C₆₀ in a peptidic cage: a case of symmetry mismatch studied by crystallography and solid-state NMR

A supramolecular complex, formed by encapsulation of C₆₀ fullerene in a molecular container built from two resorcin[4]arene rims zipped together by peptidic arms hydrogen bonded into a cylindrical β-sheet, was studied by X-ray crystallography, solid-state and solution NMR, EPR spectroscopy and differential scanning calorimetry (DSC). The crystal structure, determined at 100 K, reveals that the complex occupies 422 site symmetry, which is compatible with the molecular symmetry of the container but not of the fullerene molecule, which has only 222 symmetry. The additional crystallographic symmetry leads to a complicated but discrete dis­order, which could be resolved and modelled using advanced features of the existing refinement software. Solid-state NMR measurements at 184–333 K indicate that the thermal motion of C₆₀ in this temperature range is fast but has different activation energies at different temperatures, which was attributed to a phase transition, which was confirmed by DSC. Intriguingly, the activation energy for reorientations of C₆₀ in the solid state is very similar for the free and encaged molecules. Also, the rotational diffusion coefficients seem to be very similar or even slightly higher for the encaged fullerene compared to the free molecule. We also found that chemical shift anisotropy (CSA) is not the main relaxation mechanism for the ¹³C spins of C₆₀ in the studied complex.

1. Introduction

An inherent feature of molecular capsules is the presence of a cavity that can host and sequester other molecules (guests) from the external environment. By virtue of this, molecular capsules find application in the storage of unstable and reactive molecules, and their controlled release (Mal et al., 2009), as catalytic nanovessels that provide a constrictive environment for single reactions (Zhang & Tiefenbacher, 2015; Zhang et al., 2017) and domino-type processes (Salles et al., 2013). Interactions between a capsule and its cargo are of particular interest to molecular engineers because these are the very factors that control the thermodynamics and kinetics of the encapsulation process. However, precise characterization of the mode of such interactions is in most cases troublesome, especially for spherical guests residing in spherical cavities. Firstly, because the occupation factor (percentage of the internal volume of the cavity that is occupied by the guest molecule) is often low. For non-polar guests, an optimal occupation factor is claimed to be 55%, which is similar to the occupation factor of a non-polar liquid phase (Mecozzi & Rebek, 1998). For a polar guest, the occupation factor can reach higher values, but it is still similar to the occupation factors of polar liquid phases (e.g. ∼75%, as for liquid water) (Szumna, 2009). These low occupation factors mean that the guest molecule in the cavity behaves in a solution-like manner – it is thermally randomly dis­ordered. Another possible complication comes from the high symmetry of such systems, which often results in the distribution of the electron density over several symmetry-related positions. The importance of symmetry matching of the host and guest molecules should be noted, as it maximizes the number of points of contact and the efficiency of the interaction (Atwood et al., 1999). All these factors, together with the typically low resolution of the diffraction data, render the precise determination of the position of guests inside cavities problematic. In this article, we report the challenging and tedious but ultimately successful path toward the resolution of the dis­ordered positions of the C₆₀ spherical guest inside the cavity of a peptidic molecular capsule in a supramolecular crystal, additionally complicated by a symmetry mismatch between the host and guest components. Moreover, by measuring the solid-state ¹³C nuclear spin relaxation for the encapsulated fullerene molecule, we were able to analyze the dynamic behaviour of the entrapped fullerene over a broad temperature range. Yanagisawa et al. (2007) previously performed investigations of a similar inclusion complex by X-ray and NMR lineshape analysis, but the exploited model, i.e. an iridium porphyrin cyclic dimer with C₆₀ inside the cavity, revealed no dis­order in the solid state. The ¹³C signal broadening which was noticed in the liquid-state NMR spectra indicated very likely some dynamical behaviour of C₆₀, but in fact no convincing arguments for the origin of the broadening were shown.

Our motivation for undertaking an in-depth analysis of the interactions of encapsulated C₆₀ with its host, the peptidic capsule (3)₂ (Fig. 1), was stimulated by the unusually high affinity of fullerenes towards such capsules that is not intuitive in terms of intermolecular forces, because it involves interactions of C₆₀ with the backbones of the peptides, while in the previously reported crystal structures of C₆₀ with proteins (Kim et al., 2016), more intuitive interactions involving π–π stacking with tyrosine (Tyr) side chains were demonstrated. We have recently prepared a series of cavitands similar to 3 that are composed of resorcin[4]arenes decorated with various peptidic arms (Szymański et al., 2016, 2018; Grajda et al., 2017; Eichstaedt et al., 2019). These cavitands have vase shapes with the resorcin[4]arene parts constituting rigid bases, each equipped with four flexible oligopeptide arms. The cavitands dimerize to form non-covalent molecular capsules with an internal volume of ca 700 ų. Interactions between the two cavitands involve hydrogen bonds between the peptide backbones zipped together by a circular pattern of hydrogen bonds that mimic the association motif of a protein β-barrel. The capsules exhibit a marked preference towards encapsulation of fullerenes (C₆₀ or C₇₀), both in polar (methanol, H₂O; Grajda et al., 2017; Eichstaedt et al., 2019) and non-polar (CHCl₃; Szymański et al., 2016, 2018; Grajda et al., 2017) environments. Such a complexation preference is quite striking since the internal surface of the cavity is largely composed of the peptide backbones, with a considerably smaller contribution from the aromatic rings of the cavitand. Moreover, insensitivity to the complexation environment is also unprecedented, because in solvents of such drastically different polarity [ɛ(CHCl₃) = 4.8 and ɛ(H₂O) = 80.1] different non-covalent interactions should dominate, which in turn should lead to the formation of different complexes. Specifically, hydro­phobic effects should dominate in water, while electrostatic-based interactions should predominate in a non-polar environment. It is very unusual for these interactions, which are orthogonal under given conditions, to lead to the same type of complex. Motivated by these intriguing observations, we aimed at crystallographic and NMR investigations of the origins of the 3/C₆₀ interactions.

Figure 1 Synthesis and schematic structure of complex (3)2C60 with highlighted molecular components (blue is the lower rim, green the resorcinarene moiety, red the upper rim and gray fullerene).

2. Materials and methods

2.1. Sample preparation

Tetra­formyl­resorcin[4]arene, 1, and N-acetyl-L-phenyl­alanine hydrazide, 2, were obtained according to literature procedures (Szymański et al., 2016; Grajda et al., 2013). 1 (0.125 mmol, 103 mg), 2 (0.5 mmol, 111 mg) and fullerene C₆₀ (62.5 µmol, 47 mg) were dissolved in CHCl₃ (5 ml) in a sealed pressure vial. The reaction mixture was stirred at 70°C for 4 d. The mixture was cooled and filtered. The solution was then evaporated under reduced pressure. The products were analyzed by NMR spectroscopy. The quantitative formation of the (3)₂C₆₀ complex was detected.

2.2. Crystallization

Complex (3)₂C₆₀ (10 mg) was dissolved in a 3:1 (v/v) mixture (2 ml) of CHCl₃ and EtOH, and was allowed to crystallize by slow evaporation.

2.3. X-ray data collection

High-resolution X-ray diffraction data were collected at the EMBL beamline P13 of the Petra III storage ring (DESY, Hamburg, Germany) at a wavelength of 0.8266 Å, using a PILATUS 6M detector. The data were collected at the cryogenic temperature of 100 K. The diffraction data were indexed, integrated and scaled using the XDS package (Kabsch, 2010). Scaling of the intensities was acceptable and similar in the space groups I4 and I422, but for reasons explained below, we first chose the former. The correct latter space group was used for the final model refinement. The X-ray data collection statistics are summarized in Table 1. [Raw diffraction images for the (3)₂C₆₀ crystal were deposited in the RepOD repository at the ICM of the University of Warsaw and are available for download with the following digital object identifier (DOI): https://dx.doi.org/10.18150/XMEUNL.]

Table 1
Data collection and refinement statistics for the (3)₂C₆₀ structure

Data collection
Radiation source	P13 EMBL, Petra III, Hamburg
Wavelength (Å)	0.8266
Temperature (K)	100
Space group	I422
Cell dimensions a, c (Å)	21.910, 25.44
Resolution range (Å)	16.60–0.76 (0.81–0.76)†
Number of reflections	5405
Completeness native (%)	92.5 (55.0)†
Redundancy	5.75 (1.82)†
〈I/σI〉	34.6 (8.42)†
Rmerge (%)	4.9 (7.7)†
Wilson B-factor (Å)^2	4.87
Refinement
Refinement program	SHELXL (Sheldrick, 2015b)
Resolution (Å)	16.60–0.76
No. of reflections	5405
R (%)	8.89
No. of atoms in ASU	40.5
〈B〉 (Å)^2	5.24

†Values in parentheses correspond to the last resolution shell.

2.4. Structure solution and refinement

The crystal structure of (3)₂C₆₀ was solved in the space group I4 by direct methods using the SHELXT program (Sheldrick, 2015a). The preliminary model of the structure generated by SHELXT included two quarters of a single resorcin[4]arene skeleton decorated with L-phenyl­alanine arms and lower-rim alkyl chains (i.e. a quarter of the entire resorcinarene–peptide capsule) arranged around a fourfold axis, plus a few randomly placed fullerene atoms.

After a few cycles of isotropic refinement with SHELXL (Sheldrick, 2015b), which converged at R ∼24%, the initial electron-density maps were generated and were thoroughly inspected with the COOT program (Emsley et al., 2010). The maps clearly showed well-defined positions for all atoms forming the capsule and a characteristic spherical density corresponding to the fullerene molecule. However, the number and distribution of the peaks at the fullerene site indicated a massive dis­order of this molecule. Before the next round of refinement, the model generated by SHELXT was revised manually by assigning proper atom types and removing all spurious fullerene atoms. After a round of least-squares refinement of this model, which corresponded to about one half of the expected asymmetric unit (ASU) content in the space group I4, the R factor increased to ∼30%, but it turned out that the electron density of the fullerene molecule was still clearly visible with pronounced, fairly well separated, peaks (Fig. 2a). Interpretation of this map was, however, very difficult because we were dealing with the effect of overlapping partially occupied fullerene molecules. In addition, the fullerene molecule was located on the fourfold axis (passing through two opposite C—C bonds, each shared by two hexagons), which is not the site symmetry of the C₆₀ molecule.

Figure 2 X-ray crystal structure of (3)2C60. (a) Initial mFo–DFc electron-density OMIT map (green) contoured at 3.0σ of the fullerene molecule and the 2mFo–DFc map (blue) of the whole capsule contoured at 1.5σ (the asymmetric unit contains only of the capsule, R ≈ 30%). (b) Eight halves of the fullerene moiety in the unit cell (forming four molecules of C60) shown in the final 2mFo–DFc electron-density map contoured at 2.0σ. The four complete dis­ordered C60 molecules (two pairs: red–green and blue–yellow) lying on the fourfold axis are shown, viewed along the crystallographic c axis. (c)/(d) A stick representation of the final structure with refined dis­order of the C60 molecule.

The location of the electron density corresponding to the C₆₀ molecule within the unit cell, the I4 symmetry and the arrangement of the peaks at the fullerene site all implied that the ASU should contain two halves of the fullerene molecule with occupancies of , rotated relative to each other through a dyad perpendicular to the fourfold axis. Since building a dis­ordered fullerene model and fitting it into the electron-density map in such a complicated case, it is much easier to handle an entire C₆₀ molecule rather than its halves; thus, two complete C₆₀ molecules with occupancy were modelled into the electron-density map.

For a similar reason, the structure solution and initial refinement were carried out in the space group I4, despite the fact that already during data processing and scaling the possibility of higher symmetry, I422, was quite obvious. However, after a preliminary analysis of the electron-density map, which strongly indicated a model of two dis­ordered fullerene molecules on the fourfold axis, it was decided that the first stages of structural analysis would be carried out with the assumption of lower symmetry, where atoms of the two whole fullerene molecules would have an occupancy of , rather than , as required by the higher I422 symmetry.

After numerous attempts to model the dis­ordered fullerene molecules, it became obvious that the only possible mode of their arrangement requires exact alignment of the molecular twofold axes with the crystallographic fourfold axis of this site. During the first cycles of refinement of the complete model with two properly oriented fullerene molecules, it turned out that they tend to spin out of alignment of their twofold axes with the fourfold axis of the space group, that the R factor is still high (∼23%) and that the model becomes inconsistent with the electron-density map because the positions of the fullerene atoms no longer match the electron-density peaks. To proceed with the refinement it was, therefore, necessary to solve the problem of fullerene rotation in the electron-density map. SHELXL is probably the only program that has a mechanism to prevent such unwanted rotations and at the same time to correctly refine the structure. The twofold axes of the fullerene molecule (there are 15 different twofold axes passing through opposite C—C bonds) that are of interest in this context run through the centres of two opposite 6–6 bonds, i.e. the common bonds of two six-membered rings. To keep the fullerene in a proper orientation, first the centres of two selected bonds have to be fixed on the fourfold axis. To achieve this, the SUMP instruction of the SHELXL program was used. SUMP allows free variables to be logically related and is most commonly used to restrain the occupancy factors of more than two atoms sharing the same site, or three or more alternative conformations. SUMP can do much more but is rarely used for anything else. This command has one very important and unique feature, i.e. it makes it possible to use custom restraints by defining a linear equation describing a relationship between selected free variables along with a standard deviation that determines the weight of such a restraint. These variables are then refined under the control of the defined equations. The general command syntax is:

SUMP c sigma c1 m1 c2 m2 …, where c = c1 * fv(m1) + c2 * fv(m2) + …,

fv(m1), fv(m2), … are refinable free variables, and sigma determines the weight of the restraint.

In the present case, to fix the centres of bonds on the fourfold axis located at (x = , y = ), the SUMP command with the following parameters was used (the example is for one selected bond, i.e. C5—C6):

SUMP 1.0 0.01 1.0 2 1.0 3,

where c, c1, c2 = 1.0, fv(m1) and fv(m2) with m values of 2 and 3 correspond to the second and third free variables, assigned with starting values of the x coordinates of atoms C5 and C6, respectively.

Analogously, for the y coordinates of atoms C5 and C6, the SUMP command is:

SUMP 1.0 0.01 1.0 4 1.0 5,

where the values 4 and 5 refer to the free variables defined as the y coordinates of atoms C5 and C6, respectively. To carry out the refinement, the atom instructions for C5 and C6 in the SHELXL command file should be as follows:

C5 1 21.000000 41.000000 61.000000 10.12500 0.05

C6 1 31.000000 51.000000 61.000000 10.12500 0.05.

This means that the coordinates x1, y1 and x2, y2 of the C5 and C6 atoms, respectively, will be refined while complying with the following equations:

1 * x1 + 1 * x2 = 1 and 1 * y1 + 1 * y2 = 1,

i.e. with c, c1, c2 = 1, x1 = fv(2), x2 = fv(3), y1 = fv(4) and y2 = fv(5). The z coordinate of both atoms, defined as free variable 6 [fv(6)] will be the same for both atoms. The initial coordinates of the C5 and C6 atoms are given using the FVAR instruction defining the refined variables:

scale 21 31 41 51 61

FVAR 2.76192 0.47145 0.52856 0.51238 0.48761 0.63740

After applying the appropriate SUMP, FVAR and atom instruction (for two selected bonds per each fullerene molecule), the refinement became stable and converged with R ∼ 15%. Despite the complex dis­order, the positions of the fullerene C atoms fit the electron density well and the molecular twofold axes of the fullerene models coincided with the crystallographic fourfold axis.

However, a detailed analysis of the symmetry of the model suggested that the true symmetry of the crystal may be higher than assumed during data processing and initial refinement, and that the correct crystal class is 422. Accordingly, further refinement was carried out in the space group I422, which allowed model reduction by one-half by reason of the twofold symmetry perpendicular to the principal fourfold axis. The new ASU contains a model consisting of only of a resor­cin­arene moiety decorated with a lower-rim alkyl chain and an upper-rim L-phenyl­alanine arm ( of the whole capsule) and one fullerene molecule with an occupancy of (although we know that according to the 422 symmetry, the ASU should contain only of the C₆₀ molecule with an occupancy of ). In the following refinement, after each round of minimization, the COOT program was used for visualization of the electron-density maps and for manual rebuilding of the atomic models.

Since the refinement was stable at this stage, it was possible to remove the redundant half of the symmetrically dependent C₆₀ molecule. Ultimately, the structure was refined in the very rare space group I422 with a model consisting of only of a resorcinarene molecule with one lower-rim alkyl chain and one L-phenyl­alanine arm ( of the whole capsule) at full occupancy, and of of the fullerene molecule sitting on the fourfold axis, with an occupancy of . To perform the refinement with only of the C₆₀ molecule (i.e. with a model that is correctly represented in the ASU from a crystallographic point of view), it was necessary to change the method of restraining the direction of the twofold axis of the fullerene molecule. The SUMP instruction cannot be used for this purpose any longer because there is no possibility to define the centre of the 6–6 bond, as one of the atoms forming this bond is not part of the model (it is generated by the fourfold symmetry). An alternative method to achieve a similar effect as with the SUMP instructions is based on the observation that in the proper fullerene orientation certain groups of its atoms must have the same z coordinate, which can be refined as one free variable. After updating the SHELXL instruction file and defining all z coordinates of the fullerene molecule by reference to FVAR free variables, the refinement was still stable. Because the fullerene molecule shows a high degree of dis­order, with four alternative orientations of the molecule with an occupancy of , during refinement, geometric restraints were used for all the C₆₀ bond lengths and angles, using the DFIX and DANG instructions with default weights. The definition of such restraints was relatively straightforward, because the C₆₀ fullerene molecule has only two different bond angles with ideal values of 108° and 120° and two types of C—C bonds, i.e. double (6–6) and single (6–5), with average bond lengths of 1.397 and 1.454 Å, respectively (Schein & Sands-Kidner, 2008; Aoyagi et al., 2014). The stability of the dis­ordered L-phenyl­alanine residues and alkyl groups during refinement was enforced by appropriate stereochemical restraints with default weights.

Introducing into the model double conformations of the L-phenyl­alanine ring and alkyl groups, which are clearly visible in the electron-density map, coupled with anisotropic ADP refinement, reduced the R factor to ∼9%.

2.5. Sample preparation for NMR measurements in the solid state

65 mg of (3)₂C₆₀ was ground in an agate mortar, mixed with 42 mg of ground lead nitrate and packed into a 4 mm zirconia rotor in order to prepare the sample for solid-state NMR measurements. The ²⁰⁷Pb resonance of lead nitrate was used as an internal NMR thermometer (Beckmann & Dybowski, 2000). The ¹³C longitudinal relaxation times of fullerene C₆₀ in (3)₂ were determined in the temperature range 184–333 K at a magnetic field of 11.73 T using a Bruker AVANCE II 500 MHz machine. The direct carbon-detected inversion-recovery method was used. Typical parameters were as follows: 8–24 scans for each of the 8–14 incremented delays, spectral widths of 400 ppm, acquisition times of 160 ms and 90° pulses of 3.5 µs. The recycle delay was always longer than five times the T₁ of the ¹³C nuclei of C₆₀. A Bruker DVT 4 mm MAS probe head was used. In the temperature range 248–333 K, measurements were performed under magic angle spinning conditions with a frequency of 2–3 kHz, while below 248 K the sample was not spun in order to avoid large temperature gradients. Similar experiments were performed at a magnetic field of 7.04 T using a Bruker AVANCE II 300 MHz spectrometer equipped with a Bruker VTN 4 mm probe head. The temperature range was 194–298 K. Since samples in the VTN probe head are much less prone to temperature gradients, we used magic angle spinning over the whole temperature range.

2.6. Theory used for calculation of dynamic parameters in the solid state from NMR data

In isotropic liquids, where molecules undergo rotational Brownian motion, the nuclear spin relaxation processes are caused by time-dependent interactions involving the nuclear spins. For spin- nuclei, such as ¹³C (spin S), the most significant relaxation mechanisms often involve dipole–dipole (DD) interactions with neighbouring protons (spins I) and the anisotropic part of the shielding tensor (chemical shift anisotropy, CSA). The commonly used expression for the longitudinal relaxation rate constant reads (Canet, 1998):

where J_DD(ω) and J_CSA(ω) are dipolar and CSA spectral densities, respectively, taken at frequency ω. For rigid spherical-top molecules, these quantities are given by

and

with

and being interaction strengths for the DD and CSA relaxation mechanisms, respectively. γ denotes the nuclear magnetogyric ratio, B₀ the induction of the external magnetic field, r_IS the internuclear distance and τ_c the rotational correlation time. Δσ and η are called anisotropy and asymmetry of the shielding tensor. Both these quantities can be expressed in terms of the principal components σ_ii of the traceless part of the shielding anisotropy tensor:

with |σ₂₂| ≤ |σ₁₁| ≤ |σ₃₃|. Equation (2) describes the dipole–dipole relaxation in a rotating rigid body. It is not directly applicable to the case of the ¹³C nuclei in C₆₀ relaxed by remote protons of the hosting capsule because the rotational diffusion of C₆₀ leads to modulation of not only the direction of the internuclear vector but the length of the latter as well. Equations taking into account such modulations are available (Bernatowicz et al., 2006), but they were derived for systems involved in discrete internal motions of molecular fragments, with the latter dynamics being described by an exchange matrix. Such a matrix for C₆₀ tumbling in (3)₂ is unknown, so that even the advanced and flexible formalism of Bernatowicz et al. (2006) fails to describe the dipole–dipole mechanism for this system. Inspection of equation (2) reveals, however, some general features of the dipole–dipole mechanism which are of relevance to this work: (i) the contribution from the dipole–dipole mechanism decreases with the sixth power of the internuclear distance, so that even a large number of remote protons may not overwhelm the relaxation of the ¹³C nuclei in fullerene if they are far enough away and (ii) for motion fast enough (the so-called extreme narrowing regime, where ωτ_c ≪ 1), the contribution of the DD mechanism, in contrast to the CSA mechanism, is independent of induction of an external magnetic field. These two properties of the dipole–dipole relaxation process render it separable from that due to the field-dependent CSA mechanism. The latter seems to be faithfully described in model (3)₂C₆₀ by equation (3). The CSA mechanism should prevail over that of DD in appropriately high magnetic fields (due to its dependence on the squared strength of the external magnetic field). Thus, relaxation measurements performed at two (or more) suitably different magnetic fields enable evaluation of the contribution of the CSA mechanism with good accuracy. In order to exploit equation (3) for evaluation of the correlation time (τ_c) of the rotational tumbling of C₆₀, knowledge of the symmetric part of CSA in fullerene is required. The full shielding tensor was determined for solid fullerene (Yannoni et al., 1991) to be σ = (40, 186, 220) ppm, which corresponds to Δσ = −163.0 ppm and η = 0.31.

2.7. Differential scanning calorimetry (DSC) measurements

The phase transitions and thermal stability of the samples were studied using DSC. The DSC data were obtained using a Q200 scanning calorimeter (TA Instruments). Samples were placed in aluminium T_zero hermetic pans. An empty pan was used as a reference. Data analysis was carried out using the TA Universal Analysis application. Three cycles of cooling, heating and cooling at a rate of 10 K min⁻¹ for each scan in the temperature range from 90 to 355 K were carried out in a flow of nitro­gen.

3. Results and discussion

The X-ray crystal structure of (3)₂C₆₀ at 100 K was determined using synchrotron data. Despite the initially high R factor (∼24% for the isotropic model without dis­order), inspection of the electron-density map revealed that the fullerene molecule was clearly visible with pronounced, fairly well separated, peaks (Fig. 2a). Therefore, we undertook a tedious refinement procedure (described in detail in the Experimental section) involving the following crucial steps: (i) initial refinement of the structure in the low-symmetry space group I4 with a molecule of 3 located at the fourfold axis, noticing a mismatch of symmetry between the crystallographic fourfold symmetry and the C₂ molecular symmetry of C₆₀; (ii) location and modelling of two complete C₆₀ molecules with occupancy into the electron-density map at the position where the molecular twofold axis aligns with the crystallographic fourfold axis of this site; (iii) imposing of restrictions onto fullerene rotation during refinement; (iv) refinement in the higher-symmetry group I422. Finally, the refinement con­verged at R ≈ 9%. The ASU contains of the (3)₂C₆₀ complex. The host capsule (3)₂ resides at the site with 422 symmetry. The encapsulated C₆₀ molecule also resides at this site, but since it has only C₂ molecular symmetry in the [001] direction of its orientation, it generates a symmetry mismatch at this site, leading to discrete dis­order. This implies that the remaining symmetry operations at this 422 site (90° rotation about the fourfold axis and rotations about the diagonal twofold axis) generate C₆₀ copies in different orientations with respect to the host molecule (Figs. 2b, 2c and 2d). There are eight halves of the fullerene in the entire cell, which form four complete molecules. They constitute two pairs, rotated relative to each other around the twofold axis of C₆₀ (coinciding with the fourfold axis of the I422 space group) by an angle of 42.3°. The fullerene molecules forming a given pair are rotated by 90° relative to each other as a result of the action of the fourfold symmetry. The second pair is generated by twofold rotation perpendicular to the crystallographic c axis. However, considering the molecular 422 symmetry of the (3)₂ host, in fact, all possible arrangements are identical from a chemical point of view.

A detailed analysis of the molecular geometry and intermolecular contacts was carried out in CrystalExplorer (Fig. 3). The intramolecular distances were mapped on the molecular surface of C₆₀ (0.002 au electron-density isosurface). The C₆₀ guest is located close to the central part of the cavity but not at its geometric centre. The shift of C₆₀ from the geometric centre of the cavity is 0.012 Å in the direction of one of the resorcin[4]arene cups (Fig. 3a). It is important to note that the off-centre shift of C₆₀ results in different intermolecular interactions with the two hemispheres of the capsule that are clearly reflected in the maps. One (upper) hemisphere exhibits close contacts of the hydrazone C atoms of (3)₂ to C₆₀ (Figs. 3b, 3c and 3d); the closest distances are for C⋯C interactions of 3.15 and 3.21 Å, and the distances to the centroids of the resorcinol rings are longer. For the second (lower) hemisphere, the contacts are longer; the distances for C⋯C interactions are 3.40 and 3.46 Å, and the distances to the centroids of the resorcinol rings are similar.

Figure 3 Analysis of the intermolecular interactions. (a) van der Waals representation of C60 inside the cavity of (3)2 [(3)2 was sliced in order to visualize the interior of the cavity]. (b)–(d) Analysis of the intermolecular contacts by mapping of the intermolecular distances onto an C60 isosurface generated at 0.002 au electron density (as implemented in CrystalExplorer; Turner et al., 2017), with (3)2 shown in stick representation and C60 as the isosurface; the surface is colour-coded for host–guest contacts after subtraction of the sum of the van der Waals radii (red < 0, white = 0 and blue > 0). (b) A side view, (c) a 90° view of the upper hemisphere and (d) a 90° view of the bottom hemisphere.

Before considering the symmetry mismatch in the X-ray crystal structure of (3)₂C₆₀, the position and dynamics of the C₆₀ molecule were not clear. However, after the successful resolution of the crystal structure it can be concluded that at 100 K the molecule of C₆₀ is statistically but not thermally dis­ordered over discrete symmetry-equivalent positions. An analysis of the geometry indicates that, despite rather weak intramolecular interactions, the thermal motion of C₆₀ is frozen. In order to check the dynamics of C₆₀ over a wider temperature range, we used solid-state ¹³C NMR. The ¹³C longitudinal relaxation times of fullerene C₆₀ in complex (3)₂C₆₀ were determined in the temperature range 184–333 K at two magnetic field strengths, i.e. 7.04 and 11.73 T. Although the theory for the calculation of thermal-motion parameters from these NMR data is well elaborated, in this case, the analysis proved to be more complex than initially anticipated. It was complicated by the time-dependent changes ongoing in the solid state and biased by the rather unexpected interactions with atmospheric oxygen or water. Below, we present a detailed analysis of these problems which, after appropriate compensation, allowed us to obtain correct dynamic parameters for C₆₀.

The sample for NMR measurements was obtained by vacuum drying of (3)₂C₆₀ (amorphous solid obtained after synthesis), which was subsequently ground, mixed with ground lead nitrate, packed into a zirconia NMR rotor and hermetically sealed. The Arrhenius plot of the relaxation data in the range 298–184 K at 11.73 T is shown in Fig. 4(a) (solid squares). The data reveal non-linearity over the whole temperature range, indicating that the thermal motion of C₆₀ has different activation energies under different temperature regimes. The data were fitted with two lines: one with an activation energy of E_a = 5.57 ± 0.30 kJ mol⁻¹ in the temperature range 298–240 K and the other with an activation energy of E_a = 8.28 ± 0.65 kJ mol⁻¹ in the temperature range 223–184 K. The data for the intermediate temperature range (236–232 K; open squares in Fig. 4a) and above 298 K depart significantly from both of these trends, likely indicating phase transitions. In order to detect these phase transitions, the DSC method was employed, which indeed confirmed the high-temperature phase transition (above 298 K; Figs. 4b and 4c). However, no phase transition was detected at lower temperatures. In order to validate the above NMR data, we remeasured the sample using a different machine (7.04 T), which should eliminate incident sample-independent errors and enable separation of different relaxation mechanisms. The Arrhenius fit in the temperature range 298–248 K delivers E_a = 5.32 ± 0.31 kJ mol⁻¹, which is consistent with the data measured at 11.73 T (solid circles in Fig. 4a). However, the data below 248 K (open circles in Fig. 4) are distinctly different from this fit and also from the data measured previously at 11.73 T. The Arrhenius fit in this range yields E_a = 3.43 ± 0.29 kJ mol⁻¹. It should be noted here that although the experiments were carried out for the same sample, they were not recorded at the same time; during the time lapse between the experiments, the sample spent a few months in contact with humid air. Although the chemical formula did not change during this time (as confirmed by solution NMR), apparently some structural changes in the solid sample did occur which were ultimately reflected in the fullerene rotational mobility and, in consequence, in the rates of its spin-relaxation processes. The DSC profiles recorded for the same sample before and after `aging' (of 12 months) also reveal structural changes and substantial differences in the characteristics of the phase transition. The phase transition for the sample before aging is diffused between 298 and 333 K, while after aging a very sharp peak at ∼300 K was found (see Fig. 4c).

Figure 4 (a) Arrhenius plots of the relaxation data for the ^13C NMR signal of C60 in (3)2C60 (7.04 and 11.73 T). (b) Differential scanning calorimetry (DSC) curve for sample (3)2C60, measured eight months after crystallization. (c) Comparison of a fragment of the DSC curves for sample (3)2C60 measured at eight and 20 months after crystallization.

A similar slope of the Arrhenius fits in the range 248–298 K for data measured at different magnetic fields enables separation of the contributions from different spin-relaxation mechanisms within this temperature range (Canet, 1998). Specifically, we can exploit the fact that within the so-called extreme narrowing regime, the CSA contribution to spin relaxation is field dependent, while other contributions (comprising the DD mechanism to other nuclei and/or the DD mechanism to unpaired electrons) are not [see equations (2) and (3)]. The obtained contributions are listed in Table 2. Based on these contributions and using the components of the known fullerene CSA tensor (Yannoni et al., 1991), the application of Equation (3) enables a straightforward determination of the rotational correlation times, τ_c, of fullerene and, in consequence, its rotational diffusion coefficient D = (6τ_c)⁻¹. The latter quantities are also listed in Table 2. The Arrhenius plot of D is shown in Fig. 5(a). The activation energy obtained from this plot is E_a = 6.25 kJ mol⁻¹, while the pre-exponential factor is D₀ = 3.36 × 10¹¹ s⁻¹. Our results for C₆₀ tumbling inside the supramolecular capsule (3)₂ agree surprisingly well with similar data determined via NMR spectroscopy (Johnson et al., 1992) and QENS (Quasi Elastic Neutron Scattering) (Neumann et al., 1991) for neat C₆₀. We performed investigations similar to Johnson et al. (1992), i.e. a multiple-field NMR relaxation study, in order to separate spin relaxation induced by CSA from those induced by other mechanisms. They obtained E_a = 5.85 ± 0.42 kJ mol⁻¹, D₀ = 2.06 × 10¹¹ s⁻¹ and D = 1.8 × 10¹⁰ s⁻¹ at 283 K, while the QENS technique delivered a slightly lower E_a = 3.38 ± 1.45 kJ mol⁻¹ and D = 1.4 × 10¹⁰ s⁻¹ at 260 K (Neumann et al., 1991). More recently, very careful investigations of C₆₀ dynamics by NMR spectroscopy in the solid state were performed by Izotov & Tarasov (2002).

Table 2
Contributions of various relaxation mechanisms to spin-relaxation rates R1 = T1⁻¹ of ¹³C nuclei in C₆₀ at 7.04 and 11.73 T, and rotational diffusion coefficients, D = (6τ_c)⁻¹, determined from CSA relaxation rates as a function of temperature

T (K)	R1CSA at 7.04 T (10^−2 s^−1)	R1CSA at 11.73 T (10^−2 s^−1)	R1other (10^−2 s^−1)	D (10^10 s^−1)
298	0.51	1.40	1.96	2.69
288	0.55	1.53	2.10	2.47
278	0.61	1.68	2.27	2.24
267	0.67	1.85	2.46	2.03
258	0.75	2.07	2.69	1.82
248	0.84	2.32	2.96	1.62

Figure 5 (a) Arrhenius plot of the rotational diffusion coefficient, D, of C60 in (3)2C60 obtained from the CSA relaxation data listed in Table 2. The activation energy is Ea = 6.25 kJ mol^−1, while the pre-exponential factor was D0 = 3.36 × 10^11 s^−1. (b) EPR spectrum of the `off-the-shelf' C60 (upper panel; material exploited in the synthesis of the complex) and EPR spectrum of complex (3)2C60 (lower panel).

In conclusion, it appears that the activation energy for reorientations of free and encaged C₆₀ in the solid state is very similar. Also, the rotational diffusion coefficients seem to be very similar or even slightly higher for the encaged fullerene as compared to the free molecule. Table 2 also reveals that CSA is not the main relaxation mechanism for ¹³C spins of C₆₀ fullerene in (3)₂C₆₀, even in a magnetic field of 11.7 T. This points to a surprisingly high contribution of non-CSA mechanisms, taking into account that for neat fullerene at 11.7 T only about 10% of its relaxation comes from mechanisms other than CSA [see Fig. 2 in Johnson et al. (1992)]. A possible explanation for this large amount of non-CSA relaxation usually involves internuclear dipole–dipole interactions. However, the X-ray crystal structure of (3)₂C₆₀ reveals that there are no protons approaching the encaged C₆₀ molecule at distances shorter than ∼2.95 Å, which would correspond to ¹³C–¹H dipole–dipole coupling of only 1.2 kHz. Such couplings have a negligible impact on the ¹³C spin relaxation in C₆₀. An alternative explanation for the high contribution of non-CSA mechanisms to relaxation may come from dipole–dipole interaction with unpaired electrons. We acquired Electron Paramagnetic Resonance (EPR) spectra of the C₆₀ sample used in the synthesis (off-the-shelf sample) and of (3)₂C₆₀ (Fig. 5b). The EPR spectrum of `off-the-shelf' C<sub>60</sub> shows pronounced EPR effects. It has been demonstrated previously that although C<sub>60</sub> itself is not paramagnetic, its derivatives obtained by reactions with molecular oxygen from the air are (Paul et al., 2002). We assume that this effect is also reflected in the spectrum of the `off-the-shelf' C₆₀ sample. The EPR effects for (3)₂C₆₀ are much smaller but certainly not negligible. Electronic paramagnetism detected in the sample can be responsible for the observed high non-CSA contributions to relaxation. It should be noted that in Johnson et al. (1992), which describes ¹³C relaxation experiments on neat C₆₀, similar problems with intensive paramagnetic relaxation were not reported. However, in the cited study, in the course of the sample preparation, C₆₀ was extracted with supercritical CO₂ and the obtained material was sealed under vacuum, so that the sample was protected against the impact of oxygen.

4. Conclusions and outlook

We have described the synthesis of a molecular container formed by zipping together two resorcin[4]arene hemispheres via a system of circular β-sheet hydrogen bonds between their peptidic arms. The container, with a largely hydro­philic inner surface, has been loaded with C₆₀ fullerene and crystallized. The crystal structure studied at 100 K using synchrotron radiation reveals that the complex occupies the 422 site of the space group I422, which is compatible with the molecular symmetry of the container but not of the C₆₀ molecule, leading to its discrete dis­order. Resolving a fourfold dis­order of a fullerene molecule in the electron-density maps is quite a challenge, but it could be completed successfully, as confirmed by the final electron-density maps, and the convergent and stable least-squares refinement carried out using the advanced features available in the SHELXL program. We hope that our success and example will encourage other crystallographers to attack similar problems which at first glance appear to be intractable. The crystallographic study has been supplemented by solid-state NMR experiments over the temperature range 184–333 K, carried out for both fresh and aged samples, and using spectrometers with different magnetic field strengths (7.04 and 11.73 T). It appears that the activation energy for reorientations of free and encaged C₆₀ in the solid state is very similar. Also, the rotational diffusion coefficients seem to be very similar or even slightly higher for the encaged fullerene compared to the free one. The NMR results also show time-dependent phase transitions in the sample, confirmed at higher temperature by DSC experiments that also affect the activation energy for reorientations. A detailed study of this phase transition and an X-ray crystal structure determination of the high-temperature phase are the subject of an ongoing project.

Supporting information

Computing details

Program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2018).

(I)

Crystal data

C260H264N24O40	Dx = 1.187 Mg m^−3
Mr = 4365.00	Synchrotron radiation, λ = 0.8266 Å
Tetragonal, I422	Cell parameters from 5405 reflections
a = 21.91 (2) Å	θ = 1.4–29.6°
c = 25.44 (3) Å	µ = 0.11 mm^−1
V = 12212 (27) Å^3	T = 100 K
Z = 2	Prism, orange
F(000) = 4624

Data collection

MD3_Microdiffractometer	5281 reflections with I > 2σ(I)
Radiation source: synchrotron	Rint = 0.048
Detector resolution: 13.3 pixels mm^-1	θmax = 29.6°, θmin = 1.4°
rotation scans	h = −24→26
31450 measured reflections	k = −25→25
5405 independent reflections	l = −30→30

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.085	w = 1/[σ^2(Fo^2) + (0.1753P)^2 + 10.7774P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.259	(Δ/σ)max < 0.001
S = 1.12	Δρmax = 1.49 e Å^−3
5405 reflections	Δρmin = −0.34 e Å^−3
660 parameters	Absolute structure: Flack x determined using 2276 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
1669 restraints	Absolute structure parameter: −0.05 (14)

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C101	0.3187 (5)	0.4580 (5)	0.0588 (3)	0.078 (3)	0.695 (11)
H1A	0.350137	0.488478	0.058145	0.117*	0.695 (11)
H1B	0.331454	0.423206	0.038694	0.117*	0.695 (11)
H1C	0.281943	0.474506	0.043896	0.117*	0.695 (11)
C102	0.2568 (5)	0.3905 (5)	0.1160 (4)	0.075 (3)	0.695 (11)
H2A	0.249428	0.378492	0.151682	0.113*	0.695 (11)
H2B	0.220058	0.406956	0.101120	0.113*	0.695 (11)
H2C	0.269570	0.355657	0.095918	0.113*	0.695 (11)
C103	0.3068 (4)	0.4390 (3)	0.1146 (3)	0.056 (2)	0.695 (11)
H3	0.292460	0.474695	0.134228	0.067*	0.695 (11)
C104	0.3640 (5)	0.4148 (5)	0.1416 (3)	0.047 (2)	0.695 (11)
H4A	0.370943	0.372802	0.130965	0.056*	0.695 (11)
H4B	0.399042	0.438717	0.130593	0.056*	0.695 (11)
C201	0.3538 (10)	0.3902 (9)	0.0480 (7)	0.059 (5)	0.305 (11)
HAA	0.348654	0.353302	0.028155	0.088*	0.305 (11)
H1BA	0.323137	0.419211	0.037759	0.088*	0.305 (11)
H1CA	0.393504	0.406920	0.041305	0.088*	0.305 (11)
C202	0.2861 (8)	0.3453 (8)	0.1180 (8)	0.056 (5)	0.305 (11)
H2AA	0.284059	0.307719	0.098777	0.083*	0.305 (11)
H2BA	0.281942	0.337106	0.154933	0.083*	0.305 (11)
H2CA	0.253759	0.371857	0.106846	0.083*	0.305 (11)
C203	0.3472 (8)	0.3759 (7)	0.1079 (6)	0.047 (4)	0.305 (11)
H3A	0.379918	0.347947	0.118345	0.056*	0.305 (11)
C204	0.3561 (13)	0.4382 (12)	0.1374 (10)	0.050 (5)	0.305 (11)
H4AA	0.322405	0.465751	0.130360	0.059*	0.305 (11)
H4BA	0.393943	0.457670	0.127058	0.059*	0.305 (11)
C105	0.3577 (2)	0.4179 (3)	0.20122 (18)	0.0540 (13)
H5	0.320254	0.395977	0.210425	0.065*
C106	0.3531 (2)	0.4807 (2)	0.22559 (18)	0.0473 (11)
C107	0.3861 (2)	0.5301 (2)	0.20558 (17)	0.0470 (11)
H7	0.412073	0.523148	0.177274	0.056*
C108	0.3823 (2)	0.5890 (2)	0.22562 (18)	0.0496 (12)
C109	0.3445 (2)	0.5978 (3)	0.26897 (19)	0.0514 (12)
C110	0.3105 (2)	0.5500 (3)	0.29097 (19)	0.0533 (12)
C111	0.3152 (2)	0.4916 (3)	0.26847 (17)	0.0511 (11)
O12	0.28113 (18)	0.4466 (2)	0.29097 (14)	0.0607 (11)
H12	0.286569	0.414511	0.275068	0.091*
O13	0.3407 (2)	0.6550 (2)	0.29058 (13)	0.0609 (10)
H13	0.317046	0.654389	0.315527	0.091*
C114	0.2706 (2)	0.5580 (3)	0.33552 (19)	0.0536 (12)
H14	0.247162	0.525255	0.347141	0.064*
N15	0.2666 (2)	0.6098 (3)	0.35961 (17)	0.0584 (12)
N16	0.2258 (2)	0.6116 (2)	0.40030 (17)	0.0558 (12)
H16	0.200140	0.582285	0.404435	0.067*
C121	0.1838 (3)	0.6237 (3)	0.5637 (2)	0.0657 (15)
C122	0.2176 (3)	0.6268 (4)	0.6149 (3)	0.0746 (18)
H22A	0.249622	0.656590	0.612305	0.112*
H22B	0.189896	0.638335	0.642376	0.112*
H22C	0.234867	0.587615	0.622650	0.112*
O23	0.1404 (2)	0.5881 (3)	0.5582 (2)	0.0901 (17)
C	0.2255 (3)	0.6587 (3)	0.4336 (2)	0.0594 (14)
O	0.2620 (2)	0.7004 (2)	0.43294 (16)	0.0730 (13)
CA	0.1746 (3)	0.6570 (3)	0.4740 (2)	0.0584 (14)
HA	0.155478	0.616737	0.470871	0.070*
N	0.2017 (2)	0.6594 (2)	0.52559 (17)	0.0579 (12)
H0	0.230432	0.685248	0.531493	0.069*
CBA	0.1236 (12)	0.7035 (12)	0.4694 (9)	0.058 (5)	0.51 (2)
HB1A	0.097003	0.698710	0.499631	0.069*	0.51 (2)
HB2A	0.141525	0.743891	0.471578	0.069*	0.51 (2)
CGA	0.0857 (7)	0.7009 (9)	0.4217 (7)	0.060 (4)	0.51 (2)
CD2A	0.1061 (8)	0.7197 (8)	0.3730 (7)	0.065 (3)	0.51 (2)
HD2A	0.144696	0.736954	0.369705	0.077*	0.51 (2)
CE2A	0.0683 (8)	0.7127 (8)	0.3277 (7)	0.073 (4)	0.51 (2)
HE2A	0.081305	0.727078	0.295196	0.088*	0.51 (2)
CZA	0.0149 (10)	0.6858 (8)	0.3322 (8)	0.082 (5)	0.51 (2)
HZA	−0.008252	0.679012	0.302057	0.099*	0.51 (2)
CE1A	−0.0085 (8)	0.6668 (9)	0.3812 (8)	0.099 (6)	0.51 (2)
HE1A	−0.048055	0.651763	0.384085	0.118*	0.51 (2)
CD1A	0.0305 (7)	0.6713 (10)	0.4269 (7)	0.082 (4)	0.51 (2)
HD1A	0.018740	0.654579	0.458973	0.098*	0.51 (2)
CB	0.1351 (11)	0.7166 (14)	0.4606 (11)	0.055 (5)	0.49 (2)
HB1	0.102963	0.721915	0.486384	0.066*	0.49 (2)
HB2	0.160864	0.752603	0.460946	0.066*	0.49 (2)
CG	0.1076 (10)	0.7071 (8)	0.4055 (9)	0.061 (4)	0.49 (2)
CD2	0.1388 (12)	0.7301 (7)	0.3613 (7)	0.073 (4)	0.49 (2)
HD2	0.175226	0.751030	0.366674	0.088*	0.49 (2)
CE2	0.1184 (12)	0.7233 (7)	0.3118 (7)	0.095 (6)	0.49 (2)
HE2	0.140504	0.738635	0.283564	0.114*	0.49 (2)
CZ	0.0633 (16)	0.6926 (8)	0.3038 (10)	0.110 (8)	0.49 (2)
HZ	0.047853	0.687938	0.269978	0.132*	0.49 (2)
CE1	0.0321 (14)	0.6691 (9)	0.3462 (10)	0.105 (7)	0.49 (2)
HE1	−0.003870	0.647597	0.340361	0.125*	0.49 (2)
CD1	0.0527 (9)	0.6768 (7)	0.3980 (9)	0.080 (5)	0.49 (2)
HD1	0.030339	0.662049	0.426297	0.096*	0.49 (2)
C303	0.0975 (10)	0.5085 (15)	0.6908 (6)	0.238 (12)
H33A	0.063626	0.497950	0.712906	0.358*
H33B	0.134989	0.500923	0.709246	0.358*
H33C	0.095123	0.550900	0.681571	0.358*
O301	0.1399 (2)	0.4794 (3)	0.6066 (2)	0.0858 (16)
H301	0.122702	0.482530	0.578091	0.129*
C302	0.0959 (7)	0.4743 (6)	0.6467 (7)	0.157 (6)
H32A	0.096073	0.431956	0.657902	0.188*
H32B	0.056523	0.481537	0.630447	0.188*
C3	0.3523 (16)	0.4355 (10)	0.5284 (5)	0.058 (8)	0.25
C4	0.4237 (10)	0.5379 (8)	0.6186 (5)	0.057 (5)	0.25
C5	0.4862 (10)	0.5289 (12)	0.6370 (11)	0.067 (8)	0.25
C11	0.3532 (13)	0.4362 (10)	0.4719 (5)	0.046 (8)	0.25
C13	0.4210 (8)	0.5948 (8)	0.5901 (5)	0.054 (5)	0.25
C14	0.3484 (11)	0.5482 (8)	0.4719 (5)	0.051 (5)	0.25
C15	0.3514 (13)	0.4936 (9)	0.4440 (6)	0.059 (8)	0.25
C16	0.5219 (8)	0.5805 (11)	0.6186 (5)	0.068 (7)	0.25
C17	0.4818 (7)	0.6213 (10)	0.5901 (5)	0.060 (5)	0.25
C20	0.3846 (8)	0.6000 (8)	0.4545 (5)	0.045 (4)	0.25
C21	0.4069 (6)	0.6323 (7)	0.5004 (5)	0.057 (4)	0.25
C23	0.3894 (13)	0.4886 (8)	0.3977 (7)	0.049 (6)	0.25
C25	0.5819 (10)	0.5718 (13)	0.6021 (7)	0.057 (7)	0.25
C26	0.4653 (6)	0.6572 (7)	0.5004 (5)	0.054 (3)	0.25
C27	0.5040 (8)	0.6513 (11)	0.5461 (5)	0.058 (8)	0.25
C28	0.4246 (9)	0.5382 (7)	0.3813 (5)	0.046 (5)	0.25
C29	0.4216 (8)	0.5950 (8)	0.4101 (5)	0.058 (7)	0.25
C34	0.6053 (11)	0.6034 (14)	0.5561 (7)	0.061 (9)	0.25
C35	0.5662 (8)	0.6419 (14)	0.5284 (5)	0.053 (7)	0.25
C39	0.4870 (10)	0.5285 (9)	0.3635 (10)	0.051 (6)	0.25
C40	0.4826 (7)	0.6211 (9)	0.4101 (5)	0.052 (5)	0.25
C41	0.5044 (8)	0.6507 (10)	0.4545 (5)	0.058 (7)	0.25
C42	0.5228 (8)	0.5803 (10)	0.3813 (5)	0.056 (5)	0.25
C44	0.3836 (9)	0.6003 (8)	0.5461 (5)	0.057 (6)	0.25
C45	0.3487 (12)	0.5479 (9)	0.5284 (5)	0.061 (7)	0.25
C46	0.3512 (14)	0.4930 (9)	0.5561 (7)	0.051 (6)	0.25
C47	0.3895 (13)	0.4882 (9)	0.6021 (7)	0.058 (7)	0.25
C51	0.5665 (8)	0.6417 (12)	0.4719 (5)	0.055 (5)	0.25
C52	0.5829 (9)	0.5722 (11)	0.3977 (7)	0.048 (5)	0.25
C53	0.6057 (11)	0.6033 (12)	0.4440 (6)	0.051 (6)	0.25

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C101	0.100 (7)	0.086 (6)	0.049 (4)	−0.015 (5)	−0.025 (4)	0.018 (4)
C102	0.097 (7)	0.068 (6)	0.060 (5)	−0.024 (5)	−0.037 (5)	0.003 (4)
C103	0.073 (5)	0.058 (4)	0.036 (3)	−0.004 (3)	−0.022 (3)	−0.003 (3)
C104	0.068 (5)	0.043 (5)	0.028 (3)	−0.014 (5)	−0.006 (3)	−0.005 (4)
C201	0.079 (12)	0.054 (9)	0.043 (7)	−0.003 (8)	−0.005 (7)	−0.017 (6)
C202	0.055 (9)	0.047 (9)	0.065 (10)	−0.006 (7)	−0.008 (7)	−0.014 (8)
C203	0.055 (8)	0.043 (7)	0.042 (7)	0.004 (6)	−0.003 (6)	−0.017 (6)
C204	0.071 (13)	0.044 (11)	0.034 (6)	−0.005 (9)	0.001 (8)	−0.011 (7)
C105	0.055 (3)	0.076 (3)	0.031 (2)	−0.018 (2)	0.0011 (19)	−0.014 (2)
C106	0.039 (2)	0.071 (3)	0.032 (2)	−0.0014 (19)	−0.0092 (17)	−0.0102 (19)
C107	0.045 (2)	0.068 (3)	0.029 (2)	0.003 (2)	−0.0095 (18)	−0.0087 (19)
C108	0.051 (2)	0.064 (3)	0.034 (2)	0.009 (2)	−0.0161 (18)	−0.007 (2)
C109	0.049 (2)	0.067 (3)	0.037 (2)	0.017 (2)	−0.0170 (19)	−0.014 (2)
C110	0.044 (2)	0.082 (3)	0.034 (2)	0.008 (2)	−0.0123 (18)	−0.012 (2)
C111	0.045 (2)	0.074 (3)	0.034 (2)	0.001 (2)	−0.0119 (18)	−0.011 (2)
O12	0.054 (2)	0.082 (3)	0.0454 (19)	−0.0129 (18)	0.0035 (16)	−0.0128 (18)
O13	0.065 (2)	0.073 (2)	0.0444 (18)	0.0173 (18)	−0.0119 (17)	−0.0185 (18)
C114	0.046 (2)	0.076 (3)	0.039 (2)	0.013 (2)	−0.0117 (19)	−0.012 (2)
N15	0.048 (2)	0.090 (3)	0.037 (2)	0.017 (2)	−0.0103 (17)	−0.018 (2)
N16	0.047 (2)	0.080 (3)	0.041 (2)	0.013 (2)	−0.0066 (17)	−0.016 (2)
C121	0.050 (3)	0.093 (4)	0.054 (3)	0.008 (3)	−0.012 (2)	−0.011 (3)
C122	0.067 (4)	0.101 (5)	0.055 (3)	−0.001 (3)	−0.022 (3)	0.006 (3)
O23	0.070 (3)	0.134 (4)	0.066 (3)	−0.018 (3)	−0.019 (2)	−0.001 (3)
C	0.050 (3)	0.086 (4)	0.042 (3)	0.016 (3)	−0.013 (2)	−0.019 (3)
O	0.080 (3)	0.089 (3)	0.050 (2)	−0.004 (2)	−0.005 (2)	−0.021 (2)
CA	0.052 (3)	0.080 (4)	0.043 (2)	0.019 (3)	−0.010 (2)	−0.019 (2)
N	0.050 (2)	0.082 (3)	0.041 (2)	0.018 (2)	−0.0088 (17)	−0.018 (2)
CBA	0.060 (9)	0.066 (13)	0.047 (7)	0.015 (8)	−0.005 (6)	−0.013 (7)
CGA	0.048 (6)	0.078 (9)	0.053 (7)	0.017 (6)	−0.004 (5)	−0.002 (6)
CD2A	0.057 (7)	0.084 (9)	0.052 (7)	0.002 (6)	−0.004 (5)	−0.004 (6)
CE2A	0.096 (9)	0.064 (8)	0.061 (7)	−0.003 (7)	−0.026 (7)	0.015 (7)
CZA	0.101 (11)	0.069 (9)	0.078 (8)	−0.014 (8)	−0.054 (8)	0.016 (7)
CE1A	0.059 (8)	0.123 (13)	0.114 (11)	−0.019 (8)	−0.034 (7)	0.046 (10)
CD1A	0.058 (7)	0.121 (12)	0.067 (8)	0.006 (6)	−0.002 (6)	0.015 (8)
CB	0.043 (8)	0.067 (11)	0.056 (8)	0.005 (6)	−0.003 (6)	−0.002 (7)
CG	0.072 (10)	0.049 (7)	0.061 (8)	0.020 (6)	−0.021 (7)	−0.006 (6)
CD2	0.103 (12)	0.053 (7)	0.063 (7)	0.025 (7)	−0.014 (7)	0.006 (5)
CE2	0.154 (16)	0.065 (8)	0.065 (7)	0.029 (9)	−0.025 (9)	0.013 (6)
CZ	0.19 (2)	0.050 (8)	0.088 (10)	0.016 (9)	−0.072 (12)	0.002 (8)
CE1	0.138 (16)	0.066 (11)	0.110 (12)	0.002 (10)	−0.080 (11)	0.010 (9)
CD1	0.074 (9)	0.072 (8)	0.095 (10)	0.011 (6)	−0.046 (8)	0.004 (8)
C303	0.205 (18)	0.39 (3)	0.117 (10)	0.04 (2)	0.067 (12)	−0.057 (15)
O301	0.061 (2)	0.118 (4)	0.078 (3)	−0.003 (3)	0.020 (2)	−0.024 (3)
C302	0.149 (10)	0.116 (8)	0.205 (13)	−0.025 (7)	0.117 (10)	−0.036 (8)
C3	0.04 (2)	0.072 (13)	0.061 (9)	0.005 (14)	−0.001 (13)	−0.017 (11)
C4	0.059 (9)	0.064 (13)	0.047 (15)	0.019 (9)	0.014 (10)	−0.017 (8)
C5	0.062 (12)	0.11 (2)	0.025 (19)	0.014 (13)	0.011 (11)	0.000 (13)
C11	0.03 (2)	0.051 (9)	0.063 (9)	−0.011 (13)	−0.002 (12)	−0.017 (10)
C13	0.065 (10)	0.057 (12)	0.041 (9)	0.012 (9)	0.010 (8)	−0.024 (8)
C14	0.051 (15)	0.051 (9)	0.050 (8)	0.008 (8)	−0.001 (9)	−0.004 (7)
C15	0.05 (2)	0.055 (9)	0.070 (13)	−0.009 (11)	0.002 (13)	−0.013 (7)
C16	0.071 (9)	0.11 (2)	0.025 (13)	−0.003 (10)	−0.009 (9)	−0.022 (11)
C17	0.074 (9)	0.061 (13)	0.044 (9)	0.002 (8)	0.003 (8)	−0.035 (9)
C20	0.036 (9)	0.036 (9)	0.063 (7)	0.024 (7)	−0.004 (7)	0.001 (7)
C21	0.060 (8)	0.043 (9)	0.067 (7)	0.006 (7)	−0.002 (8)	0.000 (7)
C23	0.056 (15)	0.040 (11)	0.052 (13)	−0.001 (11)	−0.011 (11)	−0.014 (9)
C25	0.071 (12)	0.042 (17)	0.057 (17)	−0.007 (11)	−0.002 (13)	−0.016 (11)
C26	0.062 (8)	0.032 (9)	0.069 (8)	0.004 (7)	0.002 (7)	−0.001 (9)
C27	0.072 (10)	0.04 (2)	0.064 (7)	−0.005 (10)	−0.001 (7)	−0.026 (12)
C28	0.055 (10)	0.040 (11)	0.042 (13)	0.010 (9)	−0.009 (9)	0.000 (8)
C29	0.064 (11)	0.041 (15)	0.070 (11)	0.005 (10)	0.011 (10)	−0.004 (10)
C34	0.070 (19)	0.043 (17)	0.070 (16)	−0.006 (17)	0.000 (13)	−0.002 (14)
C35	0.065 (10)	0.020 (17)	0.075 (9)	−0.016 (14)	−0.002 (9)	−0.009 (10)
C39	0.061 (11)	0.071 (14)	0.021 (17)	0.015 (10)	0.003 (11)	0.011 (10)
C40	0.064 (9)	0.039 (11)	0.054 (10)	0.008 (8)	0.004 (8)	0.027 (8)
C41	0.073 (10)	0.03 (2)	0.067 (8)	−0.003 (10)	0.007 (8)	0.018 (12)
C42	0.064 (9)	0.064 (13)	0.040 (13)	0.004 (8)	0.014 (9)	0.027 (10)
C44	0.059 (14)	0.055 (12)	0.057 (7)	0.002 (10)	0.006 (8)	−0.011 (9)
C45	0.065 (19)	0.062 (12)	0.056 (8)	−0.008 (10)	0.003 (10)	−0.005 (7)
C46	0.042 (16)	0.065 (10)	0.045 (10)	−0.002 (11)	0.026 (9)	−0.003 (7)
C47	0.072 (19)	0.067 (13)	0.035 (11)	0.005 (13)	0.021 (11)	−0.011 (10)
C51	0.064 (9)	0.029 (13)	0.072 (9)	−0.022 (11)	0.010 (8)	0.014 (10)
C52	0.055 (10)	0.038 (14)	0.050 (14)	−0.006 (9)	0.022 (10)	0.030 (8)
C53	0.062 (15)	0.032 (13)	0.059 (13)	−0.016 (11)	0.015 (10)	0.030 (9)

Geometric parameters (Å, º)

C101—C103	1.503 (9)	C15—C46^iii	0.29 (3)
C102—C103	1.525 (9)	C15—C41^i	0.36 (2)
C103—C104	1.523 (10)	C15—C40^i	1.08 (2)
C104—C105	1.526 (10)	C15—C45^iii	1.15 (3)
C201—C203	1.56 (2)	C15—C17^ii	1.18 (2)
C202—C203	1.52 (2)	C15—C23	1.446 (12)
C203—C204	1.57 (3)	C15—C47^iii	1.49 (3)
C204—C105	1.68 (3)	C15—C35^ii	1.49 (3)
C105—C106	1.512 (8)	C15—C26^i	1.574 (19)
C105—C108^i	1.535 (8)	C16—C23^ii	0.81 (3)
C106—C107	1.398 (8)	C16—C42^v	0.98 (2)
C106—C111	1.392 (7)	C16—C47^vi	1.08 (3)
C107—C108	1.390 (8)	C16—C39^v	1.24 (3)
C108—C109	1.393 (7)	C16—C28^ii	1.32 (3)
C109—O13	1.371 (7)	C16—C40^v	1.15 (3)
C109—C110	1.403 (9)	C16—C52^vii	1.18 (3)
C110—C111	1.406 (8)	C16—C25	1.393 (13)
C110—C114	1.443 (7)	C16—C17	1.449 (12)
C111—O12	1.362 (7)	C17—C47^vi	0.41 (3)
C114—N15	1.293 (8)	C17—C23^ii	0.76 (2)
N15—N16	1.369 (7)	C17—C40^v	0.78 (2)
N16—C	1.335 (7)	C17—C46^vi	1.08 (3)
C121—O23	1.238 (9)	C17—C42^v	1.16 (3)
C121—N	1.305 (9)	C17—C28^ii	1.32 (2)
C121—C122	1.500 (8)	C17—C41^v	1.34 (2)
C—O	1.215 (8)	C17—C27	1.385 (11)
C—CA	1.516 (8)	C17—C25^i	1.49 (3)
CA—N	1.442 (6)	C20—C34^v	0.36 (2)
CA—CBA	1.52 (3)	C20—C53^i	0.40 (2)
CA—CB	1.60 (3)	C20—C44^ii	0.49 (3)
CBA—CGA	1.47 (3)	C20—C51^i	1.03 (2)
CGA—CD1A	1.38 (2)	C20—C21^ii	1.22 (2)
CGA—CD2A	1.38 (2)	C20—C29	1.395 (9)
CD2A—CE2A	1.43 (2)	C20—C21	1.451 (11)
CE2A—CZA	1.32 (3)	C20—C35^v	1.48 (3)
CZA—CE1A	1.41 (3)	C21—C51^v	0.94 (2)
CE1A—CD1A	1.45 (2)	C21—C35^v	0.96 (2)
CB—CG	1.54 (3)	C21—C21^ii	1.21 (3)
CG—CD2	1.41 (3)	C21—C44^ii	1.24 (2)
CG—CD1	1.39 (3)	C21—C45^ii	1.30 (2)
CD2—CE2	1.34 (2)	C21—C26	1.391 (12)
CE2—CZ	1.40 (4)	C21—C44	1.452 (11)
CZ—CE1	1.38 (4)	C23—C47^iii	0.51 (2)
CE1—CD1	1.40 (3)	C23—C40^i	0.41 (2)
C303—C302	1.35 (2)	C23—C42^i	1.08 (3)
O301—C302	1.408 (12)	C23—C28	1.396 (12)
C3—C51^ii	0.14 (5)	C23—C46^iii	1.50 (3)
C3—C14^iii	0.37 (3)	C23—C52^iv	1.46 (3)
C3—C26^i	0.99 (2)	C23—C29^i	1.54 (3)
C3—C21^i	1.01 (2)	C23—C27^ii	1.69 (2)
C3—C20^iii	1.14 (4)	C25—C52^vii	0.32 (3)
C3—C41^ii	1.39 (3)	C25—C29^v	0.60 (3)
C3—C46	1.444 (13)	C25—C28^v	0.86 (3)
C3—C35^ii	1.45 (3)	C25—C42^vii	1.16 (3)
C3—C11	1.439 (7)	C25—C53^vii	1.46 (3)
C3—C34^iv	1.44 (3)	C25—C47^iv	1.46 (3)
C3—C45^iii	1.49 (3)	C25—C34	1.451 (13)
C3—C53^ii	1.50 (4)	C26—C45^ii	0.80 (2)
C4—C16^i	0.36 (3)	C26—C51^v	1.05 (2)
C4—C52^v	0.87 (3)	C26—C35^v	1.06 (2)
C4—C25^i	1.06 (3)	C26—C41^v	1.33 (2)
C4—C23^iii	1.04 (3)	C26—C27^v	1.37 (2)
C4—C39^ii	1.27 (3)	C26—C27	1.446 (11)
C4—C28^ii	1.17 (2)	C26—C41	1.455 (11)
C4—C29^ii	1.22 (2)	C26—C26^v	1.52 (3)
C4—C47	1.388 (13)	C27—C41^v	0.18 (3)
C4—C40^ii	1.30 (2)	C27—C46^vi	0.35 (2)
C4—C42^ii	1.33 (3)	C27—C45^vi	1.06 (2)
C4—C5	1.460 (13)	C27—C40^v	1.33 (2)
C4—C13	1.444 (12)	C27—C35	1.449 (12)
C5—C39^ii	0.47 (3)	C28—C42^i	0.35 (2)
C5—C39^v	0.59 (2)	C28—C47^iii	1.05 (3)
C5—C5^i	0.99 (3)	C28—C52^i	1.07 (2)
C5—C5^vi	0.99 (3)	C28—C39^i	1.59 (3)
C5—C28^ii	1.24 (3)	C28—C39	1.456 (13)
C5—C39^iii	1.26 (3)	C29—C52^i	0.43 (2)
C5—C39^vii	1.30 (2)	C29—C53^i	1.05 (2)
C5—C42^v	1.23 (3)	C29—C34^v	1.06 (2)
C5—C5^iv	1.40 (5)	C29—C44^ii	1.30 (2)
C5—C16	1.454 (13)	C29—C40	1.454 (13)
C5—C16^i	1.54 (4)	C34—C53^vii	0.07 (4)
C11—C35^ii	0.12 (5)	C34—C44^vi	0.40 (3)
C11—C45^iii	0.36 (3)	C34—C51^vii	1.34 (4)
C11—C26^i	0.992 (19)	C34—C35	1.394 (13)
C11—C21^i	1.02 (2)	C34—C52^vii	1.45 (3)
C11—C44^iii	1.14 (3)	C35—C45^vi	0.45 (3)
C11—C27^ii	1.39 (3)	C35—C44^vi	1.04 (2)
C11—C15	1.444 (13)	C35—C53^vii	1.34 (4)
C11—C51^ii	1.44 (3)	C35—C51	1.439 (7)
C11—C53^iv	1.44 (3)	C39—C39^vi	0.97 (3)
C11—C34^ii	1.50 (4)	C39—C39^i	0.97 (3)
C11—C14^iii	1.48 (3)	C39—C42	1.452 (13)
C13—C29^ii	0.50 (2)	C39—C39^iv	1.37 (4)
C13—C25^i	0.44 (3)	C40—C47^ii	0.75 (3)
C13—C52^v	0.59 (3)	C40—C46^ii	1.18 (2)
C13—C53^v	1.06 (2)	C40—C41	1.387 (11)
C13—C34^i	1.04 (2)	C40—C42	1.453 (12)
C13—C28^ii	1.23 (2)	C40—C52^i	1.50 (3)
C13—C20^ii	1.30 (2)	C41—C46^ii	0.28 (2)
C13—C44	1.392 (11)	C41—C45^ii	1.23 (3)
C13—C42^v	1.47 (2)	C41—C51	1.445 (13)
C13—C17	1.453 (13)	C42—C47^ii	0.82 (3)
C13—C47^vi	1.54 (3)	C42—C52	1.394 (13)
C14—C51^i	0.46 (3)	C44—C53^v	0.35 (3)
C14—C26^ii	0.77 (2)	C44—C45	1.450 (12)
C14—C41^i	1.06 (2)	C44—C51^v	1.49 (3)
C14—C46^iii	1.15 (3)	C44—C52^v	1.72 (2)
C14—C27^ii	1.23 (3)	C45—C46	1.396 (12)
C14—C21^ii	1.28 (2)	C45—C51^i	1.510 (10)
C14—C15	1.392 (12)	C46—C47	1.443 (13)
C14—C45	1.439 (7)	C46—C51^ii	1.49 (3)
C14—C20	1.453 (12)	C51—C53	1.395 (13)
C14—C35^i	1.507 (10)	C52—C53	1.449 (12)
C15—C27^ii	0.26 (2)
C101—C103—C102	109.7 (6)	C26^v—C27—C17	156.5 (18)
C101—C103—C104	112.3 (8)	C41^v—C27—C35	154 (9)
C102—C103—C104	109.8 (7)	C15^ii—C27—C35	94 (7)
C105—C104—C103	110.9 (8)	C46^vi—C27—C35	147 (5)
C204—C203—C202	114.3 (16)	C45^vi—C27—C35	10.7 (17)
C204—C203—C201	106.3 (16)	C14^ii—C27—C35	139.2 (13)
C202—C203—C201	109.6 (15)	C40^v—C27—C35	89.0 (13)
C203—C204—C105	103.6 (17)	C11^ii—C27—C35	4 (2)
C106—C105—C104	117.1 (6)	C26^v—C27—C35	44.1 (11)
C106—C105—C108^i	110.3 (4)	C17—C27—C35	120.9 (13)
C104—C105—C108^i	108.1 (6)	C41^v—C27—C26	50 (7)
C106—C105—C204	98.9 (9)	C15^ii—C27—C26	155 (6)
C108^i—C105—C204	122.7 (10)	C46^vi—C27—C26	101 (4)
C107—C106—C111	117.5 (5)	C45^vi—C27—C26	100.9 (9)
C107—C106—C105	121.3 (4)	C14^ii—C27—C26	32.4 (10)
C111—C106—C105	121.1 (5)	C40^v—C27—C26	148.2 (19)
C108—C107—C106	123.7 (5)	C11^ii—C27—C26	107.1 (11)
C107—C108—C109	117.0 (5)	C26^v—C27—C26	65.4 (12)
C107—C108—C105^vi	121.8 (5)	C17—C27—C26	119.1 (12)
C109—C108—C105^vi	121.1 (5)	C35—C27—C26	108.3 (8)
O13—C109—C108	118.7 (5)	C41^v—C27—C3^vi	12 (6)
O13—C109—C110	119.4 (5)	C15^ii—C27—C3^vi	117 (6)
C108—C109—C110	121.9 (5)	C46^vi—C27—C3^vi	63 (4)
C109—C110—C111	118.6 (5)	C45^vi—C27—C3^vi	138.2 (13)
C109—C110—C114	123.0 (5)	C14^ii—C27—C3^vi	6.0 (13)
C111—C110—C114	118.4 (5)	C40^v—C27—C3^vi	115.3 (16)
O12—C111—C106	122.2 (5)	C11^ii—C27—C3^vi	143.4 (12)
O12—C111—C110	116.6 (4)	C26^v—C27—C3^vi	103.1 (13)
C106—C111—C110	121.2 (5)	C17—C27—C3^vi	82.6 (11)
N15—C114—C110	121.3 (6)	C35—C27—C3^vi	143.4 (12)
C114—N15—N16	115.3 (5)	C26—C27—C3^vi	38.1 (8)
C—N16—N15	120.4 (5)	C42^i—C28—C25^v	140 (5)
O23—C121—N	121.7 (6)	C42^i—C28—C47^iii	42 (5)
O23—C121—C122	120.3 (7)	C25^v—C28—C47^iii	99 (2)
N—C121—C122	118.0 (6)	C42^i—C28—C52^i	153 (4)
O—C—N16	124.7 (6)	C25^v—C28—C52^i	14.9 (18)
O—C—CA	120.8 (5)	C47^iii—C28—C52^i	113 (2)
N16—C—CA	114.5 (6)	C42^i—C28—C16^ii	13 (6)
N—CA—C	108.3 (4)	C25^v—C28—C16^ii	147 (2)
N—CA—CBA	110.3 (10)	C47^iii—C28—C16^ii	52.4 (17)
C—CA—CBA	118.3 (10)	C52^i—C28—C16^ii	156.8 (15)
N—CA—CB	112.6 (11)	C42^i—C28—C4^ii	153 (7)
C—CA—CB	103.5 (10)	C25^v—C28—C4^ii	60.3 (18)
C121—N—CA	122.0 (6)	C47^iii—C28—C4^ii	155 (2)
CGA—CBA—CA	116.9 (18)	C52^i—C28—C4^ii	45.5 (15)
CD1A—CGA—CD2A	120.9 (14)	C16^ii—C28—C4^ii	140 (2)
CD1A—CGA—CBA	115.6 (16)	C42^i—C28—C5^ii	81 (6)
CD2A—CGA—CBA	123.0 (16)	C25^v—C28—C5^ii	133 (2)
CGA—CD2A—CE2A	120.2 (15)	C47^iii—C28—C5^ii	121 (2)
CZA—CE2A—CD2A	119.7 (16)	C52^i—C28—C5^ii	119 (2)
CE2A—CZA—CE1A	122.1 (16)	C16^ii—C28—C5^ii	69.0 (13)
CZA—CE1A—CD1A	118.5 (15)	C4^ii—C28—C5^ii	74.4 (14)
CGA—CD1A—CE1A	118.1 (16)	C42^i—C28—C13^ii	126 (5)
CG—CB—CA	107 (2)	C25^v—C28—C13^ii	14.0 (15)
CD2—CG—CD1	118.8 (18)	C47^iii—C28—C13^ii	84.7 (15)
CD2—CG—CB	119.1 (17)	C52^i—C28—C13^ii	28.7 (14)
CD1—CG—CB	122 (2)	C16^ii—C28—C13^ii	134.0 (17)
CE2—CD2—CG	123 (2)	C4^ii—C28—C13^ii	73.9 (13)
CD2—CE2—CZ	119 (2)	C5^ii—C28—C13^ii	145 (2)
CE1—CZ—CE2	120 (2)	C42^i—C28—C17^ii	57 (4)
CD1—CE1—CZ	122 (2)	C25^v—C28—C17^ii	83.5 (18)
CE1—CD1—CG	118 (2)	C47^iii—C28—C17^ii	15.3 (11)
O301—C302—C303	122.7 (15)	C52^i—C28—C17^ii	98.0 (18)
C51^ii—C3—C14^iii	121 (10)	C16^ii—C28—C17^ii	66.6 (11)
C51^ii—C3—C26^i	111 (10)	C4^ii—C28—C17^ii	140.5 (17)
C14^iii—C3—C26^i	45 (4)	C5^ii—C28—C17^ii	134 (2)
C51^ii—C3—C21^i	57 (10)	C13^ii—C28—C17^ii	69.5 (12)
C14^iii—C3—C21^i	132 (5)	C42^i—C28—C23	25 (4)
C26^i—C3—C21^i	88.3 (14)	C25^v—C28—C23	115.3 (18)
C51^ii—C3—C20^iii	39 (10)	C47^iii—C28—C23	17.8 (14)
C14^iii—C3—C20^iii	145 (7)	C52^i—C28—C23	129.3 (17)
C26^i—C3—C20^iii	149 (3)	C16^ii—C28—C23	34.6 (13)
C21^i—C3—C20^iii	68.8 (19)	C4^ii—C28—C23	160.3 (16)
C51^ii—C3—C41^ii	111 (10)	C5^ii—C28—C23	103.4 (18)
C14^iii—C3—C41^ii	22 (4)	C13^ii—C28—C23	101.4 (13)
C26^i—C3—C41^ii	65.8 (16)	C17^ii—C28—C23	32.2 (10)
C21^i—C3—C41^ii	146 (2)	C42^i—C28—C39^i	61 (6)
C20^iii—C3—C41^ii	124 (2)	C25^v—C28—C39^i	148 (2)
C51^ii—C3—C46	108 (10)	C47^iii—C28—C39^i	101.6 (18)
C14^iii—C3—C46	33 (4)	C52^i—C28—C39^i	136 (2)
C26^i—C3—C46	76.8 (14)	C16^ii—C28—C39^i	49.6 (14)
C21^i—C3—C46	153 (3)	C4^ii—C28—C39^i	92.9 (16)
C20^iii—C3—C46	114.8 (18)	C5^ii—C28—C39^i	19.5 (12)
C41^ii—C3—C46	11.1 (9)	C13^ii—C28—C39^i	155.0 (18)
C51^ii—C3—C35^ii	82 (10)	C17^ii—C28—C39^i	114.7 (15)
C14^iii—C3—C35^ii	91 (4)	C23—C28—C39^i	83.9 (14)
C26^i—C3—C35^ii	46.9 (13)	C42^i—C28—C39	98 (6)
C21^i—C3—C35^ii	41.4 (12)	C25^v—C28—C39	115.6 (18)
C20^iii—C3—C35^ii	108 (3)	C47^iii—C28—C39	137 (2)
C41^ii—C3—C35^ii	109.8 (17)	C52^i—C28—C39	101.2 (18)
C46—C3—C35^ii	120.6 (16)	C16^ii—C28—C39	86.2 (16)
C51^ii—C3—C11	86 (10)	C4^ii—C28—C39	56.4 (14)
C14^iii—C3—C11	88 (4)	C5^ii—C28—C39	18.0 (13)
C26^i—C3—C11	43.5 (11)	C13^ii—C28—C39	128.0 (14)
C21^i—C3—C11	45.1 (12)	C17^ii—C28—C39	147.2 (17)
C20^iii—C3—C11	112.5 (19)	C23—C28—C39	119.8 (15)
C41^ii—C3—C11	107.7 (14)	C39^i—C28—C39	36.8 (13)
C46—C3—C11	118.6 (13)	C52^i—C29—C13^ii	78 (4)
C35^ii—C3—C11	5 (2)	C52^i—C29—C25^v	32 (4)
C51^ii—C3—C34^iv	40 (10)	C13^ii—C29—C25^v	47 (3)
C14^iii—C3—C34^iv	137 (7)	C52^i—C29—C53^i	154 (4)
C26^i—C3—C34^iv	151 (3)	C13^ii—C29—C53^i	78 (3)
C21^i—C3—C34^iv	76.3 (17)	C25^v—C29—C53^i	123 (3)
C20^iii—C3—C34^iv	8.1 (13)	C52^i—C29—C34^v	151 (4)
C41^ii—C3—C34^iv	116 (2)	C13^ii—C29—C34^v	74 (3)
C46—C3—C34^iv	106.7 (16)	C25^v—C29—C34^v	120 (3)
C35^ii—C3—C34^iv	115 (2)	C53^i—C29—C34^v	4 (2)
C11—C3—C34^iv	119.0 (16)	C52^i—C29—C4^ii	30 (4)
C51^ii—C3—C45^iii	94 (10)	C13^ii—C29—C4^ii	106 (3)
C14^iii—C3—C45^iii	74 (4)	C25^v—C29—C4^ii	60 (2)
C26^i—C3—C45^iii	29.5 (11)	C53^i—C29—C4^ii	161 (3)
C21^i—C3—C45^iii	58.9 (13)	C34^v—C29—C4^ii	162 (3)
C20^iii—C3—C45^iii	125 (2)	C52^i—C29—C44^ii	164 (4)
C41^ii—C3—C45^iii	94.0 (18)	C13^ii—C29—C44^ii	90 (3)
C46—C3—C45^iii	105.0 (16)	C25^v—C29—C44^ii	135 (3)
C35^ii—C3—C45^iii	17.5 (10)	C53^i—C29—C44^ii	12.0 (16)
C11—C3—C45^iii	14.0 (13)	C34^v—C29—C44^ii	15.5 (15)
C34^iv—C3—C45^iii	131 (2)	C4^ii—C29—C44^ii	154 (2)
C51^ii—C3—C53^ii	39 (10)	C52^i—C29—C20	145 (4)
C14^iii—C3—C53^ii	138 (6)	C13^ii—C29—C20	69 (2)
C26^i—C3—C53^ii	150 (3)	C25^v—C29—C20	114 (2)
C21^i—C3—C53^ii	75.0 (19)	C53^i—C29—C20	9.0 (14)
C20^iii—C3—C53^ii	6.9 (12)	C34^v—C29—C20	5.7 (19)
C41^ii—C3—C53^ii	117 (2)	C4^ii—C29—C20	159.1 (19)
C46—C3—C53^ii	107.9 (17)	C44^ii—C29—C20	20.6 (12)
C35^ii—C3—C53^ii	113 (3)	C52^i—C29—C28	25 (3)
C11—C3—C53^ii	118 (2)	C13^ii—C29—C28	55 (3)
C34^iv—C3—C53^ii	1.3 (12)	C25^v—C29—C28	10 (2)
C45^iii—C3—C53^ii	129 (2)	C53^i—C29—C28	129.3 (18)
C16^i—C4—C52^v	142 (5)	C34^v—C29—C28	126 (2)
C16^i—C4—C25^i	155 (3)	C4^ii—C29—C28	51.3 (12)
C52^v—C4—C25^i	16 (2)	C44^ii—C29—C28	139.7 (15)
C16^i—C4—C23^iii	43 (5)	C20—C29—C28	120.3 (12)
C52^v—C4—C23^iii	100 (2)	C52^i—C29—C40	87 (4)
C25^i—C4—C23^iii	115 (2)	C13^ii—C29—C40	159 (4)
C16^i—C4—C39^ii	78 (6)	C25^v—C29—C40	117 (2)
C52^v—C4—C39^ii	133 (2)	C53^i—C29—C40	113.0 (15)
C25^i—C4—C39^ii	117 (2)	C34^v—C29—C40	116.3 (15)
C23^iii—C4—C39^ii	120 (2)	C4^ii—C29—C40	57.5 (12)
C16^i—C4—C28^ii	149 (8)	C44^ii—C29—C40	101.3 (11)
C52^v—C4—C28^ii	61.0 (18)	C20—C29—C40	120.2 (8)
C25^i—C4—C28^ii	45.2 (17)	C28—C29—C40	107.3 (11)
C23^iii—C4—C28^ii	156 (2)	C52^i—C29—C23^vi	72 (3)
C39^ii—C4—C28^ii	73.2 (14)	C13^ii—C29—C23^vi	147 (4)
C16^i—C4—C29^ii	128 (5)	C25^v—C29—C23^vi	102 (2)
C52^v—C4—C29^ii	14.2 (14)	C53^i—C29—C23^vi	128 (2)
C25^i—C4—C29^ii	29.4 (15)	C34^v—C29—C23^vi	131.1 (18)
C23^iii—C4—C29^ii	85.7 (16)	C4^ii—C29—C23^vi	42.1 (12)
C39^ii—C4—C29^ii	144 (2)	C44^ii—C29—C23^vi	116.4 (14)
C28^ii—C4—C29^ii	74.3 (13)	C20—C29—C23^vi	134.6 (12)
C16^i—C4—C47	26 (5)	C28—C29—C23^vi	92.5 (14)
C52^v—C4—C47	116.3 (19)	C40—C29—C23^vi	15.5 (10)
C25^i—C4—C47	130.2 (18)	C52^i—C29—C16^v	41 (4)
C23^iii—C4—C47	17.6 (15)	C13^ii—C29—C16^v	117 (3)
C39^ii—C4—C47	102.5 (18)	C25^v—C29—C16^v	71 (2)
C28^ii—C4—C47	159.4 (16)	C53^i—C29—C16^v	154 (2)
C29^ii—C4—C47	102.1 (13)	C34^v—C29—C16^v	155 (2)
C16^i—C4—C40^ii	58 (5)	C4^ii—C29—C16^v	11.2 (12)
C52^v—C4—C40^ii	84.5 (18)	C44^ii—C29—C16^v	144.3 (17)
C25^i—C4—C40^ii	99.3 (19)	C20—C29—C16^v	155.2 (15)
C23^iii—C4—C40^ii	15.5 (11)	C28—C29—C16^v	61.6 (12)
C39^ii—C4—C40^ii	133 (2)	C40—C29—C16^v	46.5 (11)
C28^ii—C4—C40^ii	141.3 (17)	C23^vi—C29—C16^v	31.2 (10)
C29^ii—C4—C40^ii	70.3 (13)	C53^vii—C34—C44^vi	42 (10)
C47—C4—C40^ii	32.1 (11)	C53^vii—C34—C20^v	122 (10)
C16^i—C4—C42^ii	11 (6)	C44^vi—C34—C20^v	81 (5)
C52^v—C4—C42^ii	148 (2)	C53^vii—C34—C29^v	79 (10)
C25^i—C4—C42^ii	156.5 (16)	C44^vi—C34—C29^v	119 (4)
C23^iii—C4—C42^ii	52.7 (16)	C20^v—C34—C29^v	157 (7)
C39^ii—C4—C42^ii	67.9 (13)	C53^vii—C34—C13^vi	106 (10)
C28^ii—C4—C42^ii	138 (2)	C44^vi—C34—C13^vi	147 (5)
C29^ii—C4—C42^ii	134.9 (17)	C20^v—C34—C13^vi	131 (7)
C47—C4—C42^ii	35.1 (13)	C29^v—C34—C13^vi	27.6 (12)
C40^ii—C4—C42^ii	66.9 (12)	C53^vii—C34—C51^vii	146 (10)
C16^i—C4—C5	96 (7)	C44^vi—C34—C51^vii	105 (4)
C52^v—C4—C5	115.2 (18)	C20^v—C34—C51^vii	26 (5)
C25^i—C4—C5	99 (2)	C29^v—C34—C51^vii	131 (3)
C23^iii—C4—C5	137 (2)	C13^vi—C34—C51^vii	105 (3)
C39^ii—C4—C5	18.3 (13)	C53^vii—C34—C35	29 (10)
C28^ii—C4—C5	55.0 (14)	C44^vi—C34—C35	22 (4)
C29^ii—C4—C5	127.2 (14)	C20^v—C34—C35	97 (5)
C47—C4—C5	119.8 (15)	C29^v—C34—C35	100.1 (18)
C40^ii—C4—C5	147.0 (19)	C13^vi—C34—C35	127 (2)
C42^ii—C4—C5	85.7 (17)	C51^vii—C34—C35	117.5 (16)
C16^i—C4—C13	146 (3)	C53^vii—C34—C52^vii	87 (10)
C52^v—C4—C13	7.3 (15)	C44^vi—C34—C52^vii	127 (4)
C25^i—C4—C13	10.1 (15)	C20^v—C34—C52^vii	149 (7)
C23^iii—C4—C13	104.7 (15)	C29^v—C34—C52^vii	8.4 (12)
C39^ii—C4—C13	125.9 (16)	C13^vi—C34—C52^vii	20.0 (12)
C28^ii—C4—C13	54.9 (13)	C51^vii—C34—C52^vii	123 (3)
C29^ii—C4—C13	19.5 (10)	C35—C34—C52^vii	106.8 (17)
C47—C4—C13	120.2 (11)	C53^vii—C34—C3^iv	148 (10)
C40^ii—C4—C13	89.2 (12)	C44^vi—C34—C3^iv	107 (3)
C42^ii—C4—C13	149.3 (13)	C20^v—C34—C3^iv	27 (5)
C5—C4—C13	108.4 (11)	C29^v—C34—C3^iv	131 (3)
C39^ii—C5—C39^v	132 (8)	C13^vi—C34—C3^iv	104 (2)
C39^ii—C5—C5^i	23 (4)	C51^vii—C34—C3^iv	3.8 (17)
C39^v—C5—C5^i	109 (3)	C35—C34—C3^iv	120.4 (11)
C39^ii—C5—C5^vi	113 (5)	C52^vii—C34—C3^iv	122 (2)
C39^v—C5—C5^vi	19 (3)	C53^vii—C34—C11^ii	27 (10)
C5^i—C5—C5^vi	89.999 (10)	C44^vi—C34—C11^ii	22 (4)
C39^ii—C5—C28^ii	108 (4)	C20^v—C34—C11^ii	99 (5)
C39^v—C5—C28^ii	116 (4)	C29^v—C34—C11^ii	99 (2)
C5^i—C5—C28^ii	129 (3)	C13^vi—C34—C11^ii	126 (2)
C5^vi—C5—C28^ii	133 (3)	C51^vii—C34—C11^ii	119 (2)
C39^ii—C5—C39^iii	44 (4)	C35—C34—C11^ii	2.5 (17)
C39^v—C5—C39^iii	88 (4)	C52^vii—C34—C11^ii	106.2 (18)
C5^i—C5—C39^iii	20.2 (14)	C3^iv—C34—C11^ii	122.2 (13)
C5^vi—C5—C39^iii	69.8 (13)	C53^vii—C34—C21^vi	109 (10)
C28^ii—C5—C39^iii	146 (3)	C44^vi—C34—C21^vi	68 (3)
C39^ii—C5—C39^vii	88 (5)	C20^v—C34—C21^vi	17 (4)
C39^v—C5—C39^vii	44 (3)	C29^v—C34—C21^vi	158 (3)
C5^i—C5—C39^vii	64.7 (12)	C13^vi—C34—C21^vi	140 (3)
C5^vi—C5—C39^vii	25.3 (12)	C51^vii—C34—C21^vi	36.9 (11)
C28^ii—C5—C39^vii	152 (3)	C35—C34—C21^vi	82.0 (10)
C39^iii—C5—C39^vii	44.5 (13)	C52^vii—C34—C21^vi	152 (3)
C39^ii—C5—C42^v	124 (4)	C3^iv—C34—C21^vi	39.1 (7)
C39^v—C5—C42^v	99 (3)	C11^ii—C34—C21^vi	83.6 (13)
C5^i—C5—C42^v	144 (3)	C53^vii—C34—C25	99 (10)
C5^vi—C5—C42^v	117 (3)	C44^vi—C34—C25	139 (4)
C28^ii—C5—C42^v	16.5 (11)	C20^v—C34—C25	137 (6)
C39^iii—C5—C42^v	156 (4)	C29^v—C34—C25	21.0 (14)
C39^vii—C5—C42^v	139 (3)	C13^vi—C34—C25	8.0 (14)
C39^ii—C5—C5^iv	68 (4)	C51^vii—C34—C25	111 (2)
C39^v—C5—C5^iv	64 (3)	C35—C34—C25	118.6 (16)
C5^i—C5—C5^iv	45.000 (5)	C52^vii—C34—C25	12.8 (12)
C5^vi—C5—C5^iv	45.000 (14)	C3^iv—C34—C25	109.8 (18)
C28^ii—C5—C5^iv	158.0 (18)	C11^ii—C34—C25	118.2 (17)
C39^iii—C5—C5^iv	24.8 (13)	C21^vi—C34—C25	143 (2)
C39^vii—C5—C5^iv	19.7 (11)	C11^ii—C35—C45^vi	37 (10)
C42^v—C5—C5^iv	153 (2)	C11^ii—C35—C21^v	114 (10)
C39^ii—C5—C16	158 (6)	C45^vi—C35—C21^v	130.1 (18)
C39^v—C5—C16	58 (3)	C11^ii—C35—C44^vi	146 (10)
C5^i—C5—C16	156 (2)	C45^vi—C35—C44^vi	153 (2)
C5^vi—C5—C16	76 (3)	C21^v—C35—C44^vi	77 (2)
C28^ii—C5—C16	58.1 (12)	C11^ii—C35—C26^v	52 (10)
C39^iii—C5—C16	140 (3)	C45^vi—C35—C26^v	43.7 (13)
C39^vii—C5—C16	99 (2)	C21^v—C35—C26^v	86.7 (16)
C42^v—C5—C16	41.8 (11)	C44^vi—C35—C26^v	160 (3)
C5^iv—C5—C16	118 (3)	C11^ii—C35—C53^vii	146 (10)
C39^ii—C5—C4	57 (3)	C45^vi—C35—C53^vii	144 (3)
C39^v—C5—C4	159 (5)	C21^v—C35—C53^vii	84 (2)
C5^i—C5—C4	79 (3)	C44^vi—C35—C53^vii	8.9 (15)
C5^vi—C5—C4	158.4 (18)	C26^v—C35—C53^vii	161 (3)
C28^ii—C5—C4	50.6 (11)	C11^ii—C35—C34	147 (10)
C39^iii—C5—C4	98 (2)	C45^vi—C35—C34	146 (3)
C39^vii—C5—C4	139 (3)	C21^v—C35—C34	82.9 (18)
C42^v—C5—C4	66.9 (12)	C44^vi—C35—C34	8.3 (17)
C5^iv—C5—C4	122 (3)	C26^v—C35—C34	160 (3)
C16—C5—C4	107.3 (12)	C53^vii—C35—C34	1.3 (15)
C39^ii—C5—C16^i	44 (3)	C11^ii—C35—C3^ii	81 (10)
C39^v—C5—C16^i	160 (6)	C45^vi—C35—C3^ii	86.4 (17)
C5^i—C5—C16^i	66 (2)	C21^v—C35—C3^ii	43.7 (13)
C5^vi—C5—C16^i	149.5 (19)	C44^vi—C35—C3^ii	120 (2)
C28^ii—C5—C16^i	63.9 (14)	C26^v—C35—C3^ii	43.0 (12)
C39^iii—C5—C16^i	85.0 (18)	C53^vii—C35—C3^ii	126 (3)
C39^vii—C5—C16^i	127 (3)	C34—C35—C3^ii	125 (2)
C42^v—C5—C16^i	80.0 (14)	C11^ii—C35—C51	86 (10)
C5^iv—C5—C16^i	109 (2)	C45^vi—C35—C51	90.3 (8)
C16—C5—C16^i	119.4 (10)	C21^v—C35—C51	40.2 (14)
C4—C5—C16^i	13.5 (11)	C44^vi—C35—C51	115.4 (16)
C35^ii—C11—C45^iii	131 (10)	C26^v—C35—C51	46.6 (13)
C35^ii—C11—C26^i	122 (10)	C53^vii—C35—C51	121.4 (18)
C45^iii—C11—C26^i	48 (4)	C34—C35—C51	120.0 (12)
C35^ii—C11—C21^i	60 (10)	C3^ii—C35—C51	5 (2)
C45^iii—C11—C21^i	135 (5)	C11^ii—C35—C27	59 (10)
C26^i—C11—C21^i	87.5 (14)	C45^vi—C35—C27	26 (4)
C35^ii—C11—C44^iii	31 (10)	C21^v—C35—C27	147.4 (18)
C45^iii—C11—C44^iii	146 (6)	C44^vi—C35—C27	128.3 (17)
C26^i—C11—C44^iii	152 (3)	C26^v—C35—C27	63.8 (14)
C21^i—C11—C44^iii	70.2 (18)	C53^vii—C35—C27	119.6 (17)
C35^ii—C11—C27^ii	116 (10)	C34—C35—C27	120.4 (14)
C45^iii—C11—C27^ii	21 (4)	C3^ii—C35—C27	105.9 (15)
C26^i—C11—C27^ii	67.6 (15)	C51—C35—C27	108.4 (10)
C21^i—C11—C27^ii	148 (2)	C11^ii—C35—C20^v	153 (10)
C44^iii—C11—C27^ii	125 (2)	C45^vi—C35—C20^v	159 (4)
C35^ii—C11—C15	111 (10)	C21^v—C35—C20^v	69.0 (17)
C45^iii—C11—C15	31 (4)	C44^vi—C35—C20^v	9.4 (12)
C26^i—C11—C15	78.1 (14)	C26^v—C35—C20^v	151 (2)
C21^i—C11—C15	155 (2)	C53^vii—C35—C20^v	15.0 (10)
C44^iii—C11—C15	115.4 (16)	C34—C35—C20^v	13.8 (9)
C27^ii—C11—C15	10.5 (9)	C3^ii—C35—C20^v	111 (2)
C35^ii—C11—C3	94 (10)	C51—C35—C20^v	106.7 (13)
C45^iii—C11—C3	92 (4)	C27—C35—C20^v	132.9 (16)
C26^i—C11—C3	43.4 (11)	C11^ii—C35—C14^vi	72 (10)
C21^i—C11—C3	44.5 (12)	C45^vi—C35—C14^vi	72.7 (9)
C44^iii—C11—C3	113.8 (18)	C21^v—C35—C14^vi	57.7 (14)
C27^ii—C11—C3	109.8 (14)	C44^vi—C35—C14^vi	132.8 (18)
C15—C11—C3	120.1 (12)	C26^v—C35—C14^vi	29.0 (12)
C35^ii—C11—C51^ii	89 (10)	C53^vii—C35—C14^vi	138 (2)
C45^iii—C11—C51^ii	95 (4)	C34—C35—C14^vi	136.8 (16)
C26^i—C11—C51^ii	46.9 (13)	C3^ii—C35—C14^vi	14.2 (13)
C21^i—C11—C51^ii	40.7 (12)	C51—C35—C14^vi	17.6 (9)
C44^iii—C11—C51^ii	109 (2)	C27—C35—C14^vi	91.8 (11)
C27^ii—C11—C51^ii	111.8 (17)	C20^v—C35—C14^vi	123.9 (15)
C15—C11—C51^ii	121.8 (15)	C5^ii—C39—C5^v	138 (7)
C3—C11—C51^ii	6 (2)	C5^ii—C39—C39^vi	117 (4)
C35^ii—C11—C53^iv	31 (10)	C5^v—C39—C39^vi	21 (4)
C45^iii—C11—C53^iv	138 (6)	C5^ii—C39—C39^i	27 (5)
C26^i—C11—C53^iv	153 (3)	C5^v—C39—C39^i	111 (4)
C21^i—C11—C53^iv	77.1 (15)	C39^vi—C39—C39^i	90.001 (7)
C44^iii—C11—C53^iv	8.1 (14)	C5^ii—C39—C16^v	121 (4)
C27^ii—C11—C53^iv	116.7 (18)	C5^v—C39—C16^v	99 (3)
C15—C11—C53^iv	107.4 (14)	C39^vi—C39—C16^v	118 (3)
C3—C11—C53^iv	119.7 (15)	C39^i—C39—C16^v	144 (2)
C51^ii—C11—C53^iv	114.7 (19)	C5^ii—C39—C4^ii	105 (4)
C35^ii—C11—C34^ii	30 (10)	C5^v—C39—C4^ii	115 (3)
C45^iii—C11—C34^ii	138 (6)	C39^vi—C39—C4^ii	134 (3)
C26^i—C11—C34^ii	152 (3)	C39^i—C39—C4^ii	129 (3)
C21^i—C11—C34^ii	76.0 (18)	C16^v—C39—C4^ii	16.6 (12)
C44^iii—C11—C34^ii	7.5 (14)	C5^ii—C39—C5^iii	47 (4)
C27^ii—C11—C34^ii	117.4 (18)	C5^v—C39—C5^iii	92 (4)
C15—C11—C34^ii	108.2 (15)	C39^vi—C39—C5^iii	70.4 (13)
C3—C11—C34^ii	118.6 (19)	C39^i—C39—C5^iii	19.6 (12)
C51^ii—C11—C34^ii	114 (3)	C16^v—C39—C5^iii	157 (3)
C53^iv—C11—C34^ii	1.2 (13)	C4^ii—C39—C5^iii	146 (3)
C35^ii—C11—C14^iii	103 (10)	C5^ii—C39—C5^vii	92 (5)
C45^iii—C11—C14^iii	77 (4)	C5^v—C39—C5^vii	46 (3)
C26^i—C11—C14^iii	29.0 (11)	C39^vi—C39—C5^vii	24.8 (12)
C21^i—C11—C14^iii	58.6 (13)	C39^i—C39—C5^vii	65.2 (13)
C44^iii—C11—C14^iii	127 (2)	C16^v—C39—C5^vii	140 (3)
C27^ii—C11—C14^iii	95.5 (18)	C4^ii—C39—C5^vii	154 (3)
C15—C11—C14^iii	105.8 (15)	C5^iii—C39—C5^vii	45.5 (13)
C3—C11—C14^iii	14.5 (13)	C5^ii—C39—C42	159 (5)
C51^ii—C11—C14^iii	18.0 (10)	C5^v—C39—C42	57 (3)
C53^iv—C11—C14^iii	131.6 (19)	C39^vi—C39—C42	77 (2)
C34^ii—C11—C14^iii	130 (2)	C39^i—C39—C42	157.2 (17)
C29^ii—C13—C25^i	78 (4)	C16^v—C39—C42	41.7 (10)
C29^ii—C13—C52^v	46 (3)	C4^ii—C39—C42	58.2 (12)
C25^i—C13—C52^v	33 (4)	C5^iii—C39—C42	142 (3)
C29^ii—C13—C53^v	75 (3)	C5^vii—C39—C42	100 (2)
C25^i—C13—C53^v	150 (4)	C5^ii—C39—C28^vi	165 (7)
C52^v—C13—C53^v	120 (3)	C5^v—C39—C28^vi	45 (3)
C29^ii—C13—C34^i	78 (3)	C39^vi—C39—C28^vi	64.2 (18)
C25^i—C13—C34^i	153 (4)	C39^i—C39—C28^vi	148.7 (16)
C52^v—C13—C34^i	123 (3)	C16^v—C39—C28^vi	54.0 (13)
C53^v—C13—C34^i	3 (2)	C4^ii—C39—C28^vi	70.5 (15)
C29^ii—C13—C28^ii	105 (3)	C5^iii—C39—C28^vi	131 (2)
C25^i—C13—C28^ii	28 (4)	C5^vii—C39—C28^vi	88.1 (17)
C52^v—C13—C28^ii	60 (2)	C42—C39—C28^vi	12.4 (10)
C53^v—C13—C28^ii	161 (2)	C5^ii—C39—C28	54 (3)
C34^i—C13—C28^ii	160 (3)	C5^v—C39—C28	161 (4)
C29^ii—C13—C20^ii	90 (3)	C39^vi—C39—C28	158.6 (16)
C25^i—C13—C20^ii	160 (5)	C39^i—C39—C28	79 (2)
C52^v—C13—C20^ii	134 (3)	C16^v—C39—C28	66.7 (11)
C53^v—C13—C20^ii	15.3 (14)	C4^ii—C39—C28	50.4 (11)
C34^i—C13—C20^ii	12.0 (17)	C5^iii—C39—C28	98 (2)
C28^ii—C13—C20^ii	153.0 (19)	C5^vii—C39—C28	140 (3)
C29^ii—C13—C44	69 (2)	C42—C39—C28	107.2 (11)
C25^i—C13—C44	144 (4)	C28^vi—C39—C28	118.7 (10)
C52^v—C13—C44	114 (3)	C5^ii—C39—C39^iv	72 (4)
C53^v—C13—C44	5.7 (17)	C5^v—C39—C39^iv	66 (4)
C34^i—C13—C44	9.0 (15)	C39^vi—C39—C39^iv	45.001 (7)
C28^ii—C13—C44	159.1 (17)	C39^i—C39—C39^iv	45.001 (4)
C20^ii—C13—C44	20.7 (11)	C16^v—C39—C39^iv	154.2 (19)
C29^ii—C13—C42^v	116 (3)	C4^ii—C39—C39^iv	158.8 (14)
C25^i—C13—C42^v	39 (4)	C5^iii—C39—C39^iv	25.4 (13)
C52^v—C13—C42^v	71 (2)	C5^vii—C39—C39^iv	20.2 (13)
C53^v—C13—C42^v	155 (2)	C42—C39—C39^iv	119 (2)
C34^i—C13—C42^v	153 (2)	C28^vi—C39—C39^iv	107.3 (18)
C28^ii—C13—C42^v	11.3 (11)	C28—C39—C39^iv	122 (2)
C20^ii—C13—C42^v	143.4 (16)	C23^vi—C40—C47^ii	40 (3)
C44—C13—C42^v	155.9 (14)	C23^vi—C40—C17^v	71 (4)
C29^ii—C13—C17	158 (4)	C47^ii—C40—C17^v	31 (2)
C25^i—C13—C17	86 (4)	C23^vi—C40—C15^vi	148 (4)
C52^v—C13—C17	118 (3)	C47^ii—C40—C15^vi	108 (2)
C53^v—C13—C17	115.7 (15)	C17^v—C40—C15^vi	77 (2)
C34^i—C13—C17	112.5 (17)	C23^vi—C40—C46^ii	134 (4)
C28^ii—C13—C17	58.1 (12)	C47^ii—C40—C46^ii	94 (2)
C20^ii—C13—C17	100.6 (11)	C17^v—C40—C46^ii	63.1 (19)
C44—C13—C17	120.4 (9)	C15^vi—C40—C46^ii	14.1 (17)
C42^v—C13—C17	46.9 (11)	C23^vi—C40—C16^v	28 (5)
C29^ii—C13—C4	54 (3)	C47^ii—C40—C16^v	65 (2)
C25^i—C13—C4	25 (3)	C17^v—C40—C16^v	95 (2)
C52^v—C13—C4	11 (2)	C15^vi—C40—C16^v	163 (3)
C53^v—C13—C4	125.8 (18)	C46^ii—C40—C16^v	154 (2)
C34^i—C13—C4	128.9 (18)	C23^vi—C40—C27^v	148 (4)
C28^ii—C13—C4	51.2 (11)	C47^ii—C40—C27^v	108 (2)
C20^ii—C13—C4	138.6 (15)	C17^v—C40—C27^v	77.3 (18)
C44—C13—C4	120.1 (11)	C15^vi—C40—C27^v	4.2 (19)
C42^v—C13—C4	61.9 (12)	C46^ii—C40—C27^v	14.8 (11)
C17—C13—C4	107.9 (11)	C16^v—C40—C27^v	159 (2)
C29^ii—C13—C47^vi	146 (4)	C23^vi—C40—C4^ii	42 (4)
C25^i—C13—C47^vi	71 (4)	C47^ii—C40—C4^ii	80 (2)
C52^v—C13—C47^vi	103 (3)	C17^v—C40—C4^ii	110 (2)
C53^v—C13—C47^vi	130.4 (18)	C15^vi—C40—C4^ii	161 (2)
C34^i—C13—C47^vi	127 (2)	C46^ii—C40—C4^ii	162 (3)
C28^ii—C13—C47^vi	42.7 (12)	C16^v—C40—C4^ii	15.5 (13)
C20^ii—C13—C47^vi	115.5 (15)	C27^v—C40—C4^ii	157.0 (18)
C44—C13—C47^vi	134.6 (12)	C23^vi—C40—C41	141 (4)
C42^v—C13—C47^vi	31.6 (10)	C47^ii—C40—C41	101 (2)
C17—C13—C47^vi	15.4 (11)	C17^v—C40—C41	69.9 (18)
C4—C13—C47^vi	93.1 (16)	C15^vi—C40—C41	8.7 (15)
C3^iii—C14—C51^i	15 (7)	C46^ii—C40—C41	8.4 (13)
C3^iii—C14—C26^ii	115 (5)	C16^v—C40—C41	155 (2)
C51^i—C14—C26^ii	114.2 (19)	C27^v—C40—C41	7.4 (12)
C3^iii—C14—C41^i	150 (5)	C4^ii—C40—C41	158.0 (16)
C51^i—C14—C41^i	142 (5)	C23^vi—C40—C42	22 (3)
C26^ii—C14—C41^i	92 (2)	C47^ii—C40—C42	23 (2)
C3^iii—C14—C46^iii	137 (5)	C17^v—C40—C42	53 (2)
C51^i—C14—C46^iii	132 (3)	C15^vi—C40—C42	127.7 (17)
C26^ii—C14—C46^iii	106 (3)	C46^ii—C40—C42	114.2 (16)
C41^i—C14—C46^iii	13.7 (13)	C16^v—C40—C42	42.2 (11)
C3^iii—C14—C27^ii	153 (5)	C27^v—C40—C42	126.5 (15)
C51^i—C14—C27^ii	144 (5)	C4^ii—C40—C42	57.5 (12)
C26^ii—C14—C27^ii	89 (2)	C41—C40—C42	119.4 (13)
C41^i—C14—C27^ii	3.0 (11)	C23^vi—C40—C29	94 (4)
C46^iii—C14—C27^ii	16.7 (11)	C47^ii—C40—C29	132 (2)
C3^iii—C14—C21^ii	36 (4)	C17^v—C40—C29	157 (3)
C51^i—C14—C21^ii	33.7 (11)	C15^vi—C40—C29	115.1 (14)
C26^ii—C14—C21^ii	81.0 (18)	C46^ii—C40—C29	128.2 (12)
C41^i—C14—C21^ii	157 (3)	C16^v—C40—C29	67.5 (12)
C46^iii—C14—C21^ii	158 (3)	C27^v—C40—C29	113.5 (11)
C27^ii—C14—C21^ii	156 (3)	C4^ii—C40—C29	52.2 (11)
C3^iii—C14—C15	144 (5)	C41—C40—C29	120.0 (8)
C51^i—C14—C15	137 (4)	C42—C40—C29	108.3 (10)
C26^ii—C14—C15	98 (2)	C23^vi—C40—C52^i	77 (4)
C41^i—C14—C15	6.1 (10)	C47^ii—C40—C52^i	115 (2)
C46^iii—C14—C15	7.6 (15)	C17^v—C40—C52^i	144 (3)
C27^ii—C14—C15	9.2 (10)	C15^vi—C40—C52^i	131 (2)
C21^ii—C14—C15	158 (2)	C46^ii—C40—C52^i	143.5 (16)
C3^iii—C14—C45	91 (4)	C16^v—C40—C52^i	50.8 (13)
C51^i—C14—C45	90.1 (8)	C27^v—C40—C52^i	129.2 (15)
C26^ii—C14—C45	24.2 (17)	C4^ii—C40—C52^i	35.4 (10)
C41^i—C14—C45	114.6 (14)	C41—C40—C52^i	135.1 (12)
C46^iii—C14—C45	128.0 (18)	C42—C40—C52^i	92.1 (14)
C27^ii—C14—C45	111.6 (15)	C29—C40—C52^i	16.8 (10)
C21^ii—C14—C45	56.8 (11)	C27^v—C41—C46^ii	98 (9)
C15—C14—C45	120.4 (11)	C27^v—C41—C15^vi	45 (6)
C3^iii—C14—C20	27 (6)	C46^ii—C41—C15^vi	53 (6)
C51^i—C14—C20	18.9 (17)	C27^v—C41—C14^vi	159 (7)
C26^ii—C14—C20	131 (2)	C46^ii—C41—C14^vi	103 (6)
C41^i—C14—C20	124.8 (19)	C15^vi—C41—C14^vi	156 (4)
C46^iii—C14—C20	113.2 (18)	C27^v—C41—C45^ii	26 (6)
C27^ii—C14—C20	127.5 (17)	C46^ii—C41—C45^ii	123 (7)
C21^ii—C14—C20	52.3 (11)	C15^vi—C41—C45^ii	70 (4)
C15—C14—C20	119.3 (12)	C14^vi—C41—C45^ii	134.4 (13)
C45—C14—C20	107.8 (10)	C27^v—C41—C26^v	124 (7)
C3^iii—C14—C11^iii	77 (4)	C46^ii—C41—C26^v	138 (7)
C51^i—C14—C11^iii	76.2 (14)	C15^vi—C41—C26^v	169 (4)
C26^ii—C14—C11^iii	38.4 (14)	C14^vi—C41—C26^v	35.4 (11)
C41^i—C14—C11^iii	128 (2)	C45^ii—C41—C26^v	99.1 (14)
C46^iii—C14—C11^iii	141 (3)	C27^v—C41—C3^ii	166 (7)
C27^ii—C14—C11^iii	125 (2)	C46^ii—C41—C3^ii	96 (7)
C21^ii—C14—C11^iii	42.7 (11)	C15^vi—C41—C3^ii	148 (4)
C15—C14—C11^iii	133.7 (15)	C14^vi—C41—C3^ii	7.5 (14)
C45—C14—C11^iii	14.2 (13)	C45^ii—C41—C3^ii	140.9 (18)
C20—C14—C11^iii	94.3 (14)	C26^v—C41—C3^ii	42.5 (10)
C3^iii—C14—C35^i	75 (4)	C27^v—C41—C17^v	101 (8)
C51^i—C14—C35^i	72.7 (9)	C46^ii—C41—C17^v	20 (8)
C26^ii—C14—C35^i	41.6 (18)	C15^vi—C41—C17^v	57 (4)
C41^i—C14—C35^i	129.4 (16)	C14^vi—C41—C17^v	99.1 (17)
C46^iii—C14—C35^i	142 (2)	C45^ii—C41—C17^v	121.2 (18)
C27^ii—C14—C35^i	126.7 (16)	C26^v—C41—C17^v	131.8 (19)
C21^ii—C14—C35^i	39.4 (11)	C3^ii—C41—C17^v	91.6 (16)
C15—C14—C35^i	134.8 (13)	C27^v—C41—C40	68 (8)
C45—C14—C35^i	17.4 (10)	C46^ii—C41—C40	38 (6)
C20—C14—C35^i	90.6 (12)	C15^vi—C41—C40	27 (5)
C11^iii—C14—C35^i	4.4 (19)	C14^vi—C41—C40	131.4 (19)
C27^ii—C15—C46^iii	79 (8)	C45^ii—C41—C40	88.5 (14)
C27^ii—C15—C41^i	30 (6)	C26^v—C41—C40	157.2 (18)
C46^iii—C15—C41^i	49 (5)	C3^ii—C41—C40	124.0 (18)
C27^ii—C15—C40^i	159 (10)	C17^v—C41—C40	33.2 (9)
C46^iii—C15—C40^i	103 (6)	C27^v—C41—C51	166 (8)
C41^i—C15—C40^i	144 (6)	C46^ii—C41—C51	94 (7)
C27^ii—C15—C45^iii	64 (6)	C15^vi—C41—C51	146 (4)
C46^iii—C15—C45^iii	143 (6)	C14^vi—C41—C51	11.2 (16)
C41^i—C15—C45^iii	93 (4)	C45^ii—C41—C51	140.6 (13)
C40^i—C15—C45^iii	110 (2)	C26^v—C41—C51	44.1 (11)
C27^ii—C15—C17^ii	136 (7)	C3^ii—C41—C51	5 (2)
C46^iii—C15—C17^ii	63 (6)	C17^v—C41—C51	88.9 (13)
C41^i—C15—C17^ii	108 (4)	C40—C41—C51	120.6 (12)
C40^i—C15—C17^ii	40.0 (12)	C27^v—C41—C26	58 (7)
C45^iii—C15—C17^ii	147 (3)	C46^ii—C41—C26	156 (6)
C27^ii—C15—C23	157 (9)	C15^vi—C41—C26	103 (4)
C46^iii—C15—C23	95 (6)	C14^vi—C41—C26	101.3 (9)
C41^i—C15—C23	137 (5)	C45^ii—C41—C26	33.3 (10)
C40^i—C15—C23	8.6 (12)	C26^v—C41—C26	65.9 (11)
C45^iii—C15—C23	117.9 (19)	C3^ii—C41—C26	108.1 (11)
C17^ii—C15—C23	31.5 (11)	C17^v—C41—C26	149.3 (17)
C27^ii—C15—C14	48 (6)	C40—C41—C26	119.8 (12)
C46^iii—C15—C14	31 (5)	C51—C41—C26	108.7 (8)
C41^i—C15—C14	18 (3)	C27^v—C41—C11^vi	22 (7)
C40^i—C15—C14	128.7 (18)	C46^ii—C41—C11^vi	118 (6)
C45^iii—C15—C14	111.4 (16)	C15^vi—C41—C11^vi	65 (4)
C17^ii—C15—C14	90.3 (14)	C14^vi—C41—C11^vi	138.7 (13)
C23—C15—C14	120.4 (13)	C45^ii—C41—C11^vi	5.7 (14)
C27^ii—C15—C11	73 (7)	C26^v—C41—C11^vi	103.8 (13)
C46^iii—C15—C11	151 (6)	C3^ii—C41—C11^vi	144.7 (12)
C41^i—C15—C11	102 (4)	C17^v—C41—C11^vi	115.5 (15)
C40^i—C15—C11	100.6 (17)	C40—C41—C11^vi	82.9 (11)
C45^iii—C15—C11	9.4 (14)	C51—C41—C11^vi	143.8 (11)
C17^ii—C15—C11	138 (2)	C26—C41—C11^vi	38.2 (7)
C23—C15—C11	108.6 (13)	C28^vi—C42—C47^ii	121 (6)
C14—C15—C11	119.9 (10)	C28^vi—C42—C16^v	163 (8)
C27^ii—C15—C47^iii	145 (8)	C47^ii—C42—C16^v	73 (2)
C46^iii—C15—C47^iii	75 (6)	C28^vi—C42—C23^vi	147 (5)
C41^i—C15—C47^iii	119 (5)	C47^ii—C42—C23^vi	26.7 (17)
C40^i—C15—C47^iii	28.4 (11)	C16^v—C42—C23^vi	46.0 (18)
C45^iii—C15—C47^iii	136 (2)	C28^vi—C42—C25^vii	29 (4)
C17^ii—C15—C47^iii	11.6 (11)	C47^ii—C42—C25^vii	93 (3)
C23—C15—C47^iii	19.9 (9)	C16^v—C42—C25^vii	158 (2)
C14—C15—C47^iii	101.3 (15)	C23^vi—C42—C25^vii	119 (2)
C11—C15—C47^iii	127.1 (17)	C28^vi—C42—C17^v	108 (5)
C27^ii—C15—C35^ii	76 (6)	C47^ii—C42—C17^v	13.6 (16)
C46^iii—C15—C35^ii	152 (7)	C16^v—C42—C17^v	84.7 (18)
C41^i—C15—C35^ii	104 (4)	C23^vi—C42—C17^v	39.2 (14)
C40^i—C15—C35^ii	97 (2)	C25^vii—C42—C17^v	80.0 (16)
C45^iii—C15—C35^ii	12.8 (13)	C28^vi—C42—C4^ii	159 (7)
C17^ii—C15—C35^ii	134 (3)	C47^ii—C42—C4^ii	76.2 (19)
C23—C15—C35^ii	105.1 (16)	C16^v—C42—C4^ii	4 (2)
C14—C15—C35^ii	121.2 (12)	C23^vi—C42—C4^ii	49.5 (19)
C11—C15—C35^ii	4.3 (19)	C25^vii—C42—C4^ii	158.3 (19)
C47^iii—C15—C35^ii	123 (2)	C17^v—C42—C4^ii	87.9 (15)
C27^ii—C15—C26^i	35 (6)	C28^vi—C42—C5^v	83 (6)
C46^iii—C15—C26^i	113 (5)	C47^ii—C42—C5^v	152 (3)
C41^i—C15—C26^i	64 (3)	C16^v—C42—C5^v	81.2 (18)
C40^i—C15—C26^i	135 (2)	C23^vi—C42—C5^v	126 (2)
C45^iii—C15—C26^i	29.1 (12)	C25^vii—C42—C5^v	108 (2)
C17^ii—C15—C26^i	155 (3)	C17^v—C42—C5^v	158 (2)
C23—C15—C26^i	141.4 (15)	C4^ii—C42—C5^v	77.4 (18)
C14—C15—C26^i	82.4 (9)	C28^vi—C42—C13^v	43 (4)
C11—C15—C26^i	38.1 (8)	C47^ii—C42—C13^v	79 (2)
C47^iii—C15—C26^i	153 (3)	C16^v—C42—C13^v	146.9 (19)
C35^ii—C15—C26^i	40.4 (10)	C23^vi—C42—C13^v	104.8 (18)
C4^vi—C16—C23^ii	119 (6)	C25^vii—C42—C13^v	14.1 (11)
C4^vi—C16—C42^v	165 (8)	C17^v—C42—C13^v	66.0 (12)
C23^ii—C16—C42^v	74 (2)	C4^ii—C42—C13^v	148.4 (14)
C4^vi—C16—C47^vi	145 (6)	C5^v—C42—C13^v	121.2 (19)
C23^ii—C16—C47^vi	26.9 (17)	C28^vi—C42—C39	106 (6)
C42^v—C16—C47^vi	46.9 (18)	C47^ii—C42—C39	129 (2)
C4^vi—C16—C39^v	85 (6)	C16^v—C42—C39	57.7 (18)
C23^ii—C16—C39^v	152 (3)	C23^vi—C42—C39	103.1 (19)
C42^v—C16—C39^v	80.6 (18)	C25^vii—C42—C39	130 (2)
C47^vi—C16—C39^v	127 (3)	C17^v—C42—C39	139.0 (15)
C4^vi—C16—C28^ii	160 (7)	C4^ii—C42—C39	53.9 (12)
C23^ii—C16—C28^ii	77.6 (18)	C5^v—C42—C39	23.5 (11)
C42^v—C16—C28^ii	5 (2)	C13^v—C42—C39	141.1 (17)
C47^vi—C16—C28^ii	51 (2)	C28^vi—C42—C40	140 (4)
C39^v—C16—C28^ii	76.4 (18)	C47^ii—C42—C40	21.2 (16)
C4^vi—C16—C40^v	106 (5)	C16^v—C42—C40	52.4 (16)
C23^ii—C16—C40^v	13.5 (17)	C23^vi—C42—C40	8.3 (11)
C42^v—C16—C40^v	85.4 (18)	C25^vii—C42—C40	111.1 (16)
C47^vi—C16—C40^v	39.0 (16)	C17^v—C42—C40	32.3 (10)
C39^v—C16—C40^v	157 (2)	C4^ii—C42—C40	55.6 (11)
C28^ii—C16—C40^v	88.9 (15)	C5^v—C42—C40	130.9 (16)
C4^vi—C16—C52^vii	27 (4)	C13^v—C42—C40	97.2 (12)
C23^ii—C16—C52^vii	93 (3)	C39—C42—C40	108.2 (11)
C42^v—C16—C52^vii	159 (2)	C28^vi—C42—C52	20 (3)
C47^vi—C16—C52^vii	119 (2)	C47^ii—C42—C52	103 (2)
C39^v—C16—C52^vii	108 (2)	C16^v—C42—C52	161.0 (18)
C28^ii—C16—C52^vii	159.3 (19)	C23^vi—C42—C52	127.9 (18)
C40^v—C16—C52^vii	79.8 (16)	C25^vii—C42—C52	9.9 (15)
C4^vi—C16—C25	19 (2)	C17^v—C42—C52	89.5 (14)
C23^ii—C16—C25	103 (2)	C4^ii—C42—C52	159.1 (16)
C42^v—C16—C25	160.6 (19)	C5^v—C42—C52	98.4 (17)
C47^vi—C16—C25	127.9 (19)	C13^v—C42—C52	23.7 (10)
C39^v—C16—C25	97.7 (17)	C39—C42—C52	120.3 (16)
C28^ii—C16—C25	158.3 (18)	C40—C42—C52	120.0 (12)
C40^v—C16—C25	89.7 (14)	C34^i—C44—C53^v	7 (6)
C52^vii—C16—C25	10.8 (16)	C34^i—C44—C20^ii	46 (4)
C4^vi—C16—C17	138 (5)	C53^v—C44—C20^ii	53 (5)
C23^ii—C16—C17	21.7 (16)	C34^i—C44—C35^i	150 (6)
C42^v—C16—C17	53.0 (16)	C53^v—C44—C35^i	144 (6)
C47^vi—C16—C17	7.8 (12)	C20^ii—C44—C35^i	151 (3)
C39^v—C16—C17	130.8 (15)	C34^i—C44—C11^iii	151 (5)
C28^ii—C16—C17	56.5 (12)	C53^v—C44—C11^iii	145 (6)
C40^v—C16—C17	32.4 (10)	C20^ii—C44—C11^iii	153 (4)
C52^vii—C16—C17	111.3 (17)	C35^i—C44—C11^iii	3 (2)
C25—C16—C17	120.3 (12)	C34^i—C44—C29^ii	45 (3)
C4^vi—C16—C5	109 (7)	C53^v—C44—C29^ii	38 (5)
C23^ii—C16—C5	130 (2)	C20^ii—C44—C29^ii	90 (3)
C42^v—C16—C5	57.0 (18)	C35^i—C44—C29^ii	107.6 (17)
C47^vi—C16—C5	103 (2)	C11^iii—C44—C29^ii	107.4 (18)
C39^v—C16—C5	23.6 (11)	C34^i—C44—C21^ii	147 (5)
C28^ii—C16—C5	52.9 (12)	C53^v—C44—C21^ii	153 (5)
C40^v—C16—C5	139.1 (16)	C20^ii—C44—C21^ii	105 (3)
C52^vii—C16—C5	131 (2)	C35^i—C44—C21^ii	49.1 (12)
C25—C16—C5	120.0 (17)	C11^iii—C44—C21^ii	50.5 (12)
C17—C16—C5	108.3 (11)	C29^ii—C44—C21^ii	150 (2)
C4^vi—C16—C5^vi	70 (6)	C34^i—C44—C13	24 (4)
C23^ii—C16—C5^vi	162 (3)	C53^v—C44—C13	17 (5)
C42^v—C16—C5^vi	95 (2)	C20^ii—C44—C13	69 (3)
C47^vi—C16—C5^vi	140 (3)	C35^i—C44—C13	127.2 (17)
C39^v—C16—C5^vi	15.3 (11)	C11^iii—C44—C13	127.5 (17)
C28^ii—C16—C5^vi	91.0 (13)	C29^ii—C44—C13	21.1 (9)
C40^v—C16—C5^vi	158 (2)	C21^ii—C44—C13	156.7 (15)
C52^vii—C16—C5^vi	93 (2)	C34^i—C44—C45	143 (5)
C25—C16—C5^vi	82.5 (16)	C53^v—C44—C45	137 (6)
C17—C16—C5^vi	142.8 (17)	C20^ii—C44—C45	156 (3)
C5—C16—C5^vi	38.5 (14)	C35^i—C44—C45	8.2 (8)
C47^vi—C17—C23^ii	39 (4)	C11^iii—C44—C45	8.1 (16)
C47^vi—C17—C40^v	70 (4)	C29^ii—C44—C45	99.5 (14)
C23^ii—C17—C40^v	31.0 (18)	C21^ii—C44—C45	57.2 (12)
C47^vi—C17—C46^vi	147 (4)	C13—C44—C45	119.5 (12)
C23^ii—C17—C46^vi	108 (2)	C34^i—C44—C21	97 (4)
C40^v—C17—C46^vi	77 (2)	C53^v—C44—C21	104 (5)
C47^vi—C17—C42^v	28 (5)	C20^ii—C44—C21	52 (2)
C23^ii—C17—C42^v	65 (2)	C35^i—C44—C21	100.9 (10)
C40^v—C17—C42^v	95 (2)	C11^iii—C44—C21	102.8 (13)
C46^vi—C17—C42^v	162 (3)	C29^ii—C44—C21	137.5 (16)
C47^vi—C17—C15^ii	133 (4)	C21^ii—C44—C21	52.8 (12)
C23^ii—C17—C15^ii	94 (2)	C13—C44—C21	118.5 (12)
C40^v—C17—C15^ii	62.8 (18)	C45—C44—C21	108.6 (8)
C46^vi—C17—C15^ii	14.1 (17)	C34^i—C44—C51^v	60 (4)
C42^v—C17—C15^ii	153 (2)	C53^v—C44—C51^v	67 (4)
C47^vi—C17—C28^ii	42 (4)	C20^ii—C44—C51^v	16 (2)
C23^ii—C17—C28^ii	80 (2)	C35^i—C44—C51^v	134.4 (16)
C40^v—C17—C28^ii	109 (2)	C11^iii—C44—C51^v	137.1 (19)
C46^vi—C17—C28^ii	161 (3)	C29^ii—C44—C51^v	102.8 (15)
C42^v—C17—C28^ii	14.8 (12)	C21^ii—C44—C51^v	89.4 (14)
C15^ii—C17—C28^ii	161 (3)	C13—C44—C51^v	82.3 (12)
C47^vi—C17—C41^v	146 (4)	C45—C44—C51^v	140.5 (13)
C23^ii—C17—C41^v	108 (2)	C21—C44—C51^v	37.1 (9)
C40^v—C17—C41^v	76.9 (17)	C34^i—C44—C52^v	42 (4)
C46^vi—C17—C41^v	5 (2)	C53^v—C44—C52^v	36 (5)
C42^v—C17—C41^v	157 (2)	C20^ii—C44—C52^v	87 (3)
C15^ii—C17—C41^v	14.8 (11)	C35^i—C44—C52^v	109.5 (17)
C28^ii—C17—C41^v	155.7 (19)	C11^iii—C44—C52^v	109.5 (17)
C47^vi—C17—C27	139 (4)	C29^ii—C44—C52^v	4.1 (11)
C23^ii—C17—C27	100.3 (19)	C21^ii—C44—C52^v	149.9 (17)
C40^v—C17—C27	69.4 (18)	C13—C44—C52^v	18.3 (9)
C46^vi—C17—C27	8.6 (15)	C45—C44—C52^v	101.5 (13)
C42^v—C17—C27	154.6 (19)	C21—C44—C52^v	133.5 (14)
C15^ii—C17—C27	7.6 (13)	C51^v—C44—C52^v	99.1 (13)
C28^ii—C17—C27	157.7 (16)	C11^iii—C45—C35^i	12 (7)
C41^v—C17—C27	7.5 (12)	C11^iii—C45—C26^ii	112 (5)
C47^vi—C17—C16	21 (4)	C35^i—C45—C26^ii	113.3 (18)
C23^ii—C17—C16	23 (2)	C11^iii—C45—C27^i	152 (6)
C40^v—C17—C16	53 (2)	C35^i—C45—C27^i	143 (5)
C46^vi—C17—C16	127.3 (18)	C26^ii—C45—C27^i	94 (2)
C42^v—C17—C16	42.3 (11)	C11^iii—C45—C15^iii	139 (5)
C15^ii—C17—C16	113.7 (16)	C35^i—C45—C15^iii	133 (4)
C28^ii—C17—C16	56.8 (12)	C26^ii—C45—C15^iii	106 (3)
C41^v—C17—C16	125.7 (15)	C27^i—C45—C15^iii	12.9 (13)
C27—C17—C16	118.9 (13)	C11^iii—C45—C41^ii	155 (6)
C47^vi—C17—C13	95 (5)	C35^i—C45—C41^ii	146 (5)
C23^ii—C17—C13	131 (2)	C26^ii—C45—C41^ii	89 (2)
C40^v—C17—C13	156 (3)	C27^i—C45—C41^ii	4.3 (12)
C46^vi—C17—C13	115.5 (14)	C15^iii—C45—C41^ii	17.0 (11)
C42^v—C17—C13	67.1 (13)	C11^iii—C45—C21^ii	34 (4)
C15^ii—C17—C13	128.3 (12)	C35^i—C45—C21^ii	34.6 (11)
C28^ii—C17—C13	52.4 (11)	C26^ii—C45—C21^ii	79.1 (17)
C41^v—C17—C13	113.6 (11)	C27^i—C45—C21^ii	158 (3)
C27—C17—C13	120.8 (8)	C15^iii—C45—C21^ii	158 (3)
C16—C17—C13	108.0 (10)	C41^ii—C45—C21^ii	155 (3)
C47^vi—C17—C25^i	77 (4)	C11^iii—C45—C46	146 (5)
C23^ii—C17—C25^i	114 (2)	C35^i—C45—C46	138 (4)
C40^v—C17—C25^i	142 (3)	C26^ii—C45—C46	99 (2)
C46^vi—C17—C25^i	132 (2)	C27^i—C45—C46	5.7 (12)
C42^v—C17—C25^i	49.8 (14)	C15^iii—C45—C46	7.4 (14)
C15^ii—C17—C25^i	143.4 (16)	C41^ii—C45—C46	9.7 (11)
C28^ii—C17—C25^i	35.1 (10)	C21^ii—C45—C46	158 (2)
C41^v—C17—C25^i	129.1 (15)	C11^iii—C45—C14	89 (4)
C27—C17—C25^i	135.8 (12)	C35^i—C45—C14	89.9 (8)
C16—C17—C25^i	91.0 (15)	C26^ii—C45—C14	23.5 (17)
C13—C17—C25^i	17.3 (11)	C27^i—C45—C14	115.3 (15)
C34^v—C20—C53^i	8 (6)	C15^iii—C45—C14	127.9 (19)
C34^v—C20—C44^ii	53 (5)	C41^ii—C45—C14	111.0 (15)
C53^i—C20—C44^ii	45 (4)	C21^ii—C45—C14	55.6 (11)
C34^v—C20—C51^i	145 (6)	C46—C45—C14	120.5 (12)
C53^i—C20—C51^i	152 (5)	C11^iii—C45—C44	26 (5)
C44^ii—C20—C51^i	156 (3)	C35^i—C45—C44	19.1 (18)
C34^v—C20—C3^iii	145 (6)	C26^ii—C45—C44	131 (2)
C53^i—C20—C3^iii	153 (5)	C27^i—C45—C44	126 (2)
C44^ii—C20—C3^iii	159 (3)	C15^iii—C45—C44	114.1 (18)
C51^i—C20—C3^iii	5 (2)	C41^ii—C45—C44	128.6 (18)
C34^v—C20—C21^ii	158 (5)	C21^ii—C45—C44	53.4 (11)
C53^i—C20—C21^ii	151 (4)	C46—C45—C44	120.3 (14)
C44^ii—C20—C21^ii	109 (3)	C14—C45—C44	108.0 (10)
C51^i—C20—C21^ii	48.5 (12)	C11^iii—C45—C3^iii	74 (4)
C3^iii—C20—C21^ii	50.6 (12)	C35^i—C45—C3^iii	76.1 (15)
C34^v—C20—C13^ii	37 (5)	C26^ii—C45—C3^iii	37.6 (13)
C53^i—C20—C13^ii	45 (3)	C27^i—C45—C3^iii	129 (2)
C44^ii—C20—C13^ii	90 (3)	C15^iii—C45—C3^iii	141 (3)
C51^i—C20—C13^ii	108.4 (17)	C41^ii—C45—C3^iii	125 (2)
C3^iii—C20—C13^ii	107.9 (18)	C21^ii—C45—C3^iii	41.6 (12)
C21^ii—C20—C13^ii	152 (2)	C46—C45—C3^iii	134.2 (17)
C34^v—C20—C29	17 (5)	C14—C45—C3^iii	14.3 (13)
C53^i—C20—C29	25 (4)	C44—C45—C3^iii	94.6 (15)
C44^ii—C20—C29	69 (3)	C11^iii—C45—C51^i	71 (4)
C51^i—C20—C29	128.0 (18)	C35^i—C45—C51^i	72.3 (9)
C3^iii—C20—C29	128.2 (17)	C26^ii—C45—C51^i	41.0 (17)
C21^ii—C20—C29	158.8 (16)	C27^i—C45—C51^i	130.4 (18)
C13^ii—C20—C29	21.1 (9)	C15^iii—C45—C51^i	142 (2)
C34^v—C20—C14	137 (6)	C41^ii—C45—C51^i	126.1 (17)
C53^i—C20—C14	145 (5)	C21^ii—C45—C51^i	38.1 (11)
C44^ii—C20—C14	162 (3)	C46—C45—C51^i	135.1 (15)
C51^i—C20—C14	8.2 (8)	C14—C45—C51^i	17.6 (9)
C3^iii—C20—C14	8.5 (17)	C44—C45—C51^i	90.5 (12)
C21^ii—C20—C14	56.6 (12)	C3^iii—C45—C51^i	5 (2)
C13^ii—C20—C14	100.3 (13)	C15^iii—C46—C41^ii	78 (7)
C29—C20—C14	120.2 (12)	C15^iii—C46—C27^i	47 (5)
C34^v—C20—C21	107 (5)	C41^ii—C46—C27^i	31 (5)
C53^i—C20—C21	99 (4)	C15^iii—C46—C17^i	103 (6)
C44^ii—C20—C21	56 (3)	C41^ii—C46—C17^i	155 (10)
C51^i—C20—C21	100.9 (9)	C27^i—C46—C17^i	144 (7)
C3^iii—C20—C21	103.6 (13)	C15^iii—C46—C14^iii	141 (6)
C21^ii—C20—C21	53.2 (13)	C41^ii—C46—C14^iii	64 (6)
C13^ii—C20—C21	139.1 (15)	C27^i—C46—C14^iii	95 (4)
C29—C20—C21	119.7 (12)	C17^i—C46—C14^iii	110 (2)
C14—C20—C21	108.6 (8)	C15^iii—C46—C40^ii	63 (6)
C34^v—C20—C35^v	69 (5)	C41^ii—C46—C40^ii	133 (7)
C53^i—C20—C35^v	61 (4)	C27^i—C46—C40^ii	107 (5)
C44^ii—C20—C35^v	20 (2)	C17^i—C46—C40^ii	40.0 (12)
C51^i—C20—C35^v	136.0 (15)	C14^iii—C46—C40^ii	146 (3)
C3^iii—C20—C35^v	139.8 (19)	C15^iii—C46—C45	30 (5)
C21^ii—C20—C35^v	91.1 (14)	C41^ii—C46—C45	48 (6)
C13^ii—C20—C35^v	102.8 (15)	C27^i—C46—C45	17 (4)
C29—C20—C35^v	82.1 (12)	C17^i—C46—C45	128 (2)
C14—C20—C35^v	142.3 (12)	C14^iii—C46—C45	111.2 (17)
C21—C20—C35^v	38.4 (9)	C40^ii—C46—C45	89.8 (14)
C34^v—C20—C11^vi	68 (5)	C15^iii—C46—C3	150 (6)
C53^i—C20—C11^vi	61 (3)	C41^ii—C46—C3	73 (6)
C44^ii—C20—C11^vi	19 (3)	C27^i—C46—C3	104 (4)
C51^i—C20—C11^vi	137.3 (14)	C17^i—C46—C3	100.5 (18)
C3^iii—C20—C11^vi	140.9 (15)	C14^iii—C46—C3	9.9 (15)
C21^ii—C20—C11^vi	91.8 (14)	C40^ii—C46—C3	138 (2)
C13^ii—C20—C11^vi	102.9 (13)	C45—C46—C3	120.5 (12)
C29—C20—C11^vi	82.1 (9)	C15^iii—C46—C47	94 (6)
C14—C20—C11^vi	143.8 (13)	C41^ii—C46—C47	152 (9)
C21—C20—C11^vi	38.8 (8)	C27^i—C46—C47	136 (6)
C35^v—C20—C11^vi	2.0 (17)	C17^i—C46—C47	8.9 (12)
C51^v—C21—C35^v	98 (2)	C14^iii—C46—C47	118 (2)
C51^v—C21—C3^vi	7 (3)	C40^ii—C46—C47	31.1 (12)
C35^v—C21—C3^vi	94.8 (19)	C45—C46—C47	119.6 (14)
C51^v—C21—C11^vi	94.3 (18)	C3—C46—C47	108.8 (13)
C35^v—C21—C11^vi	6 (3)	C15^iii—C46—C23^iii	74 (6)
C3^vi—C21—C11^vi	90.4 (17)	C41^ii—C46—C23^iii	142 (7)
C51^v—C21—C20^ii	55.4 (16)	C27^i—C46—C23^iii	118 (5)
C35^v—C21—C20^ii	149 (2)	C17^i—C46—C23^iii	28.7 (11)
C3^vi—C21—C20^ii	60.6 (19)	C14^iii—C46—C23^iii	137 (3)
C11^vi—C21—C20^ii	147.6 (17)	C40^ii—C46—C23^iii	11.3 (10)
C51^v—C21—C21^ii	127 (2)	C45—C46—C23^iii	100.7 (14)
C35^v—C21—C21^ii	125 (2)	C3—C46—C23^iii	127.4 (18)
C3^vi—C21—C21^ii	133 (2)	C47—C46—C23^iii	19.8 (10)
C11^vi—C21—C21^ii	130.9 (19)	C15^iii—C46—C51^ii	150 (7)
C20^ii—C21—C21^ii	73.3 (14)	C41^ii—C46—C51^ii	75 (6)
C51^v—C21—C44^ii	149 (2)	C27^i—C46—C51^ii	106 (4)
C35^v—C21—C44^ii	54.2 (16)	C17^i—C46—C51^ii	97 (2)
C3^vi—C21—C44^ii	147.8 (17)	C14^iii—C46—C51^ii	13.2 (12)
C11^vi—C21—C44^ii	59.3 (17)	C40^ii—C46—C51^ii	134 (3)
C20^ii—C21—C44^ii	143 (2)	C45—C46—C51^ii	121.0 (13)
C21^ii—C21—C44^ii	72.5 (14)	C3—C46—C51^ii	5 (2)
C51^v—C21—C14^ii	15.7 (11)	C47—C46—C51^ii	105.2 (17)
C35^v—C21—C14^ii	82.9 (17)	C23^iii—C46—C51^ii	123 (2)
C3^vi—C21—C14^ii	12.4 (15)	C15^iii—C46—C26^i	113 (5)
C11^vi—C21—C14^ii	78.7 (15)	C41^ii—C46—C26^i	35 (6)
C20^ii—C21—C14^ii	71.0 (12)	C27^i—C46—C26^i	66 (3)
C21^ii—C21—C14^ii	141.7 (17)	C17^i—C46—C26^i	135 (2)
C44^ii—C21—C14^ii	135.4 (18)	C14^iii—C46—C26^i	28.7 (12)
C51^v—C21—C45^ii	83.1 (17)	C40^ii—C46—C26^i	154 (3)
C35^v—C21—C45^ii	15.3 (11)	C45—C46—C26^i	82.6 (10)
C3^vi—C21—C45^ii	79.5 (15)	C3—C46—C26^i	38.4 (8)
C11^vi—C21—C45^ii	11.4 (14)	C47—C46—C26^i	141.2 (16)
C20^ii—C21—C45^ii	136.3 (19)	C23^iii—C46—C26^i	152 (3)
C21^ii—C21—C45^ii	139.1 (18)	C51^ii—C46—C26^i	40.2 (10)
C44^ii—C21—C45^ii	69.5 (11)	C23^iii—C47—C17^i	110 (6)
C14^ii—C21—C45^ii	67.7 (12)	C23^iii—C47—C40^ii	31 (3)
C51^v—C21—C26	48.9 (15)	C17^i—C47—C40^ii	79 (4)
C35^v—C21—C26	49.5 (15)	C23^iii—C47—C42^ii	107 (4)
C3^vi—C21—C26	45.3 (11)	C17^i—C47—C42^ii	139 (6)
C11^vi—C21—C26	45.4 (11)	C40^ii—C47—C42^ii	135 (3)
C20^ii—C21—C26	103.4 (12)	C23^iii—C47—C16^i	46 (3)
C21^ii—C21—C26	158.1 (8)	C17^i—C47—C16^i	151 (5)
C44^ii—C21—C26	103.0 (12)	C40^ii—C47—C16^i	76 (2)
C14^ii—C21—C26	33.4 (9)	C42^ii—C47—C16^i	60 (2)
C45^ii—C21—C26	34.3 (9)	C23^iii—C47—C28^iii	123 (5)
C51^v—C21—C44	73.9 (17)	C17^i—C47—C28^iii	122 (5)
C35^v—C21—C44	158 (2)	C40^ii—C47—C28^iii	150 (4)
C3^vi—C21—C44	79.2 (16)	C42^ii—C47—C28^iii	16.7 (19)
C11^vi—C21—C44	160.5 (19)	C16^i—C47—C28^iii	77 (3)
C20^ii—C21—C44	18.7 (12)	C23^iii—C47—C4	38 (4)
C21^ii—C21—C44	54.7 (11)	C17^i—C47—C4	143 (4)
C44^ii—C21—C44	125.8 (13)	C40^ii—C47—C4	67.7 (19)
C14^ii—C21—C44	89.3 (12)	C42^ii—C47—C4	68.8 (19)
C45^ii—C21—C44	151.0 (17)	C16^i—C47—C4	8.6 (15)
C26—C21—C44	120.9 (8)	C28^iii—C47—C4	85.1 (17)
C51^v—C21—C20	157 (2)	C23^iii—C47—C46	86 (4)
C35^v—C21—C20	72.6 (17)	C17^i—C47—C46	24 (3)
C3^vi—C21—C20	160.6 (19)	C40^ii—C47—C46	54.7 (18)
C11^vi—C21—C20	78.0 (14)	C42^ii—C47—C46	155 (2)
C20^ii—C21—C20	124.8 (13)	C16^i—C47—C46	128.5 (19)
C21^ii—C21—C20	53.4 (11)	C28^iii—C47—C46	142.4 (17)
C44^ii—C21—C20	19.1 (12)	C4—C47—C46	120.2 (14)
C14^ii—C21—C20	149.6 (16)	C23^iii—C47—C15^iii	75 (3)
C45^ii—C21—C20	87.7 (12)	C17^i—C47—C15^iii	35 (3)
C26—C21—C20	120.1 (8)	C40^ii—C47—C15^iii	43.4 (18)
C44—C21—C20	106.9 (8)	C42^ii—C47—C15^iii	159 (3)
C47^iii—C23—C40^i	108 (6)	C16^i—C47—C15^iii	117.7 (19)
C47^iii—C23—C17^ii	31 (3)	C28^iii—C47—C15^iii	151 (2)
C40^i—C23—C17^ii	78 (4)	C4—C47—C15^iii	109.2 (15)
C47^iii—C23—C16^ii	107 (4)	C46—C47—C15^iii	11.4 (13)
C40^i—C23—C16^ii	139 (6)	C23^iii—C47—C25^iv	155 (6)
C17^ii—C23—C16^ii	135 (3)	C17^i—C47—C25^iv	87 (4)
C47^iii—C23—C4^iii	124 (5)	C40^ii—C47—C25^iv	155 (2)
C40^i—C23—C4^iii	122 (5)	C42^ii—C47—C25^iv	52 (2)
C17^ii—C23—C4^iii	151 (4)	C16^i—C47—C25^iv	111 (3)
C16^ii—C23—C4^iii	18 (2)	C28^iii—C47—C25^iv	35.8 (13)
C47^iii—C23—C42^i	47 (3)	C4—C47—C25^iv	118 (2)
C40^i—C23—C42^i	149 (4)	C46—C47—C25^iv	108.4 (12)
C17^ii—C23—C42^i	76 (2)	C15^iii—C47—C25^iv	118.8 (13)
C16^ii—C23—C42^i	60 (2)	C23^iii—C47—C13^i	163 (6)
C4^iii—C23—C42^i	78 (3)	C17^i—C47—C13^i	70 (4)
C47^iii—C23—C15	85 (4)	C40^ii—C47—C13^i	144 (2)
C40^i—C23—C15	23 (3)	C42^ii—C47—C13^i	69 (2)
C17^ii—C23—C15	54.7 (18)	C16^i—C47—C13^i	127 (3)
C16^ii—C23—C15	155 (3)	C28^iii—C47—C13^i	52.6 (13)
C4^iii—C23—C15	141.8 (18)	C4—C47—C13^i	134 (2)
C42^i—C23—C15	127.9 (17)	C46—C47—C13^i	92.2 (13)
C47^iii—C23—C28	39 (4)	C15^iii—C47—C13^i	103.0 (14)
C40^i—C23—C28	142 (4)	C25^iv—C47—C13^i	16.7 (9)
C17^ii—C23—C28	68.2 (19)	C23^iii—C47—C27^i	79 (3)
C16^ii—C23—C28	67.7 (19)	C17^i—C47—C27^i	32 (3)
C4^iii—C23—C28	85.2 (17)	C40^ii—C47—C27^i	47.4 (18)
C42^i—C23—C28	7.8 (13)	C42^ii—C47—C27^i	155 (3)
C15—C23—C28	120.2 (14)	C16^i—C47—C27^i	120.3 (18)
C47^iii—C23—C46^iii	74 (3)	C28^iii—C47—C27^i	146 (2)
C40^i—C23—C46^iii	34 (3)	C4—C47—C27^i	112.0 (13)
C17^ii—C23—C46^iii	43.4 (17)	C46—C47—C27^i	8.3 (10)
C16^ii—C23—C46^iii	159 (3)	C15^iii—C47—C27^i	5.1 (11)
C4^iii—C23—C46^iii	151 (3)	C25^iv—C47—C27^i	114.0 (10)
C42^i—C23—C46^iii	117.3 (17)	C13^i—C47—C27^i	98.3 (12)
C15—C23—C46^iii	11.3 (13)	C3^ii—C51—C14^vi	44 (10)
C28—C23—C46^iii	109.5 (14)	C3^ii—C51—C21^v	116 (10)
C47^iii—C23—C52^iv	155 (6)	C14^vi—C51—C21^v	130.6 (19)
C40^i—C23—C52^iv	87 (4)	C3^ii—C51—C20^vi	136 (10)
C17^ii—C23—C52^iv	155 (2)	C14^vi—C51—C20^vi	153 (2)
C16^ii—C23—C52^iv	54 (2)	C21^v—C51—C20^vi	76.0 (19)
C4^iii—C23—C52^iv	35.9 (14)	C3^ii—C51—C26^v	62 (10)
C42^i—C23—C52^iv	112 (3)	C14^vi—C51—C26^v	42.4 (13)
C15—C23—C52^iv	107.9 (11)	C21^v—C51—C26^v	88.7 (17)
C28—C23—C52^iv	118.7 (19)	C20^vi—C51—C26^v	160 (2)
C46^iii—C23—C52^iv	118.5 (11)	C3^ii—C51—C34^vii	136 (10)
C47^iii—C23—C29^i	162 (6)	C14^vi—C51—C34^vii	144 (2)
C40^i—C23—C29^i	70 (4)	C21^v—C51—C34^vii	84 (2)
C17^ii—C23—C29^i	143 (2)	C20^vi—C51—C34^vii	8.8 (14)
C16^ii—C23—C29^i	70 (2)	C26^v—C51—C34^vii	162 (3)
C4^iii—C23—C29^i	52.1 (13)	C3^ii—C51—C53	137 (10)
C42^i—C23—C29^i	127 (3)	C14^vi—C51—C53	146 (2)
C15—C23—C29^i	91.9 (12)	C21^v—C51—C53	82.4 (18)
C28—C23—C29^i	133 (2)	C20^vi—C51—C53	7.6 (15)
C46^iii—C23—C29^i	102.8 (13)	C26^v—C51—C53	161 (2)
C52^iv—C23—C29^i	16.3 (8)	C34^vii—C51—C53	1.5 (13)
C47^iii—C23—C27^ii	84 (3)	C3^ii—C51—C35	93 (10)
C40^i—C23—C27^ii	25 (3)	C14^vi—C51—C35	89.7 (8)
C17^ii—C23—C27^ii	53.6 (15)	C21^v—C51—C35	41.6 (14)
C16^ii—C23—C27^ii	152 (3)	C20^vi—C51—C35	115.8 (15)
C4^iii—C23—C27^ii	141 (2)	C26^v—C51—C35	47.3 (13)
C42^i—C23—C27^ii	125.6 (16)	C34^vii—C51—C35	122.4 (17)
C15—C23—C27^ii	3.5 (13)	C53—C51—C35	120.9 (12)
C28—C23—C27^ii	118.0 (12)	C3^ii—C51—C41	64 (10)
C46^iii—C23—C27^ii	10.7 (9)	C14^vi—C51—C41	27 (3)
C52^iv—C23—C27^ii	107.8 (10)	C21^v—C51—C41	147.8 (17)
C29^i—C23—C27^ii	92.1 (12)	C20^vi—C51—C41	127.9 (17)
C52^vii—C25—C13^vi	100 (8)	C26^v—C51—C41	62.4 (14)
C52^vii—C25—C29^v	45 (6)	C34^vii—C51—C41	119.1 (16)
C13^vi—C25—C29^v	55 (4)	C53—C51—C41	120.4 (13)
C52^vii—C25—C28^v	122 (7)	C35—C51—C41	107.6 (10)
C13^vi—C25—C28^v	138 (5)	C3^ii—C51—C11^ii	88 (10)
C29^v—C25—C28^v	163 (4)	C14^vi—C51—C11^ii	85.8 (16)
C52^vii—C25—C4^vi	47 (6)	C21^v—C51—C11^ii	45.0 (12)
C13^vi—C25—C4^vi	145 (5)	C20^vi—C51—C11^ii	120 (2)
C29^v—C25—C4^vi	91 (3)	C26^v—C51—C11^ii	43.7 (12)
C28^v—C25—C4^vi	74 (2)	C34^vii—C51—C11^ii	127 (3)
C52^vii—C25—C42^vii	132 (8)	C53—C51—C11^ii	125.4 (19)
C13^vi—C25—C42^vii	127 (4)	C35—C51—C11^ii	4.8 (19)
C29^v—C25—C42^vii	167 (4)	C41—C51—C11^ii	104.9 (14)
C28^v—C25—C42^vii	11.4 (16)	C3^ii—C51—C46^ii	67 (10)
C4^vi—C25—C42^vii	85 (3)	C14^vi—C51—C46^ii	35 (2)
C52^vii—C25—C16	43 (7)	C21^v—C51—C46^ii	158 (2)
C13^vi—C25—C16	139 (4)	C20^vi—C51—C46^ii	118.3 (19)
C29^v—C25—C16	85 (2)	C26^v—C51—C46^ii	73.0 (16)
C28^v—C25—C16	79.2 (18)	C34^vii—C51—C46^ii	109.6 (18)
C4^vi—C25—C16	6.3 (9)	C53—C51—C46^ii	110.9 (16)
C42^vii—C25—C16	89.3 (18)	C35—C51—C46^ii	118.2 (14)
C52^vii—C25—C53^vii	81 (6)	C41—C51—C46^ii	10.7 (9)
C13^vi—C25—C53^vii	21 (3)	C11^ii—C51—C46^ii	115.6 (18)
C29^v—C25—C53^vii	36.8 (19)	C3^ii—C51—C44^v	142 (10)
C28^v—C25—C53^vii	152 (3)	C14^vi—C51—C44^v	159 (3)
C4^vi—C25—C53^vii	124 (2)	C21^v—C51—C44^v	69.0 (17)
C42^vii—C25—C53^vii	141 (2)	C20^vi—C51—C44^v	7.7 (11)
C16—C25—C53^vii	118.4 (17)	C26^v—C51—C44^v	153 (2)
C52^vii—C25—C17^vi	168 (7)	C34^vii—C51—C44^v	14.9 (11)
C13^vi—C25—C17^vi	77 (4)	C53—C51—C44^v	13.4 (9)
C29^v—C25—C17^vi	130 (3)	C35—C51—C44^v	108.2 (13)
C28^v—C25—C17^vi	61.4 (18)	C41—C51—C44^v	132.8 (15)
C4^vi—C25—C17^vi	133 (3)	C11^ii—C51—C44^v	113 (2)
C42^vii—C25—C17^vi	50.2 (13)	C46^ii—C51—C44^v	123.8 (19)
C16—C25—C17^vi	136 (2)	C29^vi—C52—C25^vii	104 (8)
C53^vii—C25—C17^vi	92.8 (15)	C29^vi—C52—C13^v	56 (4)
C52^vii—C25—C47^iv	164 (9)	C25^vii—C52—C13^v	48 (6)
C13^vi—C25—C47^iv	93 (3)	C29^vi—C52—C4^v	136 (5)
C29^v—C25—C47^iv	145 (2)	C25^vii—C52—C4^v	117 (7)
C28^v—C25—C47^iv	45 (2)	C13^v—C52—C4^v	162 (4)
C4^vi—C25—C47^iv	118 (3)	C29^vi—C52—C28^vi	145 (4)
C42^vii—C25—C47^iv	34.3 (14)	C25^vii—C52—C28^vi	43 (6)
C16—C25—C47^iv	122 (2)	C13^v—C52—C28^vi	91 (3)
C53^vii—C25—C47^iv	108.6 (14)	C4^v—C52—C28^vi	74 (2)
C17^vi—C25—C47^iv	16.0 (9)	C29^vi—C52—C53	18 (3)
C52^vii—C25—C34	84 (6)	C25^vii—C52—C53	86 (6)
C13^vi—C25—C34	19 (3)	C13^v—C52—C53	40 (2)
C29^v—C25—C34	39 (2)	C4^v—C52—C53	148 (2)
C28^v—C25—C34	149 (2)	C28^vi—C52—C53	127.1 (19)
C4^vi—C25—C34	127 (2)	C29^vi—C52—C16^vii	125 (4)
C42^vii—C25—C34	138.5 (19)	C25^vii—C52—C16^vii	126 (8)
C16—C25—C34	120.7 (14)	C13^v—C52—C16^vii	164 (4)
C53^vii—C25—C34	2.5 (16)	C4^v—C52—C16^vii	10.8 (16)
C17^vi—C25—C34	90.4 (14)	C28^vi—C52—C16^vii	83 (3)
C47^iv—C25—C34	106.2 (14)	C53—C52—C16^vii	137.9 (19)
C52^vii—C25—C23^ii	20 (7)	C29^vi—C52—C34^vii	21 (3)
C13^vi—C25—C23^ii	113 (4)	C25^vii—C52—C34^vii	84 (6)
C29^v—C25—C23^ii	59 (2)	C13^v—C52—C34^vii	37 (2)
C28^v—C25—C23^ii	105 (2)	C4^v—C52—C34^vii	150 (3)
C4^vi—C25—C23^ii	32.3 (14)	C28^vi—C52—C34^vii	125 (2)
C42^vii—C25—C23^ii	114.8 (19)	C53—C52—C34^vii	2.6 (16)
C16—C25—C23^ii	26.7 (10)	C16^vii—C52—C34^vii	140 (2)
C53^vii—C25—C23^ii	92.3 (16)	C29^vi—C52—C42	139 (4)
C17^vi—C25—C23^ii	153 (2)	C25^vii—C52—C42	38 (7)
C47^iv—C25—C23^ii	144 (2)	C13^v—C52—C42	85 (2)
C34—C25—C23^ii	94.7 (14)	C4^v—C52—C42	79.0 (18)
C14^ii—C26—C45^ii	132 (3)	C28^vi—C52—C42	6.5 (10)
C14^ii—C26—C3^vi	20 (2)	C53—C52—C42	120.6 (14)
C45^ii—C26—C3^vi	113 (2)	C16^vii—C52—C42	88.3 (18)
C14^ii—C26—C11^vi	113 (2)	C34^vii—C52—C42	118.1 (18)
C45^ii—C26—C11^vi	20 (2)	C29^vi—C52—C23^iv	92 (3)
C3^vi—C26—C11^vi	93.1 (17)	C25^vii—C52—C23^iv	156 (9)
C14^ii—C26—C51^v	23.4 (14)	C13^v—C52—C23^iv	145 (3)
C45^ii—C26—C51^v	109 (3)	C4^v—C52—C23^iv	44.2 (19)
C3^vi—C26—C51^v	7 (3)	C28^vi—C52—C23^iv	116 (3)
C11^vi—C26—C51^v	89.5 (19)	C53—C52—C23^iv	106.6 (14)
C14^ii—C26—C35^v	109 (3)	C16^vii—C52—C23^iv	33.7 (14)
C45^ii—C26—C35^v	22.9 (14)	C34^vii—C52—C23^iv	109.1 (14)
C3^vi—C26—C35^v	90.2 (19)	C42—C52—C23^iv	120.5 (18)
C11^vi—C26—C35^v	5 (3)	C29^vi—C52—C40^vi	76 (3)
C51^v—C26—C35^v	86 (2)	C25^vii—C52—C40^vi	161 (8)
C14^ii—C26—C41^v	52.3 (18)	C13^v—C52—C40^vi	130 (3)
C45^ii—C26—C41^v	162 (3)	C4^v—C52—C40^vi	60.1 (17)
C3^vi—C26—C41^v	71.7 (17)	C28^vi—C52—C40^vi	130 (3)
C11^vi—C26—C41^v	158 (2)	C53—C52—C40^vi	90.8 (14)
C51^v—C26—C41^v	73.5 (13)	C16^vii—C52—C40^vi	49.4 (13)
C35^v—C26—C41^v	152 (2)	C34^vii—C52—C40^vi	93.3 (15)
C14^ii—C26—C27^v	164 (3)	C42—C52—C40^vi	134 (2)
C45^ii—C26—C27^v	50.8 (18)	C23^iv—C52—C40^vi	15.9 (8)
C3^vi—C26—C27^v	158 (2)	C29^vi—C52—C44^v	12 (3)
C11^vi—C26—C27^v	70.2 (17)	C25^vii—C52—C44^v	94 (6)
C51^v—C26—C27^v	151 (2)	C13^v—C52—C44^v	48 (2)
C35^v—C26—C27^v	72.0 (12)	C4^v—C52—C44^v	141 (2)
C41^v—C26—C27^v	119.3 (18)	C28^vi—C52—C44^v	133.9 (18)
C14^ii—C26—C21	65.6 (18)	C53—C52—C44^v	8.1 (12)
C45^ii—C26—C21	66.6 (18)	C16^vii—C52—C44^v	130.3 (18)
C3^vi—C26—C21	46.4 (13)	C34^vii—C52—C44^v	10.7 (11)
C11^vi—C26—C21	47.1 (12)	C42—C52—C44^v	127.4 (13)
C51^v—C26—C21	42.4 (13)	C23^iv—C52—C44^v	98.5 (11)
C35^v—C26—C21	43.8 (13)	C40^vi—C52—C44^v	82.7 (12)
C41^v—C26—C21	114.6 (11)	C34^vii—C53—C44^v	131 (10)
C27^v—C26—C21	114.5 (12)	C34^vii—C53—C20^vi	50 (10)
C14^ii—C26—C27	58.4 (19)	C44^v—C53—C20^vi	82 (5)
C45^ii—C26—C27	160 (3)	C34^vii—C53—C29^vi	98 (10)
C3^vi—C26—C27	77.8 (14)	C44^v—C53—C29^vi	130 (6)
C11^vi—C26—C27	161 (2)	C20^vi—C53—C29^vi	146 (5)
C51^v—C26—C27	79.5 (14)	C34^vii—C53—C13^v	70 (10)
C35^v—C26—C27	155 (2)	C44^v—C53—C13^v	157 (6)
C41^v—C26—C27	6.1 (11)	C20^vi—C53—C13^v	120 (4)
C27^v—C26—C27	113.6 (12)	C29^vi—C53—C13^v	27.5 (12)
C21—C26—C27	120.3 (8)	C34^vii—C53—C52	91 (10)
C14^ii—C26—C41	160 (3)	C44^v—C53—C52	136 (6)
C45^ii—C26—C41	57.3 (19)	C20^vi—C53—C52	139 (5)
C3^vi—C26—C41	161 (2)	C29^vi—C53—C52	7.5 (13)
C11^vi—C26—C41	76.6 (14)	C13^v—C53—C52	20.8 (13)
C51^v—C26—C41	154 (2)	C34^vii—C53—C35^vii	150 (10)
C35^v—C26—C41	78.3 (14)	C44^v—C53—C35^vii	27 (5)
C41^v—C26—C41	112.8 (12)	C20^vi—C53—C35^vii	104 (4)
C27^v—C26—C41	6.6 (11)	C29^vi—C53—C35^vii	104 (2)
C21—C26—C41	120.2 (8)	C13^v—C53—C35^vii	130 (3)
C27—C26—C41	107.0 (9)	C52—C53—C35^vii	110.1 (19)
C14^ii—C26—C26^v	113 (2)	C34^vii—C53—C51	33 (10)
C45^ii—C26—C26^v	111 (2)	C44^v—C53—C51	99 (5)
C3^vi—C26—C26^v	132.0 (18)	C20^vi—C53—C51	20 (4)
C11^vi—C26—C26^v	129.3 (17)	C29^vi—C53—C51	127 (2)
C51^v—C26—C26^v	132.3 (18)	C13^v—C53—C51	100.5 (17)
C35^v—C26—C26^v	129.9 (18)	C52—C53—C51	119.0 (15)
C41^v—C26—C26^v	60.9 (11)	C35^vii—C53—C51	117.7 (16)
C27^v—C26—C26^v	59.8 (10)	C34^vii—C53—C25^vii	78 (10)
C21—C26—C26^v	156.9 (8)	C44^v—C53—C25^vii	148 (6)
C27—C26—C26^v	54.8 (9)	C20^vi—C53—C25^vii	126 (5)
C41—C26—C26^v	53.3 (9)	C29^vi—C53—C25^vii	20.0 (12)
C41^v—C27—C15^ii	105 (9)	C13^v—C53—C25^vii	8.7 (13)
C41^v—C27—C46^vi	51 (7)	C52—C53—C25^vii	12.7 (11)
C15^ii—C27—C46^vi	55 (7)	C35^vii—C53—C25^vii	122 (2)
C41^v—C27—C45^vi	150 (7)	C51—C53—C25^vii	106.8 (18)
C15^ii—C27—C45^vi	103 (7)	C34^vii—C53—C11^iv	152 (10)
C46^vi—C27—C45^vi	157 (5)	C44^v—C53—C11^iv	27 (5)
C41^v—C27—C14^ii	18 (6)	C20^vi—C53—C11^iv	106 (3)
C15^ii—C27—C14^ii	123 (7)	C29^vi—C53—C11^iv	103 (2)
C46^vi—C27—C14^ii	69 (4)	C13^v—C53—C11^iv	130 (2)
C45^vi—C27—C14^ii	133.1 (13)	C52—C53—C11^iv	109.5 (16)
C41^v—C27—C40^v	105 (8)	C35^vii—C53—C11^iv	2.6 (18)
C15^ii—C27—C40^v	17 (8)	C51—C53—C11^iv	119.8 (10)
C46^vi—C27—C40^v	58 (4)	C25^vii—C53—C11^iv	121 (2)
C45^vi—C27—C40^v	99.0 (18)	C34^vii—C53—C3^ii	31 (10)
C14^ii—C27—C40^v	121.3 (18)	C44^v—C53—C3^ii	101 (5)
C41^v—C27—C11^ii	155 (8)	C20^vi—C53—C3^ii	20 (4)
C15^ii—C27—C11^ii	96 (7)	C29^vi—C53—C3^ii	126 (2)
C46^vi—C27—C11^ii	150 (5)	C13^v—C53—C3^ii	100 (2)
C45^vi—C27—C11^ii	7.1 (15)	C52—C53—C3^ii	118.6 (17)
C14^ii—C27—C11^ii	138.7 (18)	C35^vii—C53—C3^ii	120 (2)
C40^v—C27—C11^ii	91.9 (16)	C51—C53—C3^ii	3.6 (16)
C41^v—C27—C26^v	115 (7)	C25^vii—C53—C3^ii	106.2 (19)
C15^ii—C27—C26^v	138 (7)	C11^iv—C53—C3^ii	122.4 (13)
C46^vi—C27—C26^v	166 (5)	C34^vii—C53—C21^v	69 (10)
C45^vi—C27—C26^v	35.7 (11)	C44^v—C53—C21^v	63 (4)
C14^ii—C27—C26^v	97.7 (15)	C20^vi—C53—C21^v	22 (3)
C40^v—C27—C26^v	132 (2)	C29^vi—C53—C21^v	156 (3)
C11^ii—C27—C26^v	42.1 (10)	C13^v—C53—C21^v	135 (2)
C41^v—C27—C17	72 (7)	C52—C53—C21^v	149.3 (18)
C15^ii—C27—C17	36 (6)	C35^vii—C53—C21^v	82.9 (14)
C46^vi—C27—C17	27 (5)	C51—C53—C21^v	36.2 (10)
C45^vi—C27—C17	131 (2)	C25^vii—C53—C21^v	139 (2)
C14^ii—C27—C17	88.7 (14)	C11^iv—C53—C21^v	84.7 (11)
C40^v—C27—C17	33.3 (9)	C3^ii—C53—C21^v	38.2 (9)
C11^ii—C27—C17	124.3 (17)

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