C2-isomer of [Pd(tfd)]6 [tfd is S2C2(CF3)2] as its benzene solvate: a new member of the small but growing class of homoleptic palladium(II) monodi-thio-lenes in the form of hexa-meric cubes.

The title compound, hexa-kis-[μ3-1,2-bis-(tri-fluoro-meth-yl)ethene-1,2-di-thiol-ato]-octa-hedro-hexa-palladium(II), [Pd(C4F6S2)]6, crystallizes as its benzene solvate, [Pd(tfd)]6·2.5C6H6, where tfd is the di-thiol-ene S2C2(CF3)2. The mol-ecular structure of [Pd(tfd)]6 is of the hexa-metallic cube type seen previously in three examples of hexa-meric homoleptic palladium monodi-thiol-ene structures. All structures have in common: (a) the cluster closely approximates a cube containing six PdII atoms, one at the centre of each cube face; (b) 12 S atoms occupy the mid-points of all 12 cube edges, providing for each PdII atom an approximately square-planar S4 environment; (c) each S atom is part of a di-thiol-ene mol-ecule, where the size of the di-thiol-ene ligand necessitates that only sulfur atoms on adjacent cube edges can be part of the same di-thiol-ene. This general cube-type framework has so far given rise to two isomeric types: an S6-symmetric isomer and a C2-chiral type (two isomers that are enanti-omers of each other). The structure of [Pd(tfd)]6 is of the C2-type. Out of the 12 CF3 groups, three are rotationally disordered over two positions. Further, we answer the question of whether additional, previously undiscovered, isomers could follow from the cube rules (a) through (c) above. An exhaustive analysis shows that no additional isomers are possible and that the list of isomers (one S6 isomer, two C2 enanti-omers) is complete. Each isomer type could give rise to an unlimited number of compounds if the specific di-thiol-ene used is varied.

Chemical context

Metal–di­thiol­ene complexes (di­thiol­ene = S2C2 R 2) are relevant for a host of new materials and several metalloenzymes (Stiefel, 2004 ▸; Harrison et al., 2006 ▸). Homoleptic complexes normally contain two or three di­thiol­enes per metal, for bis­dithiol­enes M(di­thiol­ene)2 or tris­dithiol­enes M(di­thiol­ene)3. Monomeric homoleptic monodi­thiol­enes of the composition M(di­thiol­ene)1 are unstable and polymerize or oligomerize. A dimeric complex [Ni(S2C2(CF3)2)]2 was recently computed (Dang et al., 2013 ▸). The class of hexa­meric homoleptic palladium monodi­thiol­enes [Pd(di­thiol­ene)]6, where di­thiol­ene = R 2C2S2 with any substituent R was suggested by Stiefel and co-workers (Beswick et al., 2002 ▸), and a charge-neutral hexa­nuclear complex was crystallographically characterized (as its toluene solvate) using the di­thiol­ene S2C2(COOMe)2. The partially reduced complex, with a tetra­phenyl­phospho­nium counter-ion, was later structurally characterized by Stibrany (2012 ▸). A charge-neutral complex Pd(di­thiol­ene)6 with the di­thiol­ene S2C6H2(OMe)2 was reported by Rawson and co-workers (Wrixon et al., 2015 ▸). In this work, we generated [Pd(tfd)]6 [where tfd is the di­thiol­ene S2C2(CF3)2] from tfd and the di­benzyl­ideneacetone (dba) complex Pd2dba3 as described below. A crystal was obtained, and the structure was determined by X-ray crystallography.

Structural commentary

The molecular structure of [Pd(tfd)]6 is shown in Fig. 1 ▸, where the second position for the rotationally disordered tri­fluoro­methyl groups (attached to C1, C13, and C14), the second position for disordered atom C15, as well as the benzene solvate mol­ecules are not displayed. The structure has approximate, non-crystallographic, C 2 symmetry (C 2 through Pd2 and Pd4). The gross features of this cube-like structure will be discussed first, followed by details such as bond lengths. The structure is of the hexa­metallic cube type seen previously in the hexa­meric homoleptic palladium monodi­thiol­enes characterized by Stiefel and co-workers (Beswick et al., 2002 ▸), Stibrany (Stibrany, 2012 ▸), and Rawson and co-workers (Wrixon et al. 2015 ▸). All structures have in common: (a) the cluster closely approximates a cube containing six PdII atoms, one at the centre of each cube face; (b) 12 S atoms occupy the midpoint of all 12 cube edges, providing for each PdII atom an approximately square-planar S 4 environment; (c) each S atom is part of a di­thiol­ene mol­ecule, where the size of the di­thiol­ene ligand requires that only sulfurs on adjacent cube edges can be part of the same di­thiol­ene. This general cube-type framework has so far given rise to two isomer types: one S 6-symmetric isomer seen for the charge-neutral palladium complex of S2C2(COOMe)2 (Beswick et al., 2002 ▸) and for a partially reduced complex involving the same ligand (Stibrany, 2012 ▸). The charge-neutral complex Pd(di­thiol­ene)6 with the di­thiol­ene S2C6H2(OMe)2 was found by Rawson and co-workers (Wrixon et al., 2015 ▸) to have a different, C 2-symmetric, structure. The two isomeric types are shown here schematically, inscribed into a cube (Fig. 2 ▸).

Figure 1

A view of the mol­ecular structure of [Pd(tfd)]6. Anisotropic displacement ellipsoids are shown at the 30% probability level. The ligand backbones are highlighted.

Figure 2

Isomers for [Pd(di­thiol­ene)]6.

The question of whether additional isomers are possible remained open and is answered here (Figs. 3 ▸ and 4 ▸). The starting point is the constraint that 12 donor atoms (such as sulfur) reside at the midpoint of the 12 cube edges and that metal atoms (such as Pd) occupy the centres of all cube faces. The ligand length constraint forbids trans-spanning placement of a chelate bridge, and chelates can only bridge the short distance between adjacent edge positions. All possible isomers following from this framework are explored in an exhaustive fashion (Figs. 3 ▸ and 4 ▸), following the initially arbitrary placement of the first bridge. It results that no additional isomers are possible and that the list of isomers (one S 6 isomer, two C 2 enanti­omers) is complete. It is worthwhile noting that the S 6 isomer cannot have a dipole moment, by virtue of its inversion centre, while the C 2 isomer has a dipole.

Figure 3

Graphical proof that only one S 6 isomer and two (enanti­omeric) C 2 isomers are possible for homoleptic palladium monodi­thiol­enes in the form of hexa­meric cubes, given the ‘cube rules’ discussed in the text. Continues in Fig. 4 ▸.

Figure 4

Continued from Fig. 3 ▸.

With these general results for homoleptic square-planar metal-based short-span chelates in the fom of hexa­meric cubes [M(L 2)]6 in hand, we return to discussing the details of the structure of [Pd(tfd)]6 (Fig. 1 ▸). It is notable that not all Pd—S distances are the same. Shorter distances, on average 2.294 Å (12 values; standard deviation = 0.008 Å), are found for the Pd—S distances within an approximately planar C2S2Pd five-membered ring. Longer distances, on average 2.364 Å (12 values; standard deviation = 0.01 Å) are found for coordination of an S atom outside its own C2S2Pd ring onto a different PdII atom at an approximately right angle to the five-membered ring. All bonds to Pd2, the Pd atom at the bottom of the Pd5(tfd)4 C 4-symmetric ‘box’ (Fig. 2 ▸) are long. All bonds to Pd4, the PdII atom in the Pd(tfd)2 ‘lid’ are short. The charge on the tfd ligand can be seen from the C—C distance within the chelate ring, which is short (double bond) for the dianion (ene-di­thiol­ate; C—C distance of 1.35 Å or shorter expected) and long for monoanionic tfd (C—C bond order = 1.5; C—C distance of 1.38 Å expected), as is known from Tang et al. (2009 ▸) and Kogut et al. (2006 ▸) (see analysis in Hosking et al., 2009 ▸). The chelate C—C bond distances in the current structure of [Pd(tfd)]6 average to 1.339 Å (six values; standard deviation = 0.006 Å) and indicate a dianionic chelate. Charge balance necessitates that all palladium atoms are in the oxidation state 2+, which is also supported by the coordination geometry around each PdII atom, which is approximately square-planar, as expected for a d 8 metal centre. The structure may thus be described as a charge-neutral C 4-symmetric Pd4(di­thiol­ene)4 tiara capped on one side with a Pd2+ dication and on the other side with a Pd(tfd)2 2− dianion. While the structure is likely more charge balanced than this zwitterionic description implies, this description suggests a direction of the dipole moment.

Supra­molecular features

Mol­ecules of [Pd(tfd)]6 and benzene solvate mol­ecules pack via contacting van der Waals surfaces. There are no particularly short inter­molecular distances (such as hydrogen bonds).

Database survey

The three structures discussed (EGIDIH: Beswick et al., 2002 ▸; XARMOU: Stibrany, 2012 ▸; YUQHUP: Wrixon et al., 2015 ▸) are the only structures for hexa­metallic compounds of the type [Pd(di­thiol­ene)]6 in CSD (Groom et al., 2016 ▸), Version 5.38 including updates up to Feb 2017.

Synthesis and crystallization

General specifications: All manipulations were carried out under an inert (N2) atmosphere using standard glove box (M. Braun UniLab) and Schlenk techniques. NMR solvents were obtained from Cambridge Isotope Laboratories. Solvents were purified prior to use by vacuum distillation from purple sodium benzo­phenone ketyl. NMR data were obtained on a Bruker Avance III 400 MHz spectrometer. Pd2dba3 was obtained from Sigma–Aldrich. S2C2(CF3)2 (tfd) was synthesized as in Harrison et al. (2006 ▸).

Synthesis: A pyrex reaction vessel containing 10 ml of toluene, 80 mg of Pd2dba3 (175 µmol of Pd) and 80 µl (350 µmol) of tfd was heated to 353 K overnight. At the end of the reaction, the dark-red solution had turned an intense brown. Solvent and volatiles were removed under vacuum at room temperature, followed by heating to 383 K for 4 h, also under vacuum. NMR spectroscopy (C6D6 solvent) showed a complex mixture, as indicated by multiple 19F resonances, chiefly two intense quartets (J F–F = 14.5 Hz) at −58.7 ppm and −59.3 ppm but also a large number of overlapping signals between −56 and −58 ppm. C 2-[Pd(tfd)]6 is clearly not the only species in solution, as it would give rise to six distinct fluorine signals (quartets) in equal intensity. It seems likely that multiple species are in equilibrium in the reaction mixture, and C 2-[Pd(tfd)]6 might crystallize from non-polar solvents relatively early due to its dipole moment, which makes it less soluble in non-polar solvents compared to non-polar species. Dissolving the sample in a minimal amount of benzene, followed by storage at 285 K for one week, led to the formation of crystals suitable for X-ray crystallography.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1 ▸. The F atoms of three of the –CF3 groups were refined as disordered over two sets of sites with the ratios of refined occupancies being 0.898 (6):0.102 (6) for F1/F2/F3, 0.784 (7):0.216 (7) for F19/F20/F21 and 0.749 (9):0.251 (9) for F22/F23/F24. Both the major and minor components were refined with anisotropic displacement parameters. In the –CF3 group containing F19/F20/F21, the attached atom C15 was also refined over two sets of sites with occupancies of 0.784 (7) and 0.216 (7). The SIMU command in SHELXL (Sheldrick, 2015 ▸) was used to restrain the anisotropic displacement parameters of the disordered atoms. The asymmetric unit contains 2.5 benzene solvent mol­ecules. One benzene mol­ecule is disordered about an inversion centre and hence has 0.5 occupancy. The RIGU command in SHELXL was used to restrain the anisotropic displacement parameters of the 0.5 occupancy benzene mol­ecule. The H atoms bonded to C atoms were placed in calculated positions C—H = 0.95 Å) and included in the refinement in a riding-motion approximation with U iso(H) = 1.2U eq(C).

Table 1

Experimental details

Crystal data
Chemical formula	[Pd6(C4F6S2)6]·2.5C6H6
M r	2190.63
Crystal system, space group	Monoclinic, P21/n
Temperature (K)	147
a, b, c (Å)	15.6367 (15), 17.8970 (17), 22.532 (2)
β (°)	104.502 (2)
V (Å3)	6104.6 (10)
Z	4
Radiation type	Mo Kα
μ (mm−1)	2.28
Crystal size (mm)	0.26 × 0.18 × 0.12
Data collection
Diffractometer	Bruker Kappa APEX DUO CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2014 ▸)
T min, T max	0.615, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	52442, 13977, 10755
R int	0.035
(sin θ/λ)max (Å−1)	0.651
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S	0.040, 0.091, 1.11
No. of reflections	13977
No. of parameters	955
No. of restraints	390
H-atom treatment	H-atom parameters constrained
	w = 1/[σ2(F o 2) + (0.016P)2 + 46.8497P] where P = (F o 2 + 2F c 2)/3
Δρmax, Δρmin (e Å−3)	2.95, −1.37

Computer programs: APEX2 and SAINT (Bruker, 2014 ▸), SHELXS97 and SHELXTL (Sheldrick, 2008 ▸), SHELXL2014 (Sheldrick, 2015 ▸) and ORTEP-3 for Windows (Farrugia, 2012 ▸).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989017007897/zl2703sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989017007897/zl2703Isup2.hkl

CCDC reference: 1552666

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

[Pd6(C4F6S2)6]·2.5C6H6	F(000) = 4164
Mr = 2190.63	Dx = 2.384 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 15.6367 (15) Å	Cell parameters from 9843 reflections
b = 17.8970 (17) Å	θ = 2.6–27.5°
c = 22.532 (2) Å	µ = 2.28 mm−1
β = 104.502 (2)°	T = 147 K
V = 6104.6 (10) Å3	Plate, bronze
Z = 4	0.26 × 0.18 × 0.12 mm

Bruker Kappa APEX DUO CCD diffractometer	10755 reflections with I > 2σ(I)
Radiation source: sealed tube with Bruker Triumph monochromator	Rint = 0.035
φ and ω scans	θmax = 27.6°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Bruker, 2014)	h = −20→20
Tmin = 0.615, Tmax = 0.746	k = −23→13
52442 measured reflections	l = −24→29
13977 independent reflections

Refinement on F2	390 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040	H-atom parameters constrained
wR(F2) = 0.091	w = 1/[σ2(Fo2) + (0.016P)2 + 46.8497P] where P = (Fo2 + 2Fc2)/3
S = 1.11	(Δ/σ)max = 0.002
13977 reflections	Δρmax = 2.95 e Å−3
955 parameters	Δρmin = −1.37 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pd1	0.85082 (2)	0.76886 (2)	0.12870 (2)	0.01462 (8)
Pd2	0.69610 (3)	0.86599 (2)	0.02884 (2)	0.01675 (9)
Pd3	0.88930 (3)	0.84026 (2)	−0.00212 (2)	0.01563 (8)
Pd4	0.86910 (3)	0.65611 (2)	0.01559 (2)	0.01621 (8)
Pd5	0.67829 (2)	0.68175 (2)	0.04773 (2)	0.01439 (8)
Pd6	0.71858 (3)	0.75118 (2)	−0.08355 (2)	0.01713 (9)
S1	0.77482 (8)	0.87687 (7)	0.13250 (6)	0.0170 (2)
S2	0.95772 (8)	0.84289 (7)	0.10438 (6)	0.0167 (2)
S3	0.93246 (8)	0.65959 (7)	0.11965 (6)	0.0167 (2)
S4	0.74009 (8)	0.69237 (7)	0.15081 (5)	0.0149 (2)
S5	0.80145 (9)	0.94209 (7)	−0.00043 (6)	0.0195 (3)
S6	0.97628 (8)	0.73296 (7)	−0.00334 (6)	0.0180 (3)
S7	0.76397 (8)	0.57656 (7)	0.03498 (6)	0.0168 (2)
S8	0.59617 (8)	0.78441 (7)	0.05793 (6)	0.0163 (2)
S9	0.62407 (8)	0.84575 (7)	−0.07509 (6)	0.0192 (3)
S10	0.82459 (8)	0.83395 (7)	−0.10505 (6)	0.0180 (3)
S11	0.81170 (9)	0.64732 (7)	−0.08874 (6)	0.0202 (3)
S12	0.61665 (9)	0.67151 (7)	−0.05945 (6)	0.0184 (3)
F1	0.8470 (4)	1.0803 (2)	0.1229 (3)	0.0534 (15)	0.898 (6)
F2	0.8460 (5)	1.0370 (3)	0.2113 (2)	0.0607 (16)	0.898 (6)
F3	0.7328 (3)	1.0268 (2)	0.1361 (3)	0.0514 (14)	0.898 (6)
F1A	0.773 (3)	1.056 (2)	0.108 (2)	0.053 (6)	0.102 (6)
F2A	0.895 (3)	1.073 (2)	0.173 (2)	0.048 (6)	0.102 (6)
F3A	0.787 (3)	1.019 (2)	0.196 (2)	0.044 (6)	0.102 (6)
F4	1.0151 (3)	1.0393 (2)	0.1694 (2)	0.0555 (12)
F5	1.0809 (3)	0.9587 (2)	0.1285 (2)	0.0561 (12)
F6	0.9840 (3)	1.0317 (2)	0.07257 (19)	0.0524 (11)
F7	0.9602 (3)	0.6236 (2)	0.24481 (16)	0.0412 (9)
F8	0.9826 (3)	0.5113 (2)	0.21972 (18)	0.0456 (10)
F9	0.8612 (3)	0.5410 (2)	0.24268 (16)	0.0400 (9)
F10	0.8314 (3)	0.4306 (2)	0.16301 (18)	0.0415 (9)
F11	0.7340 (3)	0.4355 (2)	0.07866 (18)	0.0469 (10)
F12	0.7111 (3)	0.4900 (2)	0.1581 (2)	0.0499 (11)
F13	0.6177 (3)	0.7686 (3)	0.26571 (18)	0.0595 (13)
F14	0.7290 (4)	0.6985 (3)	0.27256 (17)	0.0662 (15)
F15	0.7436 (3)	0.8158 (2)	0.26936 (16)	0.0475 (10)
F16	0.4784 (3)	0.8280 (2)	0.1618 (2)	0.0564 (12)
F17	0.5903 (3)	0.8950 (3)	0.2033 (2)	0.0617 (13)
F18	0.5304 (3)	0.9068 (2)	0.10894 (19)	0.0540 (12)
C13	0.7558 (9)	0.9641 (5)	−0.0788 (7)	0.0252 (15)	0.784 (7)
C15	0.7020 (6)	1.0358 (5)	−0.0888 (4)	0.0387 (18)	0.784 (7)
F19	0.7489 (4)	1.0925 (3)	−0.0989 (4)	0.066 (2)	0.784 (7)
F20	0.6305 (4)	1.0310 (3)	−0.1355 (3)	0.0591 (18)	0.784 (7)
F21	0.6704 (4)	1.0510 (3)	−0.0405 (3)	0.0520 (16)	0.784 (7)
C13A	0.757 (4)	0.9666 (17)	−0.079 (3)	0.032 (4)	0.216 (7)
C15A	0.7193 (15)	1.0451 (13)	−0.0853 (11)	0.041 (3)	0.216 (7)
F19A	0.7626 (14)	1.0918 (11)	−0.0445 (10)	0.065 (5)	0.216 (7)
F20A	0.7169 (16)	1.0759 (12)	−0.1394 (9)	0.057 (5)	0.216 (7)
F21A	0.6353 (13)	1.0436 (12)	−0.0823 (12)	0.061 (5)	0.216 (7)
F22	0.7870 (5)	0.8980 (4)	−0.2219 (2)	0.060 (2)	0.749 (9)
F23	0.6536 (4)	0.9084 (5)	−0.2135 (3)	0.058 (2)	0.749 (9)
F24	0.7377 (5)	1.0031 (4)	−0.2071 (3)	0.0483 (17)	0.749 (9)
F22A	0.7728 (14)	0.9736 (13)	−0.2162 (9)	0.049 (4)	0.251 (9)
F23A	0.7155 (15)	0.8665 (11)	−0.2199 (8)	0.056 (4)	0.251 (9)
F24A	0.6466 (13)	0.9614 (14)	−0.2020 (9)	0.059 (5)	0.251 (9)
F25	1.0181 (3)	0.7861 (2)	−0.15739 (17)	0.0396 (9)
F26	1.0830 (3)	0.8072 (2)	−0.06401 (18)	0.0429 (10)
F27	1.1060 (2)	0.7041 (2)	−0.10540 (18)	0.0407 (9)
F28	0.9689 (3)	0.6493 (2)	−0.19661 (17)	0.0453 (10)
F29	0.8409 (3)	0.6047 (2)	−0.20204 (18)	0.0525 (12)
F30	0.8545 (3)	0.7203 (2)	−0.22092 (16)	0.0479 (11)
F31	0.3878 (3)	0.8338 (3)	−0.0521 (2)	0.0592 (13)
F32	0.4726 (3)	0.9211 (3)	−0.0621 (3)	0.0756 (17)
F33	0.4036 (3)	0.8610 (3)	−0.1401 (2)	0.083 (2)
F34	0.4510 (3)	0.6093 (2)	−0.0710 (2)	0.0506 (11)
F35	0.4151 (3)	0.6926 (3)	−0.01466 (18)	0.0495 (11)
F36	0.3690 (2)	0.6994 (2)	−0.11211 (17)	0.0460 (10)
C1	0.8539 (4)	0.9489 (3)	0.1357 (3)	0.0231 (11)
C2	0.9320 (4)	0.9340 (3)	0.1246 (2)	0.0196 (11)
C3	0.8214 (4)	1.0246 (3)	0.1518 (3)	0.0348 (14)
C4	1.0036 (4)	0.9916 (3)	0.1231 (3)	0.0315 (13)
C5	0.8808 (4)	0.5831 (3)	0.1471 (2)	0.0198 (11)
C6	0.8141 (4)	0.5462 (3)	0.1103 (2)	0.0191 (10)
C7	0.9215 (4)	0.5637 (3)	0.2139 (3)	0.0280 (13)
C8	0.7717 (4)	0.4751 (3)	0.1280 (3)	0.0279 (13)
C9	0.6713 (4)	0.7557 (3)	0.1776 (2)	0.0209 (11)
C10	0.6111 (4)	0.7969 (3)	0.1377 (2)	0.0212 (11)
C11	0.6903 (4)	0.7603 (3)	0.2468 (2)	0.0270 (12)
C12	0.5512 (4)	0.8566 (3)	0.1537 (3)	0.0309 (13)
C14	0.7675 (4)	0.9193 (3)	−0.1231 (3)	0.0242 (12)
C16	0.7327 (4)	0.9315 (4)	−0.1921 (3)	0.0346 (14)
C17	0.9684 (4)	0.7189 (3)	−0.0817 (2)	0.0204 (11)
C18	0.9005 (4)	0.6807 (3)	−0.1173 (3)	0.0254 (12)
C19	1.0447 (4)	0.7546 (3)	−0.1028 (3)	0.0286 (13)
C20	0.8913 (4)	0.6641 (4)	−0.1851 (3)	0.0333 (14)
C21	0.5226 (3)	0.8006 (3)	−0.0753 (2)	0.0232 (11)
C22	0.5192 (4)	0.7264 (3)	−0.0694 (2)	0.0229 (11)
C23	0.4460 (4)	0.8544 (4)	−0.0831 (3)	0.0286 (13)
C24	0.4372 (4)	0.6820 (4)	−0.0670 (3)	0.0292 (13)
C1S	0.5486 (13)	0.3676 (7)	−0.1795 (6)	0.114 (5)
H1SA	0.5377	0.3376	−0.2154	0.137*
C2S	0.4802 (9)	0.3953 (6)	−0.1563 (5)	0.091 (4)
H2SA	0.4206	0.3860	−0.1776	0.109*
C3S	0.4977 (8)	0.4354 (6)	−0.1035 (5)	0.078 (3)
H3SA	0.4501	0.4515	−0.0875	0.094*
C4S	0.5816 (8)	0.4529 (6)	−0.0732 (5)	0.080 (3)
H4SA	0.5910	0.4822	−0.0370	0.096*
C5S	0.6526 (9)	0.4301 (8)	−0.0928 (6)	0.105 (4)
H5SA	0.7107	0.4434	−0.0708	0.126*
C6S	0.6388 (11)	0.3874 (9)	−0.1451 (7)	0.122 (5)
H6SA	0.6879	0.3706	−0.1591	0.146*
C7S	1.1256 (5)	0.8252 (5)	0.2648 (3)	0.051 (2)
H7SA	1.1797	0.8088	0.2574	0.062*
C8S	1.1131 (6)	0.8993 (5)	0.2753 (3)	0.054 (2)
H8SA	1.1590	0.9342	0.2755	0.065*
C9S	1.0345 (6)	0.9235 (5)	0.2855 (3)	0.055 (2)
H9SA	1.0264	0.9748	0.2932	0.066*
C10S	0.9668 (5)	0.8726 (5)	0.2844 (3)	0.0486 (19)
H10A	0.9119	0.8892	0.2903	0.058*
C11S	0.9801 (5)	0.7991 (4)	0.2749 (3)	0.0408 (16)
H11A	0.9343	0.7642	0.2749	0.049*
C12S	1.0593 (5)	0.7743 (4)	0.2652 (3)	0.0438 (17)
H12A	1.0681	0.7227	0.2588	0.053*
C13S	1.0775 (8)	0.5324 (8)	0.0644 (5)	0.071 (4)	0.5
H13A	1.1182	0.5488	0.1009	0.085*	0.5
C14S	1.0094 (9)	0.4841 (7)	0.0679 (5)	0.063 (4)	0.5
H14A	1.0034	0.4674	0.1067	0.076*	0.5
C15S	0.9499 (7)	0.4602 (7)	0.0146 (7)	0.058 (4)	0.5
H15A	0.9033	0.4271	0.0169	0.070*	0.5
C16S	0.9586 (8)	0.4845 (8)	−0.0422 (5)	0.075 (4)	0.5
H16A	0.9179	0.4682	−0.0786	0.089*	0.5
C17S	1.0267 (9)	0.5329 (8)	−0.0457 (5)	0.058 (4)	0.5
H17A	1.0327	0.5496	−0.0845	0.069*	0.5
C18S	1.0862 (7)	0.5568 (7)	0.0077 (7)	0.074 (5)	0.5
H18A	1.1328	0.5899	0.0053	0.088*	0.5

	U11	U22	U33	U12	U13	U23
Pd1	0.01603 (19)	0.01422 (18)	0.01529 (18)	0.00025 (14)	0.00707 (15)	0.00090 (13)
Pd2	0.01734 (19)	0.01621 (19)	0.01881 (19)	0.00263 (14)	0.00848 (16)	0.00203 (14)
Pd3	0.01624 (19)	0.01545 (19)	0.01734 (19)	0.00239 (14)	0.00818 (15)	0.00321 (14)
Pd4	0.0200 (2)	0.01513 (19)	0.01698 (19)	0.00253 (14)	0.01104 (16)	0.00223 (14)
Pd5	0.01651 (19)	0.01516 (18)	0.01306 (18)	0.00024 (14)	0.00665 (15)	0.00022 (13)
Pd6	0.0181 (2)	0.0204 (2)	0.01470 (18)	0.00038 (15)	0.00743 (15)	0.00177 (14)
S1	0.0196 (6)	0.0151 (6)	0.0187 (6)	0.0000 (5)	0.0089 (5)	−0.0018 (4)
S2	0.0147 (6)	0.0179 (6)	0.0191 (6)	−0.0007 (4)	0.0071 (5)	0.0006 (5)
S3	0.0162 (6)	0.0168 (6)	0.0190 (6)	0.0027 (5)	0.0076 (5)	0.0035 (5)
S4	0.0164 (6)	0.0169 (6)	0.0127 (5)	0.0006 (4)	0.0061 (5)	0.0013 (4)
S5	0.0206 (6)	0.0153 (6)	0.0252 (7)	0.0033 (5)	0.0106 (5)	0.0037 (5)
S6	0.0189 (6)	0.0177 (6)	0.0209 (6)	0.0030 (5)	0.0113 (5)	0.0035 (5)
S7	0.0213 (6)	0.0136 (6)	0.0181 (6)	−0.0001 (5)	0.0097 (5)	−0.0001 (4)
S8	0.0165 (6)	0.0183 (6)	0.0160 (6)	0.0018 (5)	0.0073 (5)	0.0008 (4)
S9	0.0161 (6)	0.0246 (7)	0.0185 (6)	0.0021 (5)	0.0074 (5)	0.0057 (5)
S10	0.0179 (6)	0.0220 (7)	0.0165 (6)	0.0028 (5)	0.0087 (5)	0.0063 (5)
S11	0.0268 (7)	0.0202 (7)	0.0176 (6)	−0.0001 (5)	0.0128 (5)	−0.0017 (5)
S12	0.0191 (6)	0.0221 (7)	0.0147 (6)	−0.0032 (5)	0.0055 (5)	−0.0004 (5)
F1	0.065 (3)	0.019 (2)	0.093 (4)	0.000 (2)	0.052 (3)	0.006 (2)
F2	0.094 (5)	0.046 (3)	0.042 (3)	0.019 (3)	0.017 (3)	−0.023 (2)
F3	0.038 (3)	0.023 (2)	0.098 (4)	0.0080 (18)	0.027 (3)	−0.008 (2)
F1A	0.064 (11)	0.025 (10)	0.077 (11)	0.013 (10)	0.031 (11)	−0.014 (10)
F2A	0.064 (11)	0.026 (10)	0.064 (11)	0.005 (10)	0.034 (10)	−0.013 (10)
F3A	0.056 (11)	0.024 (10)	0.060 (11)	−0.001 (10)	0.030 (10)	−0.018 (10)
F4	0.067 (3)	0.046 (3)	0.055 (3)	−0.034 (2)	0.017 (2)	−0.015 (2)
F5	0.032 (2)	0.040 (2)	0.101 (4)	−0.0098 (18)	0.025 (2)	0.000 (2)
F6	0.058 (3)	0.051 (3)	0.048 (2)	−0.028 (2)	0.013 (2)	0.017 (2)
F7	0.055 (3)	0.039 (2)	0.0246 (18)	−0.0074 (18)	0.0003 (17)	0.0047 (15)
F8	0.046 (2)	0.043 (2)	0.043 (2)	0.0202 (18)	0.0028 (19)	0.0157 (18)
F9	0.051 (2)	0.046 (2)	0.0264 (19)	−0.0060 (18)	0.0172 (18)	0.0131 (16)
F10	0.050 (2)	0.0226 (19)	0.053 (2)	−0.0005 (16)	0.014 (2)	0.0164 (16)
F11	0.062 (3)	0.030 (2)	0.046 (2)	−0.0234 (19)	0.010 (2)	0.0023 (17)
F12	0.053 (3)	0.040 (2)	0.071 (3)	−0.0028 (19)	0.045 (2)	0.013 (2)
F13	0.045 (3)	0.115 (4)	0.029 (2)	−0.005 (2)	0.029 (2)	−0.009 (2)
F14	0.127 (5)	0.052 (3)	0.020 (2)	0.030 (3)	0.020 (2)	0.0067 (18)
F15	0.054 (3)	0.062 (3)	0.0247 (19)	−0.020 (2)	0.0075 (18)	−0.0139 (18)
F16	0.035 (2)	0.054 (3)	0.096 (4)	0.0072 (19)	0.045 (2)	0.001 (2)
F17	0.060 (3)	0.063 (3)	0.061 (3)	0.019 (2)	0.012 (2)	−0.037 (2)
F18	0.075 (3)	0.043 (2)	0.056 (3)	0.033 (2)	0.040 (2)	0.014 (2)
C13	0.027 (3)	0.021 (3)	0.033 (3)	0.009 (3)	0.017 (3)	0.015 (3)
C15	0.044 (4)	0.030 (4)	0.048 (4)	0.021 (3)	0.021 (3)	0.014 (3)
F19	0.073 (4)	0.027 (3)	0.105 (6)	0.012 (3)	0.037 (4)	0.027 (4)
F20	0.051 (3)	0.064 (4)	0.057 (4)	0.039 (3)	0.004 (3)	0.016 (3)
F21	0.068 (4)	0.048 (3)	0.046 (3)	0.041 (3)	0.026 (3)	0.012 (3)
C13A	0.035 (6)	0.026 (6)	0.039 (6)	0.013 (6)	0.018 (6)	0.016 (6)
C15A	0.046 (5)	0.033 (5)	0.049 (5)	0.018 (5)	0.018 (5)	0.018 (5)
F19A	0.075 (9)	0.036 (8)	0.074 (9)	0.028 (7)	−0.001 (8)	0.014 (8)
F20A	0.076 (9)	0.038 (8)	0.055 (8)	0.020 (7)	0.012 (8)	0.033 (7)
F21A	0.055 (8)	0.056 (8)	0.069 (9)	0.024 (7)	0.014 (8)	0.023 (8)
F22	0.072 (5)	0.083 (5)	0.028 (3)	0.040 (4)	0.020 (3)	0.016 (3)
F23	0.040 (3)	0.088 (6)	0.036 (3)	−0.025 (4)	−0.009 (3)	0.022 (3)
F24	0.067 (4)	0.040 (4)	0.037 (3)	0.010 (3)	0.013 (3)	0.028 (3)
F22A	0.047 (9)	0.057 (9)	0.041 (8)	−0.013 (7)	0.005 (7)	0.031 (7)
F23A	0.075 (10)	0.055 (8)	0.032 (7)	0.009 (8)	0.001 (7)	0.014 (7)
F24A	0.046 (8)	0.074 (10)	0.048 (8)	−0.001 (8)	−0.004 (7)	0.021 (8)
F25	0.048 (2)	0.042 (2)	0.039 (2)	0.0030 (17)	0.0293 (19)	0.0157 (17)
F26	0.050 (2)	0.040 (2)	0.049 (2)	−0.0169 (18)	0.030 (2)	−0.0025 (18)
F27	0.034 (2)	0.043 (2)	0.055 (2)	0.0116 (16)	0.0312 (19)	0.0087 (18)
F28	0.051 (2)	0.057 (3)	0.040 (2)	0.0063 (19)	0.034 (2)	−0.0085 (18)
F29	0.070 (3)	0.062 (3)	0.036 (2)	−0.023 (2)	0.031 (2)	−0.0237 (19)
F30	0.062 (3)	0.062 (3)	0.0216 (19)	0.017 (2)	0.0141 (19)	0.0102 (17)
F31	0.044 (3)	0.071 (3)	0.077 (3)	0.018 (2)	0.041 (2)	0.016 (2)
F32	0.034 (2)	0.043 (3)	0.147 (5)	0.012 (2)	0.018 (3)	−0.009 (3)
F33	0.073 (3)	0.139 (5)	0.034 (2)	0.076 (4)	0.005 (2)	0.021 (3)
F34	0.033 (2)	0.037 (2)	0.084 (3)	−0.0099 (17)	0.017 (2)	0.007 (2)
F35	0.041 (2)	0.076 (3)	0.037 (2)	−0.021 (2)	0.0197 (19)	−0.004 (2)
F36	0.0226 (19)	0.074 (3)	0.035 (2)	−0.0152 (18)	−0.0040 (16)	0.0093 (19)
C1	0.023 (3)	0.019 (3)	0.027 (3)	−0.005 (2)	0.007 (2)	−0.002 (2)
C2	0.022 (3)	0.015 (3)	0.021 (3)	−0.001 (2)	0.005 (2)	−0.0029 (19)
C3	0.041 (3)	0.023 (3)	0.049 (4)	−0.001 (2)	0.027 (3)	−0.008 (3)
C4	0.032 (3)	0.023 (3)	0.041 (4)	−0.011 (2)	0.011 (3)	−0.002 (3)
C5	0.027 (3)	0.015 (3)	0.020 (3)	0.006 (2)	0.011 (2)	0.0058 (19)
C6	0.025 (3)	0.012 (2)	0.024 (3)	0.0019 (19)	0.011 (2)	0.0034 (19)
C7	0.034 (3)	0.023 (3)	0.025 (3)	0.000 (2)	0.004 (3)	0.008 (2)
C8	0.031 (3)	0.024 (3)	0.032 (3)	−0.004 (2)	0.014 (3)	0.009 (2)
C9	0.028 (3)	0.021 (3)	0.017 (3)	−0.001 (2)	0.012 (2)	−0.001 (2)
C10	0.023 (3)	0.024 (3)	0.021 (3)	−0.003 (2)	0.014 (2)	−0.001 (2)
C11	0.035 (3)	0.033 (3)	0.015 (3)	−0.001 (2)	0.011 (2)	−0.002 (2)
C12	0.033 (3)	0.033 (3)	0.032 (3)	0.002 (3)	0.017 (3)	−0.004 (3)
C14	0.019 (3)	0.028 (3)	0.027 (3)	0.000 (2)	0.008 (2)	0.012 (2)
C16	0.033 (3)	0.042 (4)	0.030 (3)	0.008 (3)	0.009 (3)	0.016 (3)
C17	0.023 (3)	0.022 (3)	0.019 (3)	0.006 (2)	0.013 (2)	0.005 (2)
C18	0.031 (3)	0.028 (3)	0.024 (3)	0.007 (2)	0.019 (3)	0.001 (2)
C19	0.037 (3)	0.025 (3)	0.031 (3)	0.004 (2)	0.021 (3)	0.004 (2)
C20	0.043 (4)	0.038 (4)	0.024 (3)	−0.002 (3)	0.018 (3)	−0.007 (3)
C21	0.014 (3)	0.036 (3)	0.018 (3)	0.006 (2)	0.000 (2)	0.000 (2)
C22	0.025 (3)	0.027 (3)	0.016 (3)	0.002 (2)	0.003 (2)	0.000 (2)
C23	0.019 (3)	0.036 (4)	0.031 (3)	0.005 (2)	0.006 (2)	0.007 (2)
C24	0.024 (3)	0.039 (4)	0.025 (3)	−0.001 (2)	0.008 (3)	0.005 (2)
C1S	0.204 (18)	0.071 (8)	0.070 (8)	−0.025 (10)	0.041 (10)	−0.021 (6)
C2S	0.122 (10)	0.058 (7)	0.083 (8)	−0.049 (7)	0.005 (7)	0.011 (6)
C3S	0.086 (8)	0.070 (7)	0.081 (7)	−0.022 (6)	0.025 (6)	0.014 (6)
C4S	0.088 (8)	0.079 (7)	0.068 (7)	−0.021 (6)	0.012 (6)	0.010 (5)
C5S	0.089 (9)	0.137 (12)	0.085 (9)	0.005 (8)	0.015 (7)	−0.013 (8)
C6S	0.133 (13)	0.124 (13)	0.125 (13)	0.025 (10)	0.064 (11)	−0.003 (10)
C7S	0.040 (4)	0.077 (6)	0.035 (4)	−0.002 (4)	0.004 (3)	−0.002 (4)
C8S	0.058 (5)	0.070 (6)	0.032 (4)	−0.017 (4)	0.007 (4)	0.007 (4)
C9S	0.081 (6)	0.045 (5)	0.034 (4)	0.006 (4)	0.004 (4)	0.001 (3)
C10S	0.052 (5)	0.063 (5)	0.031 (4)	0.010 (4)	0.010 (3)	0.002 (3)
C11S	0.041 (4)	0.052 (5)	0.026 (3)	−0.003 (3)	0.002 (3)	0.000 (3)
C12S	0.048 (4)	0.048 (4)	0.032 (4)	−0.001 (3)	0.004 (3)	−0.005 (3)
C13S	0.070 (7)	0.060 (7)	0.082 (7)	0.032 (5)	0.016 (5)	−0.014 (5)
C14S	0.065 (7)	0.059 (7)	0.068 (7)	0.028 (5)	0.020 (5)	−0.007 (5)
C15S	0.061 (7)	0.041 (6)	0.071 (6)	0.032 (5)	0.016 (5)	−0.010 (5)
C16S	0.075 (7)	0.068 (7)	0.081 (7)	0.030 (6)	0.019 (5)	−0.007 (5)
C17S	0.061 (6)	0.050 (6)	0.064 (7)	0.038 (5)	0.019 (5)	−0.002 (5)
C18S	0.069 (7)	0.067 (8)	0.085 (7)	0.028 (6)	0.019 (5)	−0.005 (5)

Pd1—S1	2.2819 (13)	F22—C16	1.349 (8)
Pd1—S2	2.3040 (13)	F23—C16	1.279 (9)
Pd1—S4	2.3564 (12)	F24—C16	1.333 (9)
Pd1—S3	2.3718 (13)	F22A—C16	1.195 (18)
Pd1—Pd5	3.2516 (6)	F23A—C16	1.32 (2)
Pd2—S8	2.3486 (13)	F24A—C16	1.41 (2)
Pd2—S5	2.3554 (13)	F25—C19	1.321 (7)
Pd2—S9	2.3586 (14)	F26—C19	1.322 (7)
Pd2—S1	2.3599 (13)	F27—C19	1.331 (7)
Pd3—S5	2.2883 (13)	F28—C20	1.331 (7)
Pd3—S10	2.2892 (13)	F29—C20	1.322 (7)
Pd3—S6	2.3574 (13)	F30—C20	1.328 (8)
Pd3—S2	2.3706 (13)	F31—C23	1.330 (7)
Pd3—Pd6	3.2528 (6)	F32—C23	1.312 (8)
Pd4—S6	2.2892 (13)	F33—C23	1.294 (7)
Pd4—S7	2.2979 (13)	F34—C24	1.327 (7)
Pd4—S11	2.3021 (14)	F35—C24	1.323 (7)
Pd4—S3	2.3065 (13)	F36—C24	1.313 (7)
Pd5—S8	2.2858 (13)	C1—C2	1.333 (7)
Pd5—S4	2.2892 (13)	C1—C3	1.522 (8)
Pd5—S7	2.3695 (13)	C2—C4	1.528 (7)
Pd5—S12	2.3725 (13)	C5—C6	1.334 (8)
Pd6—S9	2.2860 (13)	C5—C7	1.521 (7)
Pd6—S12	2.3026 (13)	C6—C8	1.532 (7)
Pd6—S10	2.3620 (13)	C9—C10	1.347 (8)
Pd6—S11	2.3822 (14)	C9—C11	1.515 (7)
S1—C1	1.775 (5)	C10—C12	1.523 (7)
S2—C2	1.767 (5)	C14—C16	1.529 (8)
S3—C5	1.778 (5)	C17—C18	1.346 (8)
S4—C9	1.770 (5)	C17—C19	1.530 (8)
S5—C13	1.774 (15)	C18—C20	1.527 (8)
S5—C13A	1.78 (6)	C21—C22	1.339 (8)
S6—C17	1.757 (5)	C21—C23	1.513 (7)
S7—C6	1.768 (5)	C22—C24	1.519 (8)
S8—C10	1.768 (5)	C1S—C2S	1.395 (18)
S9—C21	1.779 (6)	C1S—C6S	1.47 (2)
S10—C14	1.765 (6)	C1S—H1SA	0.9500
S11—C18	1.774 (6)	C2S—C3S	1.356 (15)
S12—C22	1.779 (6)	C2S—H2SA	0.9500
F1—C3	1.307 (8)	C3S—C4S	1.356 (14)
F2—C3	1.317 (8)	C3S—H3SA	0.9500
F3—C3	1.343 (8)	C4S—C5S	1.355 (16)
F1A—C3	1.23 (5)	C4S—H4SA	0.9500
F2A—C3	1.43 (4)	C5S—C6S	1.375 (18)
F3A—C3	1.25 (4)	C5S—H5SA	0.9500
F4—C4	1.324 (7)	C6S—H6SA	0.9500
F5—C4	1.323 (7)	C7S—C8S	1.370 (12)
F6—C4	1.316 (7)	C7S—C12S	1.380 (11)
F7—C7	1.338 (7)	C7S—H7SA	0.9500
F8—C7	1.321 (7)	C8S—C9S	1.376 (12)
F9—C7	1.334 (7)	C8S—H8SA	0.9500
F10—C8	1.326 (7)	C9S—C10S	1.390 (12)
F11—C8	1.327 (7)	C9S—H9SA	0.9500
F12—C8	1.323 (7)	C10S—C11S	1.358 (10)
F13—C11	1.317 (7)	C10S—H10A	0.9500
F14—C11	1.323 (7)	C11S—C12S	1.384 (10)
F15—C11	1.314 (7)	C11S—H11A	0.9500
F16—C12	1.303 (7)	C12S—H12A	0.9500
F17—C12	1.324 (7)	C13S—C14S	1.3900
F18—C12	1.328 (7)	C13S—C18S	1.3900
C13—C14	1.328 (15)	C13S—H13A	0.9500
C13—C15	1.519 (9)	C14S—C15S	1.3900
C15—F19	1.306 (10)	C14S—H14A	0.9500
C15—F21	1.331 (9)	C15S—C16S	1.3900
C15—F20	1.334 (10)	C15S—H15A	0.9500
C13A—C14	1.35 (5)	C16S—C17S	1.3900
C13A—C15A	1.518 (16)	C16S—H16A	0.9500
C15A—F19A	1.301 (17)	C17S—C18S	1.3900
C15A—F20A	1.330 (17)	C17S—H17A	0.9500
C15A—F21A	1.331 (16)	C18S—H18A	0.9500
S1—Pd1—S2	86.42 (5)	F8—C7—F9	108.5 (5)
S1—Pd1—S4	93.84 (5)	F8—C7—F7	107.3 (5)
S2—Pd1—S4	178.49 (5)	F9—C7—F7	105.9 (5)
S1—Pd1—S3	176.57 (5)	F8—C7—C5	111.9 (5)
S2—Pd1—S3	90.89 (5)	F9—C7—C5	112.2 (5)
S4—Pd1—S3	88.80 (4)	F7—C7—C5	110.7 (4)
S1—Pd1—Pd5	93.47 (4)	F12—C8—F10	107.8 (5)
S2—Pd1—Pd5	133.76 (4)	F12—C8—F11	108.1 (5)
S4—Pd1—Pd5	44.74 (3)	F10—C8—F11	106.0 (5)
S3—Pd1—Pd5	86.86 (3)	F12—C8—C6	112.3 (5)
S8—Pd2—S5	176.83 (5)	F10—C8—C6	111.6 (5)
S8—Pd2—S9	89.77 (5)	F11—C8—C6	110.8 (5)
S5—Pd2—S9	90.25 (5)	C10—C9—C11	125.5 (5)
S8—Pd2—S1	89.64 (4)	C10—C9—S4	120.4 (4)
S5—Pd2—S1	90.08 (5)	C11—C9—S4	114.0 (4)
S9—Pd2—S1	175.18 (5)	C9—C10—C12	126.5 (5)
S5—Pd3—S10	86.63 (5)	C9—C10—S8	120.1 (4)
S5—Pd3—S6	178.23 (5)	C12—C10—S8	113.4 (4)
S10—Pd3—S6	93.32 (5)	F15—C11—F13	107.7 (5)
S5—Pd3—S2	95.05 (5)	F15—C11—F14	106.6 (5)
S10—Pd3—S2	178.23 (5)	F13—C11—F14	106.9 (5)
S6—Pd3—S2	84.98 (5)	F15—C11—C9	112.4 (5)
S5—Pd3—Pd6	89.34 (4)	F13—C11—C9	112.1 (5)
S10—Pd3—Pd6	46.55 (3)	F14—C11—C9	110.8 (5)
S6—Pd3—Pd6	89.35 (4)	F16—C12—F17	108.7 (5)
S2—Pd3—Pd6	132.79 (3)	F16—C12—F18	108.4 (5)
S6—Pd4—S7	178.58 (5)	F17—C12—F18	105.3 (5)
S6—Pd4—S11	88.12 (5)	F16—C12—C10	111.5 (5)
S7—Pd4—S11	92.14 (5)	F17—C12—C10	112.5 (5)
S6—Pd4—S3	91.43 (5)	F18—C12—C10	110.1 (4)
S7—Pd4—S3	88.23 (5)	C13—C14—C16	126.7 (7)
S11—Pd4—S3	176.66 (5)	C13A—C14—C16	125.9 (18)
S8—Pd5—S4	86.35 (4)	C13—C14—S10	120.4 (6)
S8—Pd5—S7	178.63 (5)	C13A—C14—S10	121.3 (17)
S4—Pd5—S7	94.66 (5)	C16—C14—S10	112.8 (4)
S8—Pd5—S12	93.96 (5)	F22A—C16—F23A	114.1 (15)
S4—Pd5—S12	178.97 (5)	F23—C16—F24	109.2 (6)
S7—Pd5—S12	85.01 (5)	F23—C16—F22	109.8 (7)
S8—Pd5—Pd1	88.07 (3)	F24—C16—F22	102.5 (6)
S4—Pd5—Pd1	46.43 (3)	F22A—C16—F24A	106.1 (14)
S7—Pd5—Pd1	91.96 (3)	F23A—C16—F24A	100.7 (14)
S12—Pd5—Pd1	132.58 (3)	F22A—C16—C14	117.4 (11)
S9—Pd6—S12	86.49 (5)	F23—C16—C14	113.7 (5)
S9—Pd6—S10	93.11 (5)	F23A—C16—C14	109.6 (8)
S12—Pd6—S10	178.24 (5)	F24—C16—C14	111.5 (6)
S9—Pd6—S11	176.11 (5)	F22—C16—C14	109.5 (5)
S12—Pd6—S11	89.78 (5)	F24A—C16—C14	107.3 (9)
S10—Pd6—S11	90.59 (5)	C18—C17—C19	125.9 (5)
S9—Pd6—Pd3	92.67 (4)	C18—C17—S6	121.1 (4)
S12—Pd6—Pd3	133.57 (4)	C19—C17—S6	112.9 (4)
S10—Pd6—Pd3	44.72 (3)	C17—C18—C20	123.9 (5)
S11—Pd6—Pd3	89.13 (4)	C17—C18—S11	121.9 (4)
C1—S1—Pd1	104.64 (19)	C20—C18—S11	114.2 (4)
C1—S1—Pd2	106.59 (19)	F25—C19—F26	107.3 (5)
Pd1—S1—Pd2	92.32 (4)	F25—C19—F27	108.2 (5)
C2—S2—Pd1	104.11 (18)	F26—C19—F27	107.4 (5)
C2—S2—Pd3	101.83 (18)	F25—C19—C17	112.3 (5)
Pd1—S2—Pd3	93.38 (5)	F26—C19—C17	110.5 (4)
C5—S3—Pd4	102.48 (18)	F27—C19—C17	110.9 (5)
C5—S3—Pd1	107.66 (17)	F29—C20—F30	107.3 (6)
Pd4—S3—Pd1	90.36 (4)	F29—C20—F28	106.9 (5)
C9—S4—Pd5	105.15 (18)	F30—C20—F28	108.0 (5)
C9—S4—Pd1	104.00 (18)	F29—C20—C18	110.3 (5)
Pd5—S4—Pd1	88.83 (4)	F30—C20—C18	112.3 (5)
C13—S5—Pd3	104.7 (3)	F28—C20—C18	111.9 (5)
C13A—S5—Pd3	105.4 (11)	C22—C21—C23	126.4 (5)
C13—S5—Pd2	105.7 (5)	C22—C21—S9	120.5 (4)
C13A—S5—Pd2	107.2 (19)	C23—C21—S9	113.1 (4)
Pd3—S5—Pd2	90.51 (5)	C21—C22—C24	125.2 (5)
C17—S6—Pd4	103.37 (19)	C21—C22—S12	120.4 (4)
C17—S6—Pd3	103.45 (18)	C24—C22—S12	114.3 (4)
Pd4—S6—Pd3	92.05 (5)	F33—C23—F32	108.3 (6)
C6—S7—Pd4	101.93 (18)	F33—C23—F31	107.4 (5)
C6—S7—Pd5	104.86 (17)	F32—C23—F31	105.0 (5)
Pd4—S7—Pd5	89.08 (4)	F33—C23—C21	111.4 (5)
C10—S8—Pd5	105.62 (18)	F32—C23—C21	111.5 (5)
C10—S8—Pd2	106.13 (18)	F31—C23—C21	112.9 (5)
Pd5—S8—Pd2	92.40 (5)	F36—C24—F35	108.3 (5)
C21—S9—Pd6	104.98 (19)	F36—C24—F34	107.1 (5)
C21—S9—Pd2	106.06 (18)	F35—C24—F34	106.4 (5)
Pd6—S9—Pd2	92.21 (5)	F36—C24—C22	112.2 (5)
C14—S10—Pd3	105.1 (2)	F35—C24—C22	111.6 (5)
C14—S10—Pd6	104.44 (18)	F34—C24—C22	110.9 (5)
Pd3—S10—Pd6	88.73 (4)	C2S—C1S—C6S	116.1 (11)
C18—S11—Pd4	101.9 (2)	C2S—C1S—H1SA	122.0
C18—S11—Pd6	107.36 (19)	C6S—C1S—H1SA	122.0
Pd4—S11—Pd6	89.04 (4)	C3S—C2S—C1S	120.8 (12)
C22—S12—Pd6	104.49 (19)	C3S—C2S—H2SA	119.6
C22—S12—Pd5	101.71 (18)	C1S—C2S—H2SA	119.6
Pd6—S12—Pd5	93.64 (5)	C4S—C3S—C2S	121.4 (12)
C14—C13—C15	125.0 (11)	C4S—C3S—H3SA	119.3
C14—C13—S5	121.1 (6)	C2S—C3S—H3SA	119.3
C15—C13—S5	113.9 (9)	C5S—C4S—C3S	122.3 (12)
F19—C15—F21	108.9 (8)	C5S—C4S—H4SA	118.9
F19—C15—F20	107.9 (8)	C3S—C4S—H4SA	118.9
F21—C15—F20	104.3 (7)	C4S—C5S—C6S	118.7 (13)
F19—C15—C13	111.7 (8)	C4S—C5S—H5SA	120.6
F21—C15—C13	110.9 (8)	C6S—C5S—H5SA	120.6
F20—C15—C13	112.8 (8)	C5S—C6S—C1S	120.6 (13)
C14—C13A—C15A	129 (4)	C5S—C6S—H6SA	119.7
C14—C13A—S5	119.4 (16)	C1S—C6S—H6SA	119.7
C15A—C13A—S5	112 (3)	C8S—C7S—C12S	119.9 (8)
F19A—C15A—F20A	105.7 (19)	C8S—C7S—H7SA	120.1
F19A—C15A—F21A	109 (2)	C12S—C7S—H7SA	120.1
F20A—C15A—F21A	104.6 (19)	C7S—C8S—C9S	120.3 (8)
F19A—C15A—C13A	114 (2)	C7S—C8S—H8SA	119.8
F20A—C15A—C13A	113 (2)	C9S—C8S—H8SA	119.8
F21A—C15A—C13A	110 (2)	C8S—C9S—C10S	119.9 (8)
C2—C1—C3	126.7 (5)	C8S—C9S—H9SA	120.0
C2—C1—S1	120.6 (4)	C10S—C9S—H9SA	120.0
C3—C1—S1	112.7 (4)	C11S—C10S—C9S	119.5 (8)
C1—C2—C4	125.4 (5)	C11S—C10S—H10A	120.3
C1—C2—S2	120.7 (4)	C9S—C10S—H10A	120.3
C4—C2—S2	113.7 (4)	C10S—C11S—C12S	120.8 (7)
F1A—C3—F3A	112 (3)	C10S—C11S—H11A	119.6
F1—C3—F2	109.3 (6)	C12S—C11S—H11A	119.6
F1—C3—F3	105.7 (6)	C7S—C12S—C11S	119.5 (7)
F2—C3—F3	106.4 (6)	C7S—C12S—H12A	120.2
F1A—C3—F2A	106 (3)	C11S—C12S—H12A	120.2
F3A—C3—F2A	105 (3)	C14S—C13S—C18S	120.0
F1A—C3—C1	113.3 (18)	C14S—C13S—H13A	120.0
F3A—C3—C1	110.8 (18)	C18S—C13S—H13A	120.0
F1—C3—C1	113.5 (5)	C15S—C14S—C13S	120.0
F2—C3—C1	111.3 (6)	C15S—C14S—H14A	120.0
F3—C3—C1	110.3 (5)	C13S—C14S—H14A	120.0
F2A—C3—C1	109.3 (16)	C14S—C15S—C16S	120.0
F6—C4—F5	109.3 (5)	C14S—C15S—H15A	120.0
F6—C4—F4	106.6 (5)	C16S—C15S—H15A	120.0
F5—C4—F4	105.9 (5)	C15S—C16S—C17S	120.0
F6—C4—C2	111.9 (5)	C15S—C16S—H16A	120.0
F5—C4—C2	110.9 (5)	C17S—C16S—H16A	120.0
F4—C4—C2	112.0 (5)	C16S—C17S—C18S	120.0
C6—C5—C7	124.8 (5)	C16S—C17S—H17A	120.0
C6—C5—S3	121.2 (4)	C18S—C17S—H17A	120.0
C7—C5—S3	114.0 (4)	C17S—C18S—C13S	120.0
C5—C6—C8	124.8 (5)	C17S—C18S—H18A	120.0
C5—C6—S7	122.3 (4)	C13S—C18S—H18A	120.0
C8—C6—S7	112.9 (4)