁱⁱⁱ	56.7 (2)
F5—Ce1—F9ⁱ	143.25 (19)	F6—F5—F8	80.0 (2)
F5ⁱ—Ce1—F6	122.6 (2)	F6—F5—F8ⁱⁱⁱ	108.8 (2)
F5ⁱ—Ce1—F7	75.19 (19)	F6—F5—F9	51.1 (2)
F5ⁱ—Ce1—F8	81.4 (2)	F6—F5—F10^viii	149.6 (2)
F5ⁱ—Ce1—F9	142.4 (2)	F7ⁱⁱⁱ—F5—F8	114.9 (2)
F5ⁱ—Ce1—F9ⁱ	56.81 (18)	F7ⁱⁱⁱ—F5—F8ⁱⁱⁱ	58.5 (2)
F6—Ce1—F7	70.3 (2)	F7ⁱⁱⁱ—F5—F9	57.9 (2)
F6—Ce1—F8	131.4 (2)	F7ⁱⁱⁱ—F5—F10^viii	153.6 (3)
F6—Ce1—F9	62.9 (2)	F8—F5—F8ⁱⁱⁱ	155.8 (3)
F6—Ce1—F9ⁱ	66.2 (2)	F8—F5—F9	57.1 (2)
F7—Ce1—F8	78.0 (2)	F8—F5—F10^viii	79.02 (19)
F7—Ce1—F9	72.8 (2)	F8ⁱⁱⁱ—F5—F9	110.2 (3)
F7—Ce1—F9ⁱ	58.87 (18)	F8ⁱⁱⁱ—F5—F10^viii	99.3 (2)
F8—Ce1—F9	73.1 (2)	F9—F5—F10^viii	128.8 (3)
F8—Ce1—F9ⁱ	124.7 (2)	Ce1—F6—Ce2	117.4 (3)
F9—Ce1—F9ⁱ	118.33 (19)	Ce1—F6—Ce2ⁱ	93.16 (19)
F1—Ce2—F2	153.7 (2)	Ce1—F6—Cs2^xiii	114.4 (2)
F1—Ce2—F4ⁱⁱ	77.3 (3)	Ce1—F6—F1	158.2 (3)
F1—Ce2—F6	74.7 (2)	Ce1—F6—F2ⁱ	119.1 (3)
F1—Ce2—F6ⁱⁱⁱ	122.3 (2)	Ce1—F6—F3	49.59 (17)
F1—Ce2—F7ⁱⁱⁱ	77.1 (2)	Ce1—F6—F5	45.54 (15)
F1—Ce2—F9	131.9 (2)	Ce1—F6—F7	54.58 (17)
F1—Ce2—F10	82.0 (3)	Ce1—F6—F7ⁱⁱⁱ	99.0 (3)
F1—Ce2—F10ⁱ	91.9 (3)	Ce1—F6—F9	61.76 (19)
F2—Ce2—F4ⁱⁱ	76.4 (3)	Ce1—F6—F9ⁱ	66.33 (18)
F2—Ce2—F6	124.2 (2)	Ce1—F6—F10ⁱ	114.4 (3)
F2—Ce2—F6ⁱⁱⁱ	69.0 (2)	Ce2—F6—Ce2ⁱ	98.51 (19)
F2—Ce2—F7ⁱⁱⁱ	123.1 (3)	Ce2—F6—Cs2^xiii	99.35 (19)
F2—Ce2—F9	74.2 (2)	Ce2—F6—F1	48.14 (18)
F2—Ce2—F10	88.5 (2)	Ce2—F6—F2ⁱ	107.8 (2)
F2—Ce2—F10ⁱ	81.0 (3)	Ce2—F6—F3	151.6 (3)
F4ⁱⁱ—Ce2—F6	128.6 (2)	Ce2—F6—F5	94.9 (2)
F4ⁱⁱ—Ce2—F6ⁱⁱⁱ	115.26 (18)	Ce2—F6—F7	94.0 (2)
F4ⁱⁱ—Ce2—F7ⁱⁱⁱ	138.0 (2)	Ce2—F6—F7ⁱⁱⁱ	51.62 (16)
F4ⁱⁱ—Ce2—F9	149.3 (3)	Ce2—F6—F9	55.94 (18)
F4ⁱⁱ—Ce2—F10	71.9 (2)	Ce2—F6—F9ⁱ	142.1 (3)
F4ⁱⁱ—Ce2—F10ⁱ	71.13 (18)	Ce2—F6—F10ⁱ	54.00 (16)
F6—Ce2—F6ⁱⁱⁱ	116.07 (18)	Ce2ⁱ—F6—Cs2^xiii	134.6 (2)
F6—Ce2—F7ⁱⁱⁱ	74.4 (2)	Ce2ⁱ—F6—F1	104.6 (2)
F6—Ce2—F9	64.7 (2)	Ce2ⁱ—F6—F2ⁱ	39.77 (15)
F6—Ce2—F10	142.5 (2)	Ce2ⁱ—F6—F3	106.7 (2)
F6—Ce2—F10ⁱ	67.8 (2)	Ce2ⁱ—F6—F5	137.6 (2)
F6ⁱⁱⁱ—Ce2—F7ⁱⁱⁱ	55.83 (18)	Ce2ⁱ—F6—F7	46.15 (17)
F6ⁱⁱⁱ—Ce2—F9	61.40 (19)	Ce2ⁱ—F6—F7ⁱⁱⁱ	150.0 (2)
F6ⁱⁱⁱ—Ce2—F10	54.76 (18)	Ce2ⁱ—F6—F9	106.7 (2)
F6ⁱⁱⁱ—Ce2—F10ⁱ	145.75 (19)	Ce2ⁱ—F6—F9ⁱ	44.67 (15)
F7ⁱⁱⁱ—Ce2—F9	68.3 (2)	Ce2ⁱ—F6—F10ⁱ	44.62 (15)
F7ⁱⁱⁱ—Ce2—F10	72.0 (2)	Cs2^xiii—F6—F1	60.97 (19)
F7ⁱⁱⁱ—Ce2—F10ⁱ	142.19 (19)	Cs2^xiii—F6—F2ⁱ	94.9 (2)
F9—Ce2—F10	115.9 (2)	Cs2^xiii—F6—F3	71.90 (19)
F9—Ce2—F10ⁱ	95.4 (2)	Cs2^xiii—F6—F5	81.50 (19)
F10—Ce2—F10ⁱ	142.9 (2)	Cs2^xiii—F6—F7	166.0 (2)
F1^iv—Cs1—F2	81.20 (19)	Cs2^xiii—F6—F7ⁱⁱⁱ	63.18 (17)
F1^iv—Cs1—F2^v	82.0 (2)	Cs2^xiii—F6—F9	117.9 (3)
F1^iv—Cs1—F3^vi	136.22 (19)	Cs2^xiii—F6—F9ⁱ	113.5 (2)
F1^iv—Cs1—F3ⁱⁱⁱ	166.16 (19)	Cs2^xiii—F6—F10ⁱ	131.1 (2)
F1^iv—Cs1—F5^vi	88.34 (18)	F1—F6—F2ⁱ	82.7 (2)
F1^iv—Cs1—F8	103.73 (19)	F1—F6—F3	132.8 (3)
F1^iv—Cs1—F8^vii	68.29 (17)	F1—F6—F5	114.1 (3)
F1^iv—Cs1—F9	111.1 (2)	F1—F6—F7	132.7 (3)
F2—Cs1—F2^v	68.27 (17)	F1—F6—F7ⁱⁱⁱ	59.4 (2)
F2—Cs1—F3^vi	124.79 (18)	F1—F6—F9	100.3 (3)
F2—Cs1—F3ⁱⁱⁱ	88.55 (17)	F1—F6—F9ⁱ	135.5 (3)
F2—Cs1—F5^vi	156.99 (15)	F1—F6—F10ⁱ	72.4 (2)
F2—Cs1—F8	101.01 (16)	F2ⁱ—F6—F3	100.0 (3)
F2—Cs1—F8^vii	136.56 (19)	F2ⁱ—F6—F5	157.3 (2)
F2—Cs1—F9	51.69 (16)	F2ⁱ—F6—F7	85.0 (3)
F2^v—Cs1—F3^vi	77.96 (18)	F2ⁱ—F6—F7ⁱⁱⁱ	141.6 (3)
F2^v—Cs1—F3ⁱⁱⁱ	102.87 (18)	F2ⁱ—F6—F9	144.2 (3)
F2^v—Cs1—F5^vi	90.09 (16)	F2ⁱ—F6—F9ⁱ	53.0 (2)
F2^v—Cs1—F8	167.23 (17)	F2ⁱ—F6—F10ⁱ	63.8 (2)
F2^v—Cs1—F8^vii	132.64 (17)	F3—F6—F5	57.6 (2)
F2^v—Cs1—F9	113.41 (16)	F3—F6—F7	94.2 (2)
F3^vi—Cs1—F3ⁱⁱⁱ	57.57 (16)	F3—F6—F7ⁱⁱⁱ	102.0 (3)
F3^vi—Cs1—F5^vi	53.52 (16)	F3—F6—F9	103.4 (3)
F3^vi—Cs1—F8	104.26 (16)	F3—F6—F9ⁱ	62.1 (2)
F3^vi—Cs1—F8^vii	98.44 (16)	F3—F6—F10ⁱ	150.3 (3)
F3^vi—Cs1—F9	112.58 (18)	F5—F6—F7	93.1 (2)
F3ⁱⁱⁱ—Cs1—F5^vi	104.46 (16)	F5—F6—F7ⁱⁱⁱ	55.62 (19)
F3ⁱⁱⁱ—Cs1—F8	69.01 (17)	F5—F6—F9	51.3 (2)
F3ⁱⁱⁱ—Cs1—F8^vii	114.83 (15)	F5—F6—F9ⁱ	107.8 (2)
F3ⁱⁱⁱ—Cs1—F9	55.10 (18)	F5—F6—F10ⁱ	134.0 (3)
F5^vi—Cs1—F8	101.36 (15)	F7—F6—F7ⁱⁱⁱ	123.9 (3)
F5^vi—Cs1—F8^vii	54.44 (16)	F7—F6—F9	66.6 (2)
F5^vi—Cs1—F9	150.79 (15)	F7—F6—F9ⁱ	55.8 (2)
F8—Cs1—F8^vii	59.89 (16)	F7—F6—F10ⁱ	61.2 (2)
F8—Cs1—F9	53.97 (16)	F7ⁱⁱⁱ—F6—F9	57.5 (2)
F8^vii—Cs1—F9	111.41 (16)	F7ⁱⁱⁱ—F6—F9ⁱ	162.9 (3)
F1^vi—Cs2—F1^viii	75.84 (19)	F7ⁱⁱⁱ—F6—F10ⁱ	105.6 (2)
F1^vi—Cs2—F2^ix	81.94 (19)	F9—F6—F9ⁱ	117.5 (3)
F1^vi—Cs2—F3^vi	101.58 (17)	F9—F6—F10ⁱ	82.9 (3)
F1^vi—Cs2—F3ⁱⁱⁱ	150.6 (2)	F9ⁱ—F6—F10ⁱ	89.1 (3)
F1^vi—Cs2—F6^vi	53.32 (16)	Ce1—F7—Ce2ⁱ	120.3 (2)
F1^vi—Cs2—F7^vii	53.71 (18)	Ce1—F7—Cs2^vii	127.3 (2)
F1^vi—Cs2—F8	134.27 (19)	Ce1—F7—F1ⁱ	168.5 (3)
F1^vi—Cs2—F10^viii	101.15 (17)	Ce1—F7—F5ⁱ	52.49 (17)
F1^viii—Cs2—F2^ix	98.94 (19)	Ce1—F7—F6	55.10 (18)
F1^viii—Cs2—F3^vi	163.34 (19)	Ce1—F7—F6ⁱ	115.5 (2)
F1^viii—Cs2—F3ⁱⁱⁱ	130.44 (18)	Ce1—F7—F8	48.02 (18)
F1^viii—Cs2—F6^vi	126.19 (17)	Ce1—F7—F9	56.55 (18)
F1^viii—Cs2—F7^vii	83.52 (17)	Ce1—F7—F9ⁱ	71.7 (2)
F1^viii—Cs2—F8	70.68 (17)	Ce1—F7—F10ⁱ	112.1 (3)
F1^viii—Cs2—F10^viii	55.35 (17)	Ce2ⁱ—F7—Cs2^vii	100.6 (2)
F2^ix—Cs2—F3^vi	96.96 (17)	Ce2ⁱ—F7—F1ⁱ	48.22 (19)
F2^ix—Cs2—F3ⁱⁱⁱ	80.87 (18)	Ce2ⁱ—F7—F5ⁱ	106.3 (2)
F2^ix—Cs2—F6^vi	90.96 (18)	Ce2ⁱ—F7—F6	78.0 (2)
F2^ix—Cs2—F7^vii	133.81 (17)	Ce2ⁱ—F7—F6ⁱ	53.95 (18)
F2^ix—Cs2—F8	132.82 (18)	Ce2ⁱ—F7—F8	166.6 (3)
F2^ix—Cs2—F10^viii	54.94 (17)	Ce2ⁱ—F7—F9	123.4 (2)
F3^vi—Cs2—F3ⁱⁱⁱ	57.36 (16)	Ce2ⁱ—F7—F9ⁱ	55.52 (19)
F3^vi—Cs2—F6^vi	48.29 (14)	Ce2ⁱ—F7—F10ⁱ	52.62 (17)
F3^vi—Cs2—F7^vii	81.88 (15)	Cs2^vii—F7—F1ⁱ	60.53 (18)
F3^vi—Cs2—F8	101.76 (16)	Cs2^vii—F7—F5ⁱ	86.83 (19)
F3^vi—Cs2—F10^viii	140.30 (14)	Cs2^vii—F7—F6	177.4 (2)
F3ⁱⁱⁱ—Cs2—F6^vi	103.30 (16)	Cs2^vii—F7—F6ⁱ	62.65 (17)
F3ⁱⁱⁱ—Cs2—F7^vii	131.37 (16)	Cs2^vii—F7—F8	86.0 (2)
F3ⁱⁱⁱ—Cs2—F8	73.91 (18)	Cs2^vii—F7—F9	125.8 (2)
F3ⁱⁱⁱ—Cs2—F10^viii	88.18 (15)	Cs2^vii—F7—F9ⁱ	114.8 (2)
F6^vi—Cs2—F7^vii	54.18 (16)	Cs2^vii—F7—F10ⁱ	119.1 (2)
F6^vi—Cs2—F8	133.07 (17)	F1ⁱ—F7—F5ⁱ	125.1 (3)
F6^vi—Cs2—F10^viii	142.19 (16)	F1ⁱ—F7—F6	117.2 (3)
F7^vii—Cs2—F8	91.80 (17)	F1ⁱ—F7—F6ⁱ	58.5 (2)
F7^vii—Cs2—F10^viii	137.52 (13)	F1ⁱ—F7—F8	143.1 (3)
F8—Cs2—F10^viii	84.64 (17)	F1ⁱ—F7—F9	128.2 (3)
Ce2—F1—Cs1^xii	125.5 (3)	F1ⁱ—F7—F9ⁱ	97.6 (3)
Ce2—F1—Cs2^xiii	110.4 (2)	F1ⁱ—F7—F10ⁱ	63.3 (2)
Ce2—F1—Cs2ⁱⁱ	115.6 (3)	F5ⁱ—F7—F6	95.6 (2)
Ce2—F1—F4ⁱⁱ	54.7 (2)	F5ⁱ—F7—F6ⁱ	67.7 (2)
Ce2—F1—F6	57.14 (19)	F5ⁱ—F7—F8	62.1 (2)
Ce2—F1—F7ⁱⁱⁱ	54.6 (2)	F5ⁱ—F7—F9	106.6 (3)
Ce2—F1—F8ⁱⁱ	104.8 (3)	F5ⁱ—F7—F9ⁱ	55.3 (2)
Ce2—F1—F10	50.81 (19)	F5ⁱ—F7—F10ⁱ	147.2 (3)
Ce2—F1—F10ⁱ	45.99 (18)	F6—F7—F6ⁱ	117.6 (3)
Cs1^xii—F1—Cs2^xiii	101.4 (2)	F6—F7—F8	95.8 (3)
Cs1^xii—F1—Cs2ⁱⁱ	97.03 (18)	F6—F7—F9	54.2 (2)
Cs1^xii—F1—F4ⁱⁱ	87.6 (2)	F6—F7—F9ⁱ	66.3 (2)
Cs1^xii—F1—F6	102.2 (3)	F6—F7—F10ⁱ	58.4 (2)
Cs1^xii—F1—F7ⁱⁱⁱ	162.4 (3)	F6ⁱ—F7—F8	121.4 (2)
Cs1^xii—F1—F8ⁱⁱ	59.84 (16)	F6ⁱ—F7—F9	170.4 (3)
Cs1^xii—F1—F10	139.3 (3)	F6ⁱ—F7—F9ⁱ	54.7 (2)
Cs1^xii—F1—F10ⁱ	80.6 (2)	F6ⁱ—F7—F10ⁱ	104.9 (3)
Cs2^xiii—F1—Cs2ⁱⁱ	104.2 (2)	F8—F7—F9	58.6 (2)
Cs2^xiii—F1—F4ⁱⁱ	164.8 (3)	F8—F7—F9ⁱ	111.2 (3)
Cs2^xiii—F1—F6	65.71 (18)	F8—F7—F10ⁱ	133.7 (3)
Cs2^xiii—F1—F7ⁱⁱⁱ	65.76 (18)	F9—F7—F9ⁱ	115.8 (3)
Cs2^xiii—F1—F8ⁱⁱ	144.5 (3)	F9—F7—F10ⁱ	75.5 (2)
Cs2^xiii—F1—F10	118.0 (3)	F9ⁱ—F7—F10ⁱ	93.7 (2)
Cs2^xiii—F1—F10ⁱ	115.8 (2)	Ce1—F8—Cs1	117.9 (2)
Cs2ⁱⁱ—F1—F4ⁱⁱ	86.7 (2)	Ce1—F8—Cs1^vii	111.9 (2)
Cs2ⁱⁱ—F1—F6	159.7 (3)	Ce1—F8—Cs2	130.2 (3)
Cs2ⁱⁱ—F1—F7ⁱⁱⁱ	97.8 (3)	Ce1—F8—F1^viii	106.0 (2)
Cs2ⁱⁱ—F1—F8ⁱⁱ	54.42 (15)	Ce1—F8—F4	54.7 (2)
Cs2ⁱⁱ—F1—F10	65.24 (19)	Ce1—F8—F5	45.86 (17)
Cs2ⁱⁱ—F1—F10ⁱ	139.7 (2)	Ce1—F8—F5ⁱ	52.21 (18)
F4ⁱⁱ—F1—F6	100.5 (3)	Ce1—F8—F7	54.00 (19)
F4ⁱⁱ—F1—F7ⁱⁱⁱ	102.7 (3)	Ce1—F8—F8^vii	147.1 (3)
F4ⁱⁱ—F1—F8ⁱⁱ	50.8 (2)	Ce1—F8—F9	59.58 (19)
F4ⁱⁱ—F1—F10	56.7 (2)	Cs1—F8—Cs1^vii	120.1 (2)
F4ⁱⁱ—F1—F10ⁱ	53.06 (19)	Cs1—F8—Cs2	80.98 (17)
F6—F1—F7ⁱⁱⁱ	62.2 (2)	Cs1—F8—F1^viii	131.9 (2)
F6—F1—F8ⁱⁱ	143.1 (3)	Cs1—F8—F4	154.6 (3)
F6—F1—F10	102.9 (3)	Cs1—F8—F5	102.8 (2)
F6—F1—F10ⁱ	51.7 (2)	Cs1—F8—F5ⁱ	140.3 (3)
F7ⁱⁱⁱ—F1—F8ⁱⁱ	137.5 (3)	Cs1—F8—F7	83.54 (19)
F7ⁱⁱⁱ—F1—F10	56.8 (2)	Cs1—F8—F8^vii	61.99 (16)
F7ⁱⁱⁱ—F1—F10ⁱ	94.0 (3)	Cs1—F8—F9	60.92 (16)
F8ⁱⁱ—F1—F10	81.2 (2)	Cs1^vii—F8—Cs2	91.41 (16)
F8ⁱⁱ—F1—F10ⁱ	92.0 (2)	Cs1^vii—F8—F1^viii	51.88 (15)
F10—F1—F10ⁱ	90.4 (3)	Cs1^vii—F8—F4	82.68 (19)
Ce2—F2—Cs1	116.7 (2)	Cs1^vii—F8—F5	136.2 (2)
Ce2—F2—Cs1^v	125.0 (3)	Cs1^vii—F8—F5ⁱ	60.67 (16)
Ce2—F2—Cs2^xiv	114.7 (3)	Cs1^vii—F8—F7	101.4 (2)
Ce2—F2—F2^v	155.1 (3)	Cs1^vii—F8—F8^vii	58.11 (15)
Ce2—F2—F4ⁱⁱ	55.1 (2)	Cs1^vii—F8—F9	163.2 (3)
Ce2—F2—F6ⁱⁱⁱ	71.2 (2)	Cs2—F8—F1^viii	54.90 (16)
Ce2—F2—F9	55.89 (18)	Cs2—F8—F4	87.8 (2)
Ce2—F2—F10	47.28 (17)	Cs2—F8—F5	86.7 (2)
Ce2—F2—F10ⁱ	51.8 (2)	Cs2—F8—F5ⁱ	137.0 (2)
Cs1—F2—Cs1^v	111.7 (2)	Cs2—F8—F7	163.5 (3)
Cs1—F2—Cs2^xiv	95.48 (19)	Cs2—F8—F8^vii	82.6 (2)
Cs1—F2—F2^v	53.51 (14)	Cs2—F8—F9	105.1 (3)
Cs1—F2—F4ⁱⁱ	166.1 (3)	F1^viii—F8—F4	51.8 (2)
Cs1—F2—F6ⁱⁱⁱ	80.7 (2)	F1^viii—F8—F5	93.6 (2)
Cs1—F2—F9	60.88 (17)	F1^viii—F8—F5ⁱ	82.3 (2)
Cs1—F2—F10	130.2 (3)	F1^viii—F8—F7	141.6 (3)
Cs1—F2—F10ⁱ	109.3 (2)	F1^viii—F8—F8^vii	91.5 (2)
Cs1^v—F2—Cs2^xiv	84.12 (17)	F1^viii—F8—F9	141.9 (3)
Cs1^v—F2—F2^v	58.21 (15)	F4—F8—F5	53.57 (19)
Cs1^v—F2—F4ⁱⁱ	81.1 (2)	F4—F8—F5ⁱ	58.6 (2)
Cs1^v—F2—F6ⁱⁱⁱ	93.0 (2)	F4—F8—F7	104.0 (3)
Cs1^v—F2—F9	151.4 (3)	F4—F8—F8^vii	139.2 (3)
Cs1^v—F2—F10	81.74 (19)	F4—F8—F9	100.8 (3)
Cs1^v—F2—F10ⁱ	130.1 (3)	F5—F8—F5ⁱ	92.5 (2)
Cs2^xiv—F2—F2^v	89.9 (2)	F5—F8—F7	91.1 (2)
Cs2^xiv—F2—F4ⁱⁱ	80.1 (2)	F5—F8—F8^vii	162.5 (3)
Cs2^xiv—F2—F6ⁱⁱⁱ	174.1 (3)	F5—F8—F9	50.06 (18)
Cs2^xiv—F2—F9	122.9 (3)	F5ⁱ—F8—F7	59.4 (2)
Cs2^xiv—F2—F10	134.2 (3)	F5ⁱ—F8—F8^vii	104.8 (3)
Cs2^xiv—F2—F10ⁱ	64.7 (2)	F5ⁱ—F8—F9	106.9 (3)
F2^v—F2—F4ⁱⁱ	139.0 (3)	F7—F8—F8^vii	95.3 (3)
F2^v—F2—F6ⁱⁱⁱ	84.2 (2)	F7—F8—F9	61.7 (2)
F2^v—F2—F9	108.3 (3)	F8^vii—F8—F9	120.0 (2)
F2^v—F2—F10	117.8 (3)	Ce1—F9—Ce1ⁱⁱⁱ	103.6 (2)
F2^v—F2—F10ⁱ	149.3 (3)	Ce1—F9—Ce2	114.4 (3)
F4ⁱⁱ—F2—F6ⁱⁱⁱ	104.6 (3)	Ce1—F9—Cs1	110.27 (19)
F4ⁱⁱ—F2—F9	110.4 (3)	Ce1—F9—F2	139.8 (3)
F4ⁱⁱ—F2—F10	54.7 (2)	Ce1—F9—F3ⁱⁱⁱ	108.9 (2)
F4ⁱⁱ—F2—F10ⁱ	56.9 (2)	Ce1—F9—F5	53.54 (18)
F6ⁱⁱⁱ—F2—F9	59.1 (2)	Ce1—F9—F6	55.29 (17)
F6ⁱⁱⁱ—F2—F10	50.09 (19)	Ce1—F9—F6ⁱⁱⁱ	150.8 (3)
F6ⁱⁱⁱ—F2—F10ⁱ	120.8 (3)	Ce1—F9—F7	50.68 (16)
F9—F2—F10	84.2 (2)	Ce1—F9—F7ⁱⁱⁱ	101.9 (2)
F9—F2—F10ⁱ	75.3 (2)	Ce1—F9—F8	47.29 (17)
F10—F2—F10ⁱ	92.8 (2)	Ce1—F9—F10ⁱ	88.3 (2)
Ce1—F3—Cs1^xiii	110.3 (3)	Ce1ⁱⁱⁱ—F9—Ce2	100.8 (2)
Ce1—F3—Cs1ⁱ	124.6 (3)	Ce1ⁱⁱⁱ—F9—Cs1	109.0 (2)
Ce1—F3—Cs2^xiii	109.0 (2)	Ce1ⁱⁱⁱ—F9—F2	115.2 (3)
Ce1—F3—Cs2ⁱ	127.9 (2)	Ce1ⁱⁱⁱ—F9—F3ⁱⁱⁱ	43.46 (17)
Ce1—F3—F3^x	161.8 (3)	Ce1ⁱⁱⁱ—F9—F5	50.11 (18)
Ce1—F3—F4	54.6 (2)	Ce1ⁱⁱⁱ—F9—F6	108.1 (2)
Ce1—F3—F5	51.44 (19)	Ce1ⁱⁱⁱ—F9—F6ⁱⁱⁱ	47.52 (16)
Ce1—F3—F5ⁱ	47.28 (16)	Ce1ⁱⁱⁱ—F9—F7	154.3 (2)
Ce1—F3—F6	55.92 (18)	Ce1ⁱⁱⁱ—F9—F7ⁱⁱⁱ	49.44 (18)
Ce1—F3—F9ⁱ	68.3 (2)	Ce1ⁱⁱⁱ—F9—F8	105.5 (2)
Cs1^xiii—F3—Cs1ⁱ	122.4 (2)	Ce1ⁱⁱⁱ—F9—F10ⁱ	141.3 (2)
Cs1^xiii—F3—Cs2^xiii	72.60 (14)	Ce2—F9—Cs1	117.2 (2)
Cs1^xiii—F3—Cs2ⁱ	81.08 (15)	Ce2—F9—F2	49.88 (18)
Cs1^xiii—F3—F3^x	61.33 (18)	Ce2—F9—F3ⁱⁱⁱ	129.8 (3)
Cs1^xiii—F3—F4	77.1 (2)	Ce2—F9—F5	117.3 (3)
Cs1^xiii—F3—F5	61.03 (19)	Ce2—F9—F6	59.41 (18)
Cs1^xiii—F3—F5ⁱ	132.2 (2)	Ce2—F9—F6ⁱⁱⁱ	73.93 (19)
Cs1^xiii—F3—F6	114.8 (3)	Ce2—F9—F7	91.3 (2)
Cs1^xiii—F3—F9ⁱ	176.8 (2)	Ce2—F9—F7ⁱⁱⁱ	56.16 (18)
Cs1ⁱ—F3—Cs2^xiii	74.44 (13)	Ce2—F9—F8	150.9 (3)
Cs1ⁱ—F3—Cs2ⁱ	78.80 (16)	Ce2—F9—F10ⁱ	42.01 (14)
Cs1ⁱ—F3—F3^x	61.10 (18)	Cs1—F9—F2	67.43 (18)
Cs1ⁱ—F3—F4	149.1 (3)	Cs1—F9—F3ⁱⁱⁱ	66.80 (18)
Cs1ⁱ—F3—F5	151.4 (2)	Cs1—F9—F5	124.4 (3)
Cs1ⁱ—F3—F5ⁱ	99.7 (2)	Cs1—F9—F6	142.6 (3)
Cs1ⁱ—F3—F6	85.8 (2)	Cs1—F9—F6ⁱⁱⁱ	87.5 (2)
Cs1ⁱ—F3—F9ⁱ	58.10 (17)	Cs1—F9—F7	84.64 (19)
Cs2^xiii—F3—Cs2ⁱ	122.6 (2)	Cs1—F9—F7ⁱⁱⁱ	145.4 (3)
Cs2^xiii—F3—F3^x	53.91 (14)	Cs1—F9—F8	65.10 (17)
Cs2^xiii—F3—F4	136.5 (3)	Cs1—F9—F10ⁱ	100.6 (2)
Cs2^xiii—F3—F5	80.86 (19)	F2—F9—F3ⁱⁱⁱ	106.4 (3)
Cs2^xiii—F3—F5ⁱ	147.0 (2)	F2—F9—F5	161.8 (3)
Cs2^xiii—F3—F6	59.80 (17)	F2—F9—F6	100.7 (3)
Cs2^xiii—F3—F9ⁱ	104.9 (2)	F2—F9—F6ⁱⁱⁱ	67.9 (2)
Cs2ⁱ—F3—F3^x	68.73 (17)	F2—F9—F7	90.0 (3)
Cs2ⁱ—F3—F4	81.45 (19)	F2—F9—F7ⁱⁱⁱ	95.7 (3)
Cs2ⁱ—F3—F5	127.7 (2)	F2—F9—F8	124.9 (3)
Cs2ⁱ—F3—F5ⁱ	86.59 (18)	F2—F9—F10ⁱ	54.8 (2)
Cs2ⁱ—F3—F6	162.4 (3)	F3ⁱⁱⁱ—F9—F5	70.9 (2)
Cs2ⁱ—F3—F9ⁱ	102.1 (2)	F3ⁱⁱⁱ—F9—F6	147.4 (3)
F3^x—F3—F4	131.3 (3)	F3ⁱⁱⁱ—F9—F6ⁱⁱⁱ	55.9 (2)
F3^x—F3—F5	114.2 (3)	F3ⁱⁱⁱ—F9—F7	137.0 (3)
F3^x—F3—F5ⁱ	150.6 (3)	F3ⁱⁱⁱ—F9—F7ⁱⁱⁱ	91.5 (3)
F3^x—F3—F6	111.0 (2)	F3ⁱⁱⁱ—F9—F8	78.9 (2)
F3^x—F3—F9ⁱ	119.1 (3)	F3ⁱⁱⁱ—F9—F10ⁱ	161.2 (2)
F4—F3—F5	57.1 (2)	F5—F9—F6	77.7 (2)
F4—F3—F5ⁱ	55.4 (2)	F5—F9—F6ⁱⁱⁱ	97.4 (3)
F4—F3—F6	108.7 (3)	F5—F9—F7	104.2 (3)
F4—F3—F9ⁱ	103.9 (3)	F5—F9—F7ⁱⁱⁱ	66.7 (2)
F5—F3—F5ⁱ	93.2 (2)	F5—F9—F8	72.9 (2)
F5—F3—F6	69.3 (2)	F5—F9—F10ⁱ	127.3 (3)
F5—F3—F9ⁱ	116.8 (3)	F6—F9—F6ⁱⁱⁱ	122.1 (3)
F5ⁱ—F3—F6	87.7 (2)	F6—F9—F7	59.2 (2)
F5ⁱ—F3—F9ⁱ	49.21 (18)	F6—F9—F7ⁱⁱⁱ	67.8 (2)
F6—F3—F9ⁱ	62.0 (2)	F6—F9—F8	100.1 (3)
Ce1—F4—Ce2^viii	173.3 (4)	F6—F9—F10ⁱ	49.8 (2)
Ce1—F4—F1^viii	125.2 (4)	F6ⁱⁱⁱ—F9—F7	157.8 (3)
Ce1—F4—F2^viii	138.2 (4)	F6ⁱⁱⁱ—F9—F7ⁱⁱⁱ	58.0 (2)
Ce1—F4—F3	48.98 (18)	F6ⁱⁱⁱ—F9—F8	134.0 (3)
Ce1—F4—F5	53.23 (16)	F6ⁱⁱⁱ—F9—F10ⁱ	111.7 (2)
Ce1—F4—F5ⁱ	53.36 (16)	F7—F9—F7ⁱⁱⁱ	126.9 (3)
Ce1—F4—F8	48.67 (18)	F7—F9—F8	59.6 (2)
Ce1—F4—F10^xi	127.4 (3)	F7—F9—F10ⁱ	50.06 (18)
Ce1—F4—F10^viii	126.2 (2)	F7ⁱⁱⁱ—F9—F8	139.4 (3)
Ce2^viii—F4—F1^viii	48.04 (19)	F7ⁱⁱⁱ—F9—F10ⁱ	92.3 (2)
Ce2^viii—F4—F2^viii	48.52 (18)	F8—F9—F10ⁱ	109.4 (3)
Ce2^viii—F4—F3	137.6 (4)	Ce2—F10—Ce2ⁱⁱⁱ	138.6 (3)
Ce2^viii—F4—F5	128.2 (3)	Ce2—F10—Cs2ⁱⁱ	106.3 (2)
Ce2^viii—F4—F5ⁱ	124.8 (2)	Ce2—F10—F1	47.22 (17)
Ce2^viii—F4—F8	124.7 (4)	Ce2—F10—F1ⁱⁱⁱ	118.6 (3)
Ce2^viii—F4—F10^xi	53.56 (16)	Ce2—F10—F2	44.21 (16)
Ce2^viii—F4—F10^viii	52.57 (15)	Ce2—F10—F2ⁱⁱⁱ	142.4 (3)
F1^viii—F4—F2^viii	96.5 (2)	Ce2—F10—F4^xv	157.3 (3)
F1^viii—F4—F3	168.0 (3)	Ce2—F10—F4ⁱⁱ	55.57 (16)
F1^viii—F4—F5	123.7 (3)	Ce2—F10—F5ⁱⁱ	105.4 (2)
F1^viii—F4—F5ⁱ	98.5 (3)	Ce2—F10—F6ⁱⁱⁱ	80.6 (2)
F1^viii—F4—F8	77.4 (3)	Ce2—F10—F7ⁱⁱⁱ	55.37 (17)
F1^viii—F4—F10^xi	70.8 (2)	Ce2—F10—F9ⁱⁱⁱ	106.3 (2)
F1^viii—F4—F10^viii	63.1 (3)	Ce2ⁱⁱⁱ—F10—Cs2ⁱⁱ	106.1 (2)
F2^viii—F4—F3	90.3 (3)	Ce2ⁱⁱⁱ—F10—F1	147.4 (3)
F2^viii—F4—F5	104.6 (3)	Ce2ⁱⁱⁱ—F10—F1ⁱⁱⁱ	42.08 (17)
F2^viii—F4—F5ⁱ	128.9 (3)	Ce2ⁱⁱⁱ—F10—F2	113.0 (3)
F2^viii—F4—F8	167.5 (3)	Ce2ⁱⁱⁱ—F10—F2ⁱⁱⁱ	47.22 (18)
F2^viii—F4—F10^xi	63.5 (2)	Ce2ⁱⁱⁱ—F10—F4^xv	55.32 (16)
F2^viii—F4—F10^viii	68.1 (2)	Ce2ⁱⁱⁱ—F10—F4ⁱⁱ	152.2 (3)
F3—F4—F5	63.3 (2)	Ce2ⁱⁱⁱ—F10—F5ⁱⁱ	104.9 (2)
F3—F4—F5ⁱ	69.6 (2)	Ce2ⁱⁱⁱ—F10—F6ⁱⁱⁱ	58.2 (2)
F3—F4—F8	97.6 (2)	Ce2ⁱⁱⁱ—F10—F7ⁱⁱⁱ	96.2 (2)
F3—F4—F10^xi	103.9 (3)	Ce2ⁱⁱⁱ—F10—F9ⁱⁱⁱ	42.60 (14)
F3—F4—F10^viii	128.8 (3)	Cs2ⁱⁱ—F10—F1	59.42 (18)
F5—F4—F5ⁱ	106.6 (2)	Cs2ⁱⁱ—F10—F1ⁱⁱⁱ	134.3 (2)
F5—F4—F8	70.8 (2)	Cs2ⁱⁱ—F10—F2	140.5 (3)
F5—F4—F10^xi	163.6 (4)	Cs2ⁱⁱ—F10—F2ⁱⁱⁱ	60.40 (18)
F5—F4—F10^viii	77.6 (2)	Cs2ⁱⁱ—F10—F4^xv	79.2 (2)
F5ⁱ—F4—F8	63.3 (2)	Cs2ⁱⁱ—F10—F4ⁱⁱ	85.3 (2)
F5ⁱ—F4—F10^xi	76.2 (2)	Cs2ⁱⁱ—F10—F5ⁱⁱ	80.24 (16)
F5ⁱ—F4—F10^viii	158.1 (4)	Cs2ⁱⁱ—F10—F6ⁱⁱⁱ	146.5 (3)
F8—F4—F10^xi	123.2 (3)	Cs2ⁱⁱ—F10—F7ⁱⁱⁱ	96.0 (2)
F8—F4—F10^viii	99.3 (3)	Cs2ⁱⁱ—F10—F9ⁱⁱⁱ	100.21 (19)
F10^xi—F4—F10^viii	106.1 (2)	F1—F10—F1ⁱⁱⁱ	165.7 (3)
Ce1—F5—Ce1ⁱⁱⁱ	135.5 (3)	F1—F10—F2	88.8 (2)
Ce1—F5—Cs1^xiii	111.0 (2)	F1—F10—F2ⁱⁱⁱ	106.5 (3)
Ce1—F5—F3	47.69 (18)	F1—F10—F4^xv	135.6 (3)
Ce1—F5—F3ⁱⁱⁱ	106.9 (2)	F1—F10—F4ⁱⁱ	60.2 (2)
Ce1—F5—F4	54.91 (17)	F1—F10—F5ⁱⁱ	101.2 (2)
Ce1—F5—F4ⁱⁱⁱ	146.6 (3)	F1—F10—F6ⁱⁱⁱ	116.1 (2)
Ce1—F5—F6	47.24 (15)	F1—F10—F7ⁱⁱⁱ	59.9 (2)
Ce1—F5—F7ⁱⁱⁱ	101.7 (2)	F1—F10—F9ⁱⁱⁱ	107.6 (2)
Ce1—F5—F8	42.39 (17)	F1ⁱⁱⁱ—F10—F2	77.1 (2)
Ce1—F5—F8ⁱⁱⁱ	155.2 (3)	F1ⁱⁱⁱ—F10—F2ⁱⁱⁱ	86.6 (2)
Ce1—F5—F9	62.5 (2)	F1ⁱⁱⁱ—F10—F4^xv	56.2 (2)
Ce1—F5—F10^viii	103.2 (2)	F1ⁱⁱⁱ—F10—F4ⁱⁱ	112.4 (3)
Ce1ⁱⁱⁱ—F5—Cs1^xiii	110.3 (2)	F1ⁱⁱⁱ—F10—F5ⁱⁱ	80.1 (2)
Ce1ⁱⁱⁱ—F5—F3	150.7 (3)	F1ⁱⁱⁱ—F10—F6ⁱⁱⁱ	55.9 (2)
Ce1ⁱⁱⁱ—F5—F3ⁱⁱⁱ	42.70 (15)	F1ⁱⁱⁱ—F10—F7ⁱⁱⁱ	115.7 (3)
Ce1ⁱⁱⁱ—F5—F4	149.7 (3)	F1ⁱⁱⁱ—F10—F9ⁱⁱⁱ	76.1 (2)
Ce1ⁱⁱⁱ—F5—F4ⁱⁱⁱ	53.13 (16)	F2—F10—F2ⁱⁱⁱ	159.0 (3)
Ce1ⁱⁱⁱ—F5—F6	105.16 (19)	F2—F10—F4^xv	118.6 (3)
Ce1ⁱⁱⁱ—F5—F7ⁱⁱⁱ	52.32 (16)	F2—F10—F4ⁱⁱ	57.1 (2)
Ce1ⁱⁱⁱ—F5—F8	110.0 (2)	F2—F10—F5ⁱⁱ	84.2 (2)
Ce1ⁱⁱⁱ—F5—F8ⁱⁱⁱ	46.43 (17)	F2—F10—F6ⁱⁱⁱ	66.1 (2)
Ce1ⁱⁱⁱ—F5—F9	73.1 (2)	F2—F10—F7ⁱⁱⁱ	85.8 (2)
Ce1ⁱⁱⁱ—F5—F10^viii	102.6 (2)	F2—F10—F9ⁱⁱⁱ	112.3 (2)
Cs1^xiii—F5—F3	65.45 (18)	F2ⁱⁱⁱ—F10—F4^xv	59.6 (2)
Cs1^xiii—F5—F3ⁱⁱⁱ	139.2 (3)	F2ⁱⁱⁱ—F10—F4ⁱⁱ	143.2 (3)
Cs1^xiii—F5—F4	80.3 (2)	F2ⁱⁱⁱ—F10—F5ⁱⁱ	106.2 (2)
Cs1^xiii—F5—F4ⁱⁱⁱ	84.7 (2)	F2ⁱⁱⁱ—F10—F6ⁱⁱⁱ	93.8 (3)
Cs1^xiii—F5—F6	106.0 (2)	F2ⁱⁱⁱ—F10—F7ⁱⁱⁱ	89.5 (3)
Cs1^xiii—F5—F7ⁱⁱⁱ	103.7 (2)	F2ⁱⁱⁱ—F10—F9ⁱⁱⁱ	49.86 (18)
Cs1^xiii—F5—F8	135.8 (2)	F4^xv—F10—F4ⁱⁱ	104.0 (2)
Cs1^xiii—F5—F8ⁱⁱⁱ	64.89 (17)	F4^xv—F10—F5ⁱⁱ	53.02 (19)
Cs1^xiii—F5—F9	155.3 (3)	F4^xv—F10—F6ⁱⁱⁱ	107.2 (3)
Cs1^xiii—F5—F10^viii	75.28 (16)	F4^xv—F10—F7ⁱⁱⁱ	147.1 (3)
F3—F5—F3ⁱⁱⁱ	154.5 (3)	F4^xv—F10—F9ⁱⁱⁱ	94.1 (2)
F3—F5—F4	59.6 (2)	F4ⁱⁱ—F10—F5ⁱⁱ	51.12 (17)
F3—F5—F4ⁱⁱⁱ	146.3 (3)	F4ⁱⁱ—F10—F6ⁱⁱⁱ	122.9 (3)
F3—F5—F6	53.13 (19)	F4ⁱⁱ—F10—F7ⁱⁱⁱ	108.0 (2)
F3—F5—F7ⁱⁱⁱ	99.3 (2)	F4ⁱⁱ—F10—F9ⁱⁱⁱ	161.8 (2)
F3—F5—F8	87.2 (2)	F5ⁱⁱ—F10—F6ⁱⁱⁱ	130.4 (3)
F3—F5—F8ⁱⁱⁱ	116.3 (3)	F5ⁱⁱ—F10—F7ⁱⁱⁱ	158.8 (3)
F3—F5—F9	99.2 (3)	F5ⁱⁱ—F10—F9ⁱⁱⁱ	146.7 (2)
F3—F5—F10^viii	104.0 (2)	F6ⁱⁱⁱ—F10—F7ⁱⁱⁱ	60.4 (2)
F3ⁱⁱⁱ—F5—F4	111.0 (3)	F6ⁱⁱⁱ—F10—F9ⁱⁱⁱ	47.38 (19)
F3ⁱⁱⁱ—F5—F4ⁱⁱⁱ	55.0 (2)	F7ⁱⁱⁱ—F10—F9ⁱⁱⁱ	54.4 (2)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x+1, −y+3/2, z+1/2; (iii) x, −y+3/2, z+1/2; (iv) −x+2, y−1/2, −z+1/2; (v) −x+2, −y+1, −z+1; (vi) −x+1, y−1/2, −z+1/2; (vii) −x+1, −y+1, −z; (viii) x−1, −y+3/2, z−1/2; (ix) x−1, y, z; (x) −x+1, −y+2, −z; (xi) x−1, y, z−1; (xii) −x+2, y+1/2, −z+1/2; (xiii) −x+1, y+1/2, −z+1/2; (xiv) x+1, y, z; (xv) x+1, y, z+1.

Selected bond lengths (Å) top

Ce1—F3	2.133 (6)	Cs1—F2	3.152 (6)
Ce1—F4	2.304 (5)	Cs1—F2^v	2.982 (6)
Ce1—F5	2.256 (6)	Cs1—F3^vi	3.222 (7)
Ce1—F5ⁱ	2.311 (6)	Cs1—F3ⁱⁱⁱ	3.229 (7)
Ce1—F6	2.320 (5)	Cs1—F5^vi	3.099 (6)
Ce1—F7	2.306 (6)	Cs1—F8	3.095 (6)
Ce1—F8	2.119 (7)	Cs1—F8^vii	3.218 (6)
Ce1—F9	2.487 (6)	Cs1—F9	2.982 (5)
Ce2—F1	2.123 (7)	Cs2—F1^vi	2.998 (6)
Ce2—F2	2.128 (7)	Cs2—F1^viii	2.998 (7)
Ce2—F4ⁱⁱ	2.329 (5)	Cs2—F2^ix	3.042 (8)
Ce2—F6	2.395 (6)	Cs2—F3^vi	3.437 (6)
Ce2—F7ⁱⁱⁱ	2.322 (6)	Cs2—F3ⁱⁱⁱ	2.981 (6)
Ce2—F9	2.304 (6)	Cs2—F6^vi	3.125 (6)
Ce2—F10	2.242 (5)	Cs2—F7^vii	3.140 (6)
Ce2—F10ⁱ	2.279 (6)	Cs2—F8	2.980 (7)
Cs1—F1^iv	2.928 (8)	Cs2—F10^viii	3.162 (6)

Acknowledgements

We thank Karen Friese for discussions. We also acknowledge the National Science Foundation grant No. DMR-0907359 for financial support.

References

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Volume 70| Part 3| March 2014| Pages i12-i13

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