On the puzzling case of sodium saccharinate 1.875-hydrate: structure description in (3+1)-dimensional superspace

Rekis, T.; Schönleber, A.; van Smaalen, S.

doi:10.1107/S2052520619014938

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ISSN: 2052-5206

Volume 76| Part 1| February 2020| Pages 18-27

https://doi.org/10.1107/S2052520619014938

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On the puzzling case of sodium saccharinate 1.875-hydrate: structure description in (3+1)-dimensional superspace

Toms Rekis,^a Andreas Schönleber ^a and Sander van Smaalen ^a ^*

^aLaboratory of Crystallography, University of Bayreuth, Universitätsstrasse 30, 95447 Bayreuth, Germany
^*Correspondence e-mail: smash@uni-bayreuth.de

(Received 8 July 2019; accepted 5 November 2019)

The structure of sodium saccharinate 1.875-hydrate is presented in three- and (3+1)-dimensional space. The present model is more accurate than previously published superstructures, due to an excellent data set collected up to a high resolution of 0.89 Å⁻¹. The present study confirms the unusual complexity of the structure comprising a very large primitive unit cell with Z′ = 16. A much smaller degree of correlated disorder of parts of the unit cell is found than is present in the previously published models. As a result of pseudo-symmetry, the structure can be described in a higher-dimensional space. The X-ray diffraction data clearly indicate a (3+1)-dimensional periodic structure with stronger main reflections and weaker superstructure reflections. Furthermore, the structure is established as being commensurate. The structure description in superspace results in a four times smaller unit cell with an additional base centring of the lattice, resulting in an eightfold substructure (Z′ = 2) of the 3D superstructure. Therefore, such a superspace approach is desirable to work out this high-Z′ structure. The displacement and occupational modulation of the saccharinate anions have been studied, as well as their conformational variation along the fourth dimension.

Keywords: sodium saccharinate 1.875-hydrate; high-Z′ structures; superstructures; superspace; rigid-body modelling; commensurate structures.

CCDC references: 1963817; 1963818

1. Introduction

Usually, the lattice parameters, space-group symmetry and spatial arrangement of the atoms of the asymmetric unit are sufficient to describe a crystal structure considered as a static idealized state of matter. This formalism is the very essence of crystallography. For molecular crystals, in the vast majority of cases, there is only one molecule (or formula unit in the case of multi-component phases) in the asymmetric unit (Z′ = 1). It has been reported, however, that Z′ > 1 for around 8% of crystal structures (Steed, 2003 ). It is imaginable that sometimes larger aggregates can form from the constituent molecules. Such aggregates may possess no crystallographic symmetry, or if they do then it does not transfer to the space-group symmetry. For example, it does not seem unusual that efficiently interacting dimers or trimers could exist that are then packed according to some space-group symmetry. More intriguing, however, are cases for which Z′ is high (i.e. Z′ > 4; Brock, 2016 ). There have been a number of studies dealing with high-Z′ structures (Steed, 2003; Steed & Steed, 2015 ; Desiraju, 2007 ; Brock, 2016) and one of the conclusions is that sometimes such structures must be described as modulated, as considerable pseudo-symmetry can be identified.

Since the pioneering work of de Wolff and co-workers (Brouns et al., 1964 ; de Wolff, 1974 ) and Janner & Janssen (1977 ), modulated structures are well understood and the mathematical apparatus has been well established (Janssen et al., 2007 ; van Smaalen, 2007 ; Petricek et al., 1985 ). However, they perhaps do not gain the attention they deserve, especially in the field of chemical crystallography where the studied systems constitute molecular compounds (Schönleber, 2011 ). Moreover, high-Z′ structures of molecular crystals, should they give any indication of the presence of possible modulation, must be treated very cautiously. For example, incommensurately modulated structures may sometimes be relatively well approximated by a sufficiently large supercell in the conventional 3D space (Schönleber & Chapuis, 2004 ; Wagner & Schönleber, 2009 ). However, such an approximated structure model is fundamentally wrong. A description of a commensurately modulated structure in 3D space is fully valid, but a more sophisticated approach in a higher-dimensional space is found to be much more suitable when, for example, consecutive phase transformations including low-Z′ phases are to be analysed (Zuñiga et al., 1989 ; Harris et al., 1994 ; Schönleber et al., 2003 ) or the origins of the structure formation are to be explained (Dey et al., 2016 , 2018 ).

One example of a molecular crystal structure with a high Z′ value is that of sodium saccharinate 1.875-hydrate. The saccharinate chemical scheme is presented in Fig. 1. In spite of this artificial sweetener having been used in the food industry for over 100 years (Baran & Yilmaz, 2006 ), its crystal structure has been published only relatively recently (Naumov et al., 2005 ; Banerjee et al., 2005 ). The reason for that might be the unusual complexity of this Z′ = 16 structure. It is surprising that the large number of crystal constituents, comprising 16 saccharinate anions, 16 sodium cations and 30 water molecules, could be consistently arranged in a reproducible manner, replicated according to the space-group symmetry and then translated in all three directions. Furthermore, some of the entities in the asymmetric unit are disordered. The two independently elucidated structure models for crystals measured at around the same temperature (95 and 100 K) and published at nearly the same time are virtually identical, including the occupancies of the disordered sites. This indicates that the particular structural complexity of this organic salt hydrate is prevalent and does not arise from some specific experimental conditions of crystal growth or other non-equilibrium processes. In one of the studies (Naumov et al., 2005) it was pointed out that some pseudo-symmetry is present, but this only fully applies to the saccharinate ions. Nevertheless, it means that the structure could be described in a higher-dimensional space with a smaller unit cell and thus higher symmetry.

Figure 1
The chemical scheme of the saccharinate anion, with the atom numbering used in this study.

The aim of this study is to gain a deeper understanding of the sodium saccharinate 1.875-hydrate structure by describing it within the superspace approach and establishing its true commensurate or incommensurate nature.

2. Experimental

2.1. Materials

Sodium saccharinate hydrate (assay ≥99%) was purchased from Sigma–Aldrich and used without further purification. Deionized water was treated in a Millipore purification system. Single crystals were grown by slow evaporation from water solution. Transparent prismatic crystals of different sizes were obtained.

2.2. X-ray diffraction data collection

Single-crystal X-ray diffraction data were collected on a mar345dtb diffractometer equipped with an image-plate detector. A Bruker–Nonius rotating-anode X-ray generator was used with a wavelength of 0.56089 Å (Ag Kα radiation). A crystal of dimensions 0.22 × 0.35 × 0.45 mm was glued onto a glass fibre and coated with a thin layer of glue to prevent dehydration of the sample. An open-flow nitrogen cryostat was exploited for temperature regulation and the sample was cooled to 95 K with a cooling rate of 2 K min⁻¹. φ scans were performed with a step size of 1°. In total 360 frames were collected. An exposure time of 100 s per frame was used.

Data indexing and integration (with respect to the supercell structure previously reported in P2₁/n; Naumov et al., 2005; Banerjee et al., 2005) was performed up to the diffraction limit of 0.89 Å⁻¹ with the CrysAlisPro 39.46 software (Rigaku Oxford Diffraction, 2018 $[Rigaku Oxford Diffraction (2018). CrysAlis PRO. Rigaku Oxford Diffraction Yarnton, England]$ ). Outlier rejection according to the Laue class 2/m was applied. Empirical absorption correction using spherical harmonics, implemented in the SCALE3 ABSPACK scaling algorithm within the CrysAlisPro 39.46 software, was applied. The data are listed in Table 1.

Table 1
Summary of the X-ray diffraction data acquisition

Temperature (K)	95
Radiation type, wavelength (Å)	Ag Kα, λ = 0.56089
No. of reflections (cell measurement)	6894
θ range (°) (cell measurement)	2.84–29.89
Crystal size (mm)	0.22 × 0.35 × 0.45
T_min, T_max	0.912, 1
No. of measured, unique and observed [I > 3σ(I)] reflections	651 280, 88 532, 59 317
R_int (observed), R_int (unique)	0.0691, 0.0856
θ range (°) (data collection)	2.84–29.89
[sin(θ)/λ]_max (Å⁻¹)	0.89
Index ranges	−32 → h → 32
	−50 → k → 50
	−51 → l → 51

2.3. Structure refinement

2.3.1. Supercell structure

Structure refinements were performed with the software JANA2006 (Petříček et al., 2014 ). Initial non-H atom positions were taken from a published structure model (Banerjee et al., 2005). Non-H atoms were refined anisotropically. H atoms were added geometrically or located from the difference Fourier maps. Riding isotropic atomic displacement parameters (ADPs) were applied. No H atoms could be located for a few disordered water molecules with reduced site-occupancy factors. The data are listed in Table 2. The low R₁ and R_int values indicate the excellent fit of the refined structure model to the diffraction data. Furthermore, the use of silver radiation allowed the collection of good data up to an exceptionally high resolution of 0.89 Å⁻¹ for this light-atom structure. This is particularly important for an appropriate refinement of e.g. the ADPs. In Fig. 2 the number of observed and unobserved reflections [according to I > 3σ(I)] and the R₁ and R_int values (all cumulative) are plotted versus the resolution limit [sin(θ)/λ]_max. The R₁ value drops down to around 0.03 if the conventional limit for light-atom structures of 0.62 Å⁻¹ is chosen. At this limit, the R₁ values obtained in previous studies are 0.08 (Naumov et al., 2005) and 0.045 (Banerjee et al., 2005).

Table 2
Crystallographic data for the structure models in 3D and (3+1)D space

Parameter	3D	(3+1)D
Crystal data
Formula	Na(C₇H₄NO₃S)·1.875H₂O
Formula weight	238.94
Temperature (K)	95
Crystal system	Monoclinic
Space group	P2₁/n	C2/c(0,σ₂,0)s0
q, t₀		(0, 3/4, 0), 0
a (Å)	18.62120 (10)	18.62120 (10)
b (Å)	28.4622 (2)	7.11555 (5)
c (Å)	29.1642 (2)	29.1642 (2)
β (°)	93.4511 (6)	93.4511 (6)
V (Å³)	15429.00 (17)	3857.25 (4)
Z, Z′	64, 16	16, 2
F(000)	7845	1904
D_x (g cm⁻³)	1.6446	1.6446
μ (mm⁻¹)	0.201	0.201

Refinement
Refinement method	Full-matrix least-squares on F
R₁ [F² > 3σ(F²)], wR(F²), S	0.048, 0.055, 1.57	0.054, 0.065, 1.87
R_m=0 [F² > 3σ(F²)]		0.050
R_m=±1 [F² > 3σ(F²)]		0.052
R_m=±2 [F² > 3σ(F²)]		0.055
R_m=±3 [F² > 3σ(F²)]		0.056
R_m=±4 [F² > 3σ(F²)]		0.060
No. of reflections (individual, observed)	88 532, 59 317
No. of parameters	2016	1734
H-atom treatment	Mixed	Constrained
Weighting scheme	w = 1/[σ²(F) + 0.0001F²]
Δρ_max, Δρ_min (e Å⁻³)	1.64, −1.30	0.48, −0.21

Figure 2
The number of observed and unobserved reflections [according to I > 3σ(I)], R₁ and R_int (all cumulative) versus the resolution limit [sin(θ)/λ]_max used for refinement.

Owing to the excellent data quality, subtle differences in saccharinate anion conformations were noted. Although it is an aromatic and therefore seemingly rigid molecule, the forces of the different crystallographic environments deform the 16 independent molecules significantly. Using the rigid-body approach for the whole molecule, the R₁ value doubled in magnitude. Although this approach is very appealing, since it reduces the number of refinement parameters from 2387 to 1105 or even lower (Naumov et al., 2005), if the probable mirror plane through the molecule is considered then the conformational variance of the saccharinate anions throughout the crystal structure cannot be neglected. The rigidity of the molecule was studied by generating best overlays of every two molecules. It was found that there can be a deviation as large as 0.1 Å between corresponding atoms (see Fig. 3, where the best overlay of molecules 1 and 11 is depicted). Such deviations can be considered large and are most certainly reflected in the increase in the R₁ value when the rigid-body approach is applied for the molecule as whole.

Figure 3
Best overlays (left: all atoms are matched; right: only phenyl ring atoms are matched) of molecules 1 and 11, showing their non-identical conformations. Deviations between corresponding atoms are given in Å.

It was, however, found that the phenyl ring can be considered rigid. The best overlays of the phenyl ring atoms (taken from the refined structure with no restrictions applied to the atomic positions) showed that the corresponding atoms are usually not more than around 0.01 Å apart (see Fig. 3), and this is also confirmed by calculating the best planes through the six atoms. The distances of the saccharinate anion atoms from the best planes through the corresponding phenyl rings are listed in Table S1 in the supporting information.

In the final structure model a rigid-body approach was applied to the phenyl ring, defining it as a set of six coplanar atoms, but refining its internal structure in terms of bond lengths and angles. The R₁ value increased only slightly compared with that of the free-atom model, confirming that the geometries of the phenyl rings are consistently identical and are not influenced by the different crystallographic environments. The number of refinement parameters could be decreased from 2394 to 2016.

Furthermore, one saccharinate anion, three sodium cations and four water molecules are each disordered over two sites. In the previously reported structure models the occupancies were restricted to be equal for all atoms of the major site and all atoms of the minor site with a sum of unity. The reported occupancy ratios from those studies are 0.67:0.33 (Naumov et al., 2005) and 0.70:0.30 (Banerjee et al., 2005). It was also established in the present study that the disorder is correlated, as refining it separately (only restricting the sum to be unity for a major and the corresponding minor site) revealed that it is very similar among all the major (and minor) components. The refined unified ratio of 0.88:0.12 for the correlated disordered entity is, however, different from that reported previously.

2.3.2. Superspace structure

From the established superstructure model of sodium saccharinate 1.875-hydrate it was noted that there is pseudo-translation symmetry present in the P2₁/n unit cell. The particular crystal structure can be described in (3+1)D superspace with the basic cell (bc) and the present supercell (sc) being related by the following transformation:

$[\left (a_{\rm bc}, b_{\rm bc}, c_{\rm bc} \right) = \left (a_{\rm sc}, b_{\rm sc}, c_{\rm sc} \right) \left (\matrix{1 & 0 & 0 \cr 0 & {1\over 4} & 0 \cr 0 & 0 & 1} \right). \eqno(1)]$

The superspace structure is an eightfold substructure of the one described in 3D space, as the former is represented by a four-times smaller unit cell with an additional base-centring of the lattice.

In Fig. 4 a section of the reciprocal layer 0kl is shown, as well as a schematic representation of possible satellite reflection indexing. The 0kl section features strong main reflections and systematically absent reflections according to the C-centre condition h + k = 2n. The modulation wavevector q lies along the b* axis. Assuming that the structure is truly commensurate, the value of q is either ( $[0, {1\over 4}, 0]$ ) or ( $[0, {3\over 4}, 0]$ ). Thus, up to the fourth order satellites are present, with m = ±4 satellites coinciding at the positions of the absent main reflections. It can be noted in Fig. 4 that the satellite reflections at ±¾ distance from the present main reflections appear stronger than those at ±¼ distance, which are barely visible. Inspection of the intensity statistics of the complete reflection list reveals that the modulation wavevector is most favourably defined as ( $[0, {3\over 4}, 0]$ ) (see Table 3). The presence of the C-centre is also evident. The intensity statistics and observations in Fig. 4 are an indication that this structure is well described in superspace.

Table 3
Intensity statistics of different reflection classes

Condition with respect to the supercell	m	〈I〉_all	n_all	〈I〉_obs	n_obs
4h + k = 8n	0	162	81 978	314	41 596
4h + k = 8n + 4 ± 1	±1	68	163 894	139	76 905
4h + k = 8n ± 2	±2	43	163 926	95	69 711
4h + k = 8n ± 1	±3	49	163 979	108	70 845
4h + k = 8n + 4	±4	31	82 033	73	31 209

Figure 4
Section (0kl) of the reciprocal-space reconstruction of the experimental data, with k indices according to the basic cell (bc) and supercell (sc). The top panel gives a schematic representation of possible indexing, alternately based on different q vectors. Large circles indicate main reflections, small circles satellite reflections, open circles absent reflections and full circles allowed reflections.

Although there is a proper solution of the structure in 3D space suggesting commensurability, it cannot be excluded that the structure might be incommensurate. One indication for that would be splitting of the fourth-order satellite reflections, if the component σ₂ of the modulation wavevector q were to deviate from the rational number of ¾. Otherwise (h, k, l, 4) and (h, k + 6, l, −4) describe the same point in reciprocal space (see Fig. 4). Careful examination of the strongest fourth-order satellite reflections in the diffraction data frames showed single peaks with good shapes. Minor splitting of a few peaks recorded at higher 2θ angles was associated with non-monochromaticity of the incident beam. In Fig. 5 a few strongest fourth-order satellite reflections located in the raw data frames are shown, confirming the above statement. Commensurability of the structure at the analysed temperature was therefore established, and ultimately proven upon structure refinement.

Figure 5
Pairs of equivalent strongest fourth-order satellite reflections ( $[\in]$ 4h + k = 8n + 4, indices with respect to the supercell). Slight splitting of the $[-12 \, 12 \, 14]$ reflections is associated with the combination of non-monochromaticity of the incident beam and the geometry of the data collection at higher 2θ angles.

Because of this commensurability, the reflection data for structure refinement in (3+1)D space could be re-indexed by an in-house script using the reflection list from the supercell structure refinement, therefore avoiding new data integration, scaling and corrections. In such a way, different refinement parameters can be more straightforwardly related to those of the refinement in 3D space.

A space-group symmetry test in the JANA2006 software suite indicated the superspace group C2/c(0,σ₂,0)s0 [standard setting B2/b(0,0,σ₃)s0, No. 15.1.7.3 (Stokes et al., 2011 ; van Smaalen et al., 2013 )]. An origin shift of (¼, ¼, 0, 0) was applied so that the fractional coordinates of the atoms correspond to those of the superstructure. The resulting symmetry operators are: x₁, x₂, x₃, x₄; −x₁, x₂ + ½, −x₃ + ½, x₄ + ½; −x₁, −x₂, −x₃, −x₄; x₁, −x₂ + ½, x₃ + ½, −x₄ + ½. Regarding commensurability, there are three inequivalent options for t₀, namely general, t₀ = 0 and t₀ = $[1\over 16]$ . These correspond to the supercell space groups P2₁, P2₁/n and P2₁/c, respectively. The value t₀ = 0 was selected, as the presented unit cell is indexed in such a way as to correspond to P2₁/n.

Structure solution with SUPERFLIP (Palatinus & Chapuis, 2007 ) gave a satisfying starting model. However, such ab initio refinement did not lead to an accurate structure model. Apparently, this failure is due to the presence of an intricate occupational modulation in a crenel function fashion. Initial coordinates for the basic positions and parameters for the modulation and crenel functions were then derived from the supercell structure model. Average positions were used as initial basic positions and, for most atoms, up to fourth-order harmonics were necessary to describe their positional modulation properly. Each harmonic adds up to 2 × 3 parameters, meaning that (together with the three basic position coordinates) three independent atomic positions of the supercell can be described. Coefficients for the highest-order harmonic sine or cosine terms were fixed to 0 values when necessary so as not to exceed the required number of parameters and thus avoid singularities, for example for atoms describing eight independent positions in the supercell. In such a way the initial structure model in (3+1)D superspace was set up for the refinement.

Because of the eightfold relation between the cells and Z′ of 16 for the supercell, the basic cell comprised two saccharinate anions (atoms C1A/B, C2A/B, C3A/B, C4A/B, C5A/B, C6A/B, C7A/B, S1A/B, N1A/B, O1A/B, O2A/B, O3A/B), four sodium cation sites (Na2, Na6, Na14, Na16) and four water O atom sites (O18W, O23W, O24W, O28W) in the asymmetric unit. The occupancy of the sodium cations along the x₄ coordinate is thus zero for some intervals as, according to the stoichiometry, formally only two are required for the two saccharinate anions. The situation is similar for the O atom O23W as the hydrate stoichiometry is not exactly two, requiring fewer than four water molecules per two saccharinate anions.

Several additional atoms were included with respective crenel functions to account for the disorder. As for the 3D model, a rigid-body approach was used for the phenyl rings of the two saccharinate ions. Non-H atoms were refined anisotropically applying modulated ADPs using the same order as the corresponding order for positional modulation. Hydrogen atoms of the saccharinate ions were added geometrically. TLS parameters were used for the phenyl ring carbon atoms and their respective H atoms. The ADP values of the minor disorder component of the saccharinate anion were constrained to be equal to those of the major component. No H atoms of the water molecules were added. Crystallographic and refinement data are listed in Table 2. The larger R₁ value compared with the 3D model is explained by the absence of water H atoms.

2.4. Density functional theory (DFT) calculations

The single-point energy of the saccharinate anions was calculated with the program GAUSSIAN09 (Frisch et al., 2009 ). Atomic coordinates were taken from the superstructure refinement with no restraints. H-atom distances were renormalized to 1.09 Å. The M062X level of theory and 6-311++g(d,p) basis set were used. No calculations were performed for the two saccharinate anions superimposed at the disordered site, since the atomic positions are not accurate enough. An additional calculation was performed allowing the atomic positions to relax to obtain the gas-phase reference energy. The obtained energy values are listed in Table S2.

3. Results and discussion

3.1. Superstructure of sodium saccharinate 1.875-hydrate

The asymmetric unit of the title compound at 95 K described in space group P2₁/n is depicted in Fig. 6. There are a total of 16 saccharinate anions, 16 sodium cations and exactly 30 water molecules. The arrangement of the ions and molecules in the asymmetric unit is somewhat puzzling, as only a part of it can be considered modulated. The saccharinate anions are consistently stacked in a column along b. A regular arrangement is also present for approximately half of the sodium cations and water molecules. However, there is a strong deviation from this modulated pattern as the remaining sodium cations and water molecules are positioned very differently. Furthermore, there is disorder present concerning molecule 13 and neighbouring sodium cations and water molecules. This rather irregular pattern indicates that it is a somewhat of a compromise solution for the crystal structure to form.

Figure 6
The asymmetric unit of sodium saccharinate 1.875-hydrate at 95 K, showing the molecule numbering scheme. Minor components of the disordered sites are depicted as partly transparent. C atoms (gray), O atoms (red), N atoms (blue), S atoms (yellow), Na ions (violet).

It is intriguing that such a large, complex and not even fully pseudo-symmetrically consistent aggregate can apparently be found as a regular pattern throughout the crystal structure. The supramolecular arrangement, including the sophisticated disorder of one saccharinate anion, three sodium cations and four water molecules, is identical for several crystals tested within this study. Moreover, it is virtually the same as that found in the previous studies of this very same solid phase at 95 and 100 K (Naumov et al., 2005; Banerjee et al., 2005). This rules out the possibility that this high-Z′ structure would be any kind of fossil relic of the solution aggregation process as proposed for some high-Z′ compounds (Steed, 2003; Desiraju, 2007). The most notable difference between the present model and previous models is the disorder, with an occupancy ratio of 0.88:0.12 compared with that of around 0.70:0.30 reported previously (Naumov et al., 2005; Banerjee et al., 2005).

3.2. Superspace structure of sodium saccharinate 1.875-hydrate

3.2.1. Modulation of the asymmetric unit entities

Due to the eightfold relation between the unit cells in 3D and (3+1)D space (see the Experimental section), the asymmetric unit of the superspace structure (Z′ = 2) formally consists of two saccharinate anions, two sodium cations and 3.75 water molecules. However, the basic structure is more complex than that.

There are indeed two saccharinate anions defined, which are denoted A and B (see Fig. 1 for the atom numbering). Modulation functions are applied for entity A to define the eight saccharinate positions along the x₄ direction, and similarly for entity B. However, at a certain t value the anion is disordered over two positions, hence additional basic positions of the saccharinate anion with reduced site occupancy have been defined, namely B′ and B′′. Corresponding crenel functions to alter the B/B′/B′′ occupancy between 0 and the respective non-zero value have been defined, and these are summarized in a t-plot of the modulations of atoms O1A and O1B as an example (Fig. 7). The largest modulation amplitudes are found for modulation functions u_y, but the corresponding unit-cell dimension b is several times smaller than a and c (see Table 2). Modulation functions u_z are approximately constant throughout the modulation period. For the saccharinate anion B the disordered molecular site occurs at t = 0.625 where the saccharinate anion adopts two slightly different orientations with an occupancy ratio of 0.88:0.12 (corresponding to saccharinate 13 in the superstructure). Only a single position needs to be described for B′ and B′′, which is already defined by the corresponding basic positions (x, y and z values), so no additional displacive modulation function need be added for the atoms of the B′ and B′′ entities.

Figure 7
t-Plots of the positional (bottom) and occupational (top) modulation of atoms O1A (vermillion), O1B (blue), O1B′ (yellow), O1B′′ (grey). Commensurate t-sections are indicated by dashed lines.

It can be noted, however, that the position of atom O1B′ fits relatively well within the modulation curve of O1B. Restricting the B′ atoms to have the same basic positions and modulation functions as the B atoms was found to be not feasible since such a refinement resulted in unreasonable basic positions for some atoms and an increase in R₁. t-Plots for atoms O1B, O2B, O3B, S1B, N1B and C7B defining the flexible part of the molecule (and their B′ counterparts) are given in the supporting information, showing that the B′ positions deviate rather significantly from the assumed positions according to the modulation function of the B atoms.

It must be added that for the other saccharinate atoms the modulation functions are very similar to each other and possess the same characteristics, as shown for atoms O1A and O1B in Fig. 7.

Regarding the sodium cations in the asymmetric unit, the picture is more complex (see Fig. 8). For the two asymmetric sodium ions named Na2 and Na6 there is a severe discontinuity in their modulation functions. Additional sodium cations have therefore been defined in limited crenel intervals. Furthermore, there is an inconsistency in the ion density in the t-sections, as apparently one of the sodium ions is absent at section t = 0.5 and instead an additional cation appears at t = 0.625. Finally, all three atoms at this particular t-section are disordered over two sites.

Figure 8
t-Plots of the positional modulation of sodium cations (vermillion: u_y + y₀; blue: u_x + x₀; yellow: coordinate u_z + z₀). Atoms in the shaded area are disordered over two sites and only the major occupancy site is depicted. Commensurate t-sections are indicated by dashed lines.

The modulation of the water molecules (or their respective O atoms) is depicted in Fig. 9. The component u_z has been omitted for the sake of clarity. Furthermore, u_z is approximately constant, similar to the previously discussed atoms. For one of the water molecules there are two sites empty from the eight sites within one period along the x₄ axis, resulting in the unusual stoichiometry of 1:1.875 between the saccharinate (sodium) ions and water molecules. At four t values (shaded grey) the water molecules are disordered over two sites. Here, the major occupancy sites have been restrained to have the same basic positions and modulation function parameters as atoms O18W, O28W and O24W, respectively.

Figure 9
t-Plots of the positional modulation of water molecule O atoms (vermillion: u_y + y₀; blue: u_x + x₀). Atoms in the shaded areas are disordered over two sites and only the major occupancy site is depicted. Commensurate t-sections are indicated by dashed lines.

From the t-plots discussed above it has been shown that half of the sodium ions, in particular, are inconsistently positioned throughout the structure, albeit in a periodic fashion. The rather odd cation placement and disorder around the section t = 0.625 correlates with the absence and disorder of the water molecules around the same section. Regarding the independent saccharinate anions, the inconsistencies are not so severe, except for the presence of a disordered site and larger deviations from the basic positions in terms of y coordinate (see Fig. 7).

3.2.2. Variation in the saccharinate anion conformation

As already noted in the analysis of the supercell model, the saccharinate anion geometry varies throughout the crystal structure, except for the phenyl ring. The conformational variation of the two independent saccharinate anions can be noted in t-plots where the bond lengths between the constituent atoms are depicted (see Figs. 10 and 11). Furthermore, the molecule is not planar, and therefore no internal mirror symmetry can be exploited to reduce the number of refinement parameters. This is proven by t-plots showing the torsion angles S1—N1—C7—O3 and N1—C7—O3—phenyl (Figs. 12 and 13). Torsion-angle values for S1—N1—C7—O3 span ranges of around 176°–180° and 176°–184° for molecules A and B, respectively, indicating non-planarity of the saccharinate heterocycle. Furthermore, the planar phenyl ring is situated at angles in the ranges of 2°–4° and 2°–6° with respect to the plane N1—C7—O3 for molecules A and B, respectively.

Figure 10
t-Plots of the interatomic distances between atom C7 and the respective covalently bonded atoms N1, O3 and C2 (vermillion: molecule A, blue: molecule B, yellow: major component of the disordered site). Commensurate t-sections are indicated by dashed lines.

Figure 11
t-Plots of the interatomic distances between atom S1 and the respective covalently bonded atoms C1, O1, O2 and N1 (vermillion: molecule A, blue: molecule B, yellow: major component of the disordered site). Commensurate t-sections are indicated by dashed lines.

Figure 12
t-Plots of the torsion angle S1—N1—C7—O3 (vermillion: molecule A, blue: molecule B, yellow: major component of the disordered site). Commensurate t-sections are indicated by dashed lines.

Figure 13
t-Plots of the torsion angle N1—C7—O3—phenyl (vermillion: molecule A, blue: molecule B, yellow: major component of the disordered site). Commensurate t-sections are indicated by dashed lines.

DFT calculations of conformer energies show that they vary between 9 and 15 kJ mol⁻¹ compared with the gas-phase conformation (see Table S2). The energy variance for both asymmetric saccharinate anions A and B versus the modulation period t is depicted in Fig. 14. The energy of the site-A saccharinate anions is consistently lower than that of the B anions. This indicates that there is a smaller frustration exerted on the site-A molecules. However, the difference in conformer energy of at least 9 kJ mol⁻¹ compared with the gas-phase conformation shows that the crystal environment exerts a considerable force on the saccharinate anions.

Figure 14
Conformer energy versus t (vermillion: molecule A, blue: molecule B). Fourth-order harmonics were used to fit the data points.

3.2.3. Sodium coordination spheres

Most of the sodium ions are octahedrally coordinated. Sodium cation Na2 is coordinated by water molecules O18W and O28W and by saccharinate anions through carbonyl O atoms O3A and O3B. Interatomic distances are presented in Fig. 15. Opposite water molecules O18W and O28W are more consistently located equidistant from the Na2 cation. Deviations from an optimal distance to the central atom are more pronounced in the case of the O atoms of the saccharinate ion, especially those of the asymmetric molecule B.

Figure 15
t-Plots of the interatomic distances in the Na2 coordination sphere. Commensurate t-sections are indicated by dashed lines.

Sodium cation Na6 is coordinated by all four asymmetric water molecules, namely, O18W, O23W, O24W and O28W. It also interacts with some of the sulfonyl group O atoms of saccharinate anion B (Fig. 16).

Figure 16
t-Plots of the interatomic distances in the Na6 coordination sphere. Commensurate t-sections are indicated by dashed lines.

The remaining sodium cations Na2′, Na14, Na14′, Na16 and Na16′, and the respective minor sites Na14′′ and Na16′′, all interact with neighbouring water molecules and with the O and N atoms of the saccharinate anions, but do not show clear octahedral coordination polyhedra.

4. Conclusions

The analysis of X-ray diffraction data intensity statistics shows that the structure of sodium saccharinate 1.875-hydrate is well described in (3+1)D superspace as a commensurate case in a C-centred lattice with a modulation wavevector q of (0, $[3\over 4]$ , 0). The centred unit cell in the superspace group C2/c(0, σ₂, 0)s0 corresponds to an eightfold substructure of a four times larger primitive 3D supercell in P2₁/n. The superspace approach allows Z′ to be reduced from 16 to 2, while the 2 × 8 = 16 different conformations are described by modulation functions. The 3D model is in accordance with the two previously published models, but it is more accurate due to better data quality and considerably higher resolution.

The structure of the title compound possess an intricate organization of constituent entities and it is accompanied by a correlated disorder. Although the saccharinate anion is aromatic and seemingly rigid, a subtle conformation variance has been found involving the heterocyclic part of the molecule. The organic anions are organized uniformly throughout the crystal structure. The sodium cations, by contrast, are only partly consistently positioned. This can be explained by the fact that such single-atom ions can equally well interact with counter-ions in any direction, whilst for the saccharinate anions there is steric hindrance present, and only a limited volume in space around the negatively charged amide entity is accessible to form a favourable interaction. The water molecules follow the arrangement of the sodium ions as they are coordinated around them. The unusual hydrate stoichiometry, however, indicates that they are rather acting as void fillers. It is not clear what causes around half of the 16 crystallographically independent sodium ions not to obey the pseudo-symmetrical arrangement as found for the rest. The overall structure is rather surprising, as such a complex and large asymmetric arrangement consistently spans across the crystal structure.

Supporting information

CCDC references: 1963817; 1963818

Crystal structure: contains datablocks global, I, II. DOI: https://doi.org/10.1107/S2052520619014938/dk5088sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2052520619014938/dk5088Isup2.hkl

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S2052520619014938/dk5088IIsup3.hkl

Supporting information file. DOI: https://doi.org/10.1107/S2052520619014938/dk5088sup4.pdf

Computing details top

Data collection: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018) for (I). Cell refinement: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018) for (I). Data reduction: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018) for (I).

Sodium Saccharinate 1.875-Hydrate (I) top

Crystal data top

C₇H_7.75O_4.875NSNa	F(000) = 7845
M_r = 238.8	D_x = 1.645 Mg m⁻³
Monoclinic, P2₁/n	Ag Kα radiation, λ = 0.56089 Å
Hall symbol: -P 2yabc	Cell parameters from 86894 reflections
a = 18.6212 (1) Å	θ = 2.8–29.8°
b = 28.4622 (2) Å	µ = 0.20 mm⁻¹
c = 29.1642 (2) Å	T = 95 K
β = 93.4511 (6)°	Prism, white translucent
V = 15429.00 (17) Å³	0.45 × 0.35 × 0.22 mm
Z = 64

Data collection top

Mar dtb diffractometer	88532 independent reflections
Radiation source: X-ray tube	59317 reflections with I > 3σ(I)
Equatorial mounted graphite monochromator	R_int = 0.086
φ scans	θ_max = 29.9°, θ_min = 2.8°
Absorption correction: empirical (using intensity measurements) CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −32→32
T_min = 0.912, T_max = 1	k = −50→50
651280 measured reflections	l = −51→51

Refinement top

Refinement on F	38 constraints
R[F² > 2σ(F²)] = 0.048	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.055	Weighting scheme based on measured s.u.'s w = 1/(σ²(F) + 0.0001F²)
S = 1.57	(Δ/σ)_max = 0.018
88532 reflections	Δρ_max = 1.64 e Å⁻³
2010 parameters	Δρ_min = −1.30 e Å⁻³
0 restraints

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.00451 (3)	0.880502 (19)	0.252679 (18)	0.01584 (13)
Na2	−0.00116 (2)	1.002808 (18)	0.250815 (18)	0.01529 (13)
Na3	−0.00472 (3)	1.126766 (19)	0.248782 (18)	0.01521 (13)
Na4	0.16309 (3)	1.210473 (19)	0.197136 (18)	0.01539 (13)
Na5	0.17686 (3)	0.943185 (18)	0.189307 (18)	0.01553 (13)
Na6	−0.18552 (3)	1.068630 (18)	0.306019 (18)	0.01553 (13)
Na7	0.08906 (3)	0.387281 (19)	0.158035 (18)	0.01576 (13)
Na8	0.20383 (3)	0.68451 (2)	0.209047 (19)	0.01786 (14)
Na9	−0.16671 (3)	0.804005 (18)	0.297547 (18)	0.01558 (13)
Na10	−0.19199 (3)	0.332876 (19)	0.294712 (18)	0.01684 (14)
Na11	−0.02390 (3)	0.30127 (2)	0.249668 (18)	0.01697 (14)
Na12	0.02330 (3)	0.76275 (2)	0.23912 (2)	0.02402 (17)
Na13	0.15305 (3)	0.440255 (19)	0.277503 (18)	0.01688 (14)
Na14	−0.09262 (3)	0.61998 (2)	0.34954 (2)	0.01582 (15)	0.8763 (8)
Na16	−0.13587 (3)	0.54676 (3)	0.23679 (2)	0.02122 (19)	0.8763 (8)
Na18	0.10392 (3)	0.56521 (2)	0.21843 (2)	0.01753 (16)	0.8763 (8)
O10w	−0.21855 (5)	0.33883 (4)	0.21325 (3)	0.0173 (2)
O11w	−0.07988 (5)	0.37399 (4)	0.27368 (3)	0.0182 (2)
O12w	−0.14237 (6)	0.82058 (4)	0.37669 (4)	0.0260 (3)
O13w	−0.18801 (5)	0.80072 (3)	0.21373 (3)	0.0170 (2)
O14w	0.11443 (5)	0.87684 (3)	0.21546 (3)	0.0160 (2)
O15w	−0.11104 (5)	0.87685 (3)	0.28277 (3)	0.0161 (2)
O16w	0.14098 (6)	1.19907 (4)	0.11726 (4)	0.0232 (3)
O17w	0.17018 (6)	0.69835 (4)	0.13099 (4)	0.0237 (3)
O18w	−0.11556 (5)	1.13122 (3)	0.28255 (3)	0.0158 (2)
O19w	0.13818 (6)	0.45529 (4)	0.12754 (5)	0.0311 (3)
O20w	0.10939 (5)	1.13274 (3)	0.21260 (3)	0.0170 (2)
O21w	0.22320 (5)	0.67499 (4)	0.29128 (4)	0.0181 (2)
O22w	−0.17108 (6)	0.31430 (4)	0.37248 (4)	0.0267 (3)
O23w	−0.25352 (5)	1.07212 (4)	0.23276 (3)	0.0179 (2)
O24w	−0.15314 (7)	1.06881 (4)	0.38463 (4)	0.0285 (3)
O25w	0.08130 (5)	0.37096 (4)	0.23721 (3)	0.0192 (2)
O26w	0.14408 (5)	0.75469 (3)	0.22490 (3)	0.0174 (2)
O27w	0.14427 (6)	0.95134 (4)	0.11131 (4)	0.0281 (3)
O28w	−0.11526 (5)	1.00142 (3)	0.28594 (3)	0.0164 (2)
O29w	0.24345 (5)	0.94233 (4)	0.26423 (3)	0.0170 (2)
O30w	0.11013 (5)	1.00717 (3)	0.21267 (3)	0.0157 (2)
O31w	−0.12113 (5)	0.26057 (4)	0.27661 (4)	0.0231 (3)
O32w	0.17771 (5)	1.21697 (3)	0.28022 (3)	0.0166 (2)
O33w	0.05090 (5)	1.24794 (4)	0.20764 (3)	0.0171 (2)
O34w	−0.07701 (5)	0.74664 (4)	0.27954 (4)	0.0196 (3)
O35w	−0.05536 (6)	0.50591 (4)	0.28687 (4)	0.0250 (3)
O36w	−0.08404 (6)	0.61792 (4)	0.27021 (4)	0.0174 (3)	0.8763 (8)
O38w	0.06773 (6)	0.48669 (4)	0.23320 (4)	0.0179 (3)	0.8763 (8)
O40w	0.07341 (8)	0.64227 (5)	0.23614 (5)	0.0294 (4)	0.8763 (8)
O42w	−0.14421 (6)	0.55235 (5)	0.37499 (5)	0.0232 (3)	0.8763 (8)
S11	0.045182 (15)	1.072762 (11)	0.086128 (10)	0.01354 (7)
O11	0.08209 (5)	1.11584 (3)	0.07538 (3)	0.0194 (2)
O21	0.07345 (5)	1.03122 (3)	0.06462 (3)	0.0181 (2)
O31	−0.04490 (5)	1.06062 (3)	0.19383 (3)	0.0175 (2)
N11	0.04176 (5)	1.06582 (4)	0.14090 (4)	0.0155 (3)
C71	−0.02777 (6)	1.06607 (4)	0.15369 (4)	0.0138 (3)
S12	−0.241859 (15)	1.192015 (11)	0.170777 (11)	0.01519 (7)
O12	−0.28754 (5)	1.15041 (4)	0.16908 (4)	0.0208 (3)
O22	−0.27643 (6)	1.23374 (4)	0.18638 (4)	0.0273 (3)
O32	−0.04729 (5)	1.17487 (4)	0.18718 (3)	0.0200 (2)
N12	−0.16778 (6)	1.18136 (4)	0.20027 (4)	0.0177 (3)
C72	−0.11067 (6)	1.18307 (4)	0.17319 (4)	0.0153 (3)
S13	0.028375 (15)	0.314600 (11)	0.082681 (10)	0.01354 (7)
O13	0.07362 (5)	0.35555 (3)	0.07722 (3)	0.0188 (2)
O23	0.05653 (5)	0.27116 (3)	0.06503 (3)	0.0187 (2)
O33	−0.08938 (4)	0.31214 (4)	0.17875 (3)	0.0179 (2)
N13	0.00987 (5)	0.31018 (4)	0.13578 (4)	0.0149 (2)
C73	−0.06205 (6)	0.31510 (4)	0.14102 (4)	0.0139 (3)
S14	−0.204993 (15)	0.461061 (11)	0.173827 (11)	0.01682 (8)
O14	−0.26210 (5)	0.42786 (4)	0.18131 (4)	0.0245 (3)
O24	−0.22080 (5)	0.50895 (3)	0.18762 (3)	0.0200 (3)
O34	−0.01527 (5)	0.42779 (4)	0.17437 (3)	0.0211 (3)
N14	−0.12878 (6)	0.44396 (4)	0.19766 (4)	0.0186 (3)
C74	−0.07900 (6)	0.43981 (4)	0.16552 (4)	0.0159 (3)
S15	0.062210 (15)	0.576045 (12)	0.090321 (10)	0.01549 (7)
O15	0.10001 (5)	0.61996 (4)	0.08404 (3)	0.0226 (3)
O25	0.09893 (5)	0.53538 (4)	0.07283 (3)	0.0223 (3)
O35	−0.05675 (5)	0.56150 (4)	0.18378 (3)	0.0244 (3)
N15	0.04337 (5)	0.56842 (4)	0.14258 (4)	0.0175 (3)
C75	−0.02926 (6)	0.56741 (5)	0.14669 (4)	0.0165 (3)
S16	−0.205343 (15)	0.677212 (11)	0.175515 (11)	0.01563 (7)
O16	−0.22795 (5)	0.62878 (4)	0.17751 (4)	0.0234 (3)
O26	−0.25605 (5)	0.71119 (4)	0.19133 (4)	0.0221 (3)
O36	−0.01184 (5)	0.70328 (4)	0.18458 (4)	0.0210 (3)
N16	−0.12712 (6)	0.68425 (4)	0.20251 (4)	0.0181 (3)
C76	−0.07632 (6)	0.69539 (4)	0.17263 (4)	0.0156 (3)
S17	0.064601 (15)	0.819885 (11)	0.089907 (10)	0.01372 (7)
O17	0.10566 (5)	0.86084 (3)	0.07746 (3)	0.0190 (2)
O27	0.09344 (5)	0.77556 (3)	0.07509 (3)	0.0186 (2)
O37	−0.04426 (5)	0.82051 (4)	0.19061 (3)	0.0176 (2)
N17	0.05062 (5)	0.81931 (4)	0.14421 (4)	0.0160 (3)
C77	−0.02039 (6)	0.82175 (4)	0.15131 (4)	0.0149 (3)
S18	−0.230901 (15)	0.946577 (11)	0.171368 (10)	0.01363 (7)
O18	−0.27615 (5)	0.90558 (3)	0.16997 (3)	0.0196 (2)
O28	−0.26798 (5)	0.99020 (3)	0.18099 (3)	0.0200 (3)
O38	−0.03813 (4)	0.93909 (3)	0.20347 (3)	0.0168 (2)
N18	−0.16142 (5)	0.94014 (4)	0.20685 (4)	0.0161 (3)
C78	−0.09940 (6)	0.94207 (4)	0.18412 (4)	0.0142 (3)
S19	0.232342 (14)	1.067542 (11)	0.322180 (11)	0.01396 (7)
O19	0.27044 (5)	1.02281 (3)	0.32096 (3)	0.0200 (2)
O29	0.27799 (5)	1.10660 (4)	0.31111 (4)	0.0211 (3)
O39	0.03758 (4)	1.06496 (3)	0.29890 (3)	0.0159 (2)
N19	0.15941 (5)	1.06572 (4)	0.28982 (4)	0.0156 (3)
C79	0.10038 (6)	1.06785 (4)	0.31558 (4)	0.0134 (3)
S110	−0.059599 (15)	1.192786 (11)	0.408533 (10)	0.01465 (7)
O110	−0.10018 (5)	1.23525 (4)	0.41621 (3)	0.0208 (3)
O210	−0.08943 (5)	1.15111 (4)	0.42896 (3)	0.0215 (3)
O310	0.04848 (5)	1.17794 (3)	0.30875 (3)	0.0172 (2)
N110	−0.04693 (5)	1.18506 (4)	0.35484 (4)	0.0168 (3)
C710	0.02449 (6)	1.18587 (4)	0.34694 (4)	0.0145 (3)
S111	0.218127 (14)	0.337039 (10)	0.338598 (10)	0.01254 (7)
O111	0.28029 (4)	0.30681 (3)	0.33779 (3)	0.0181 (2)
O211	0.23091 (4)	0.38543 (3)	0.32495 (3)	0.0166 (2)
O311	0.03194 (5)	0.29685 (3)	0.32185 (3)	0.0179 (2)
N111	0.14940 (5)	0.31570 (4)	0.30922 (3)	0.0145 (2)
C711	0.09193 (6)	0.31031 (4)	0.33636 (4)	0.0132 (3)
S112	−0.063195 (15)	0.427113 (11)	0.412761 (11)	0.01558 (7)
O112	−0.11225 (5)	0.46617 (4)	0.41780 (3)	0.0210 (3)
O212	−0.08903 (5)	0.38269 (3)	0.42980 (3)	0.0206 (3)
O312	0.06447 (5)	0.42566 (4)	0.32282 (3)	0.0208 (3)
N112	−0.03933 (5)	0.42271 (4)	0.36075 (4)	0.0167 (3)
C712	0.03297 (6)	0.42907 (4)	0.35883 (4)	0.0153 (3)
S114	−0.030608 (15)	0.702137 (12)	0.412033 (10)	0.01503 (7)
O114	−0.07138 (5)	0.74344 (4)	0.42362 (3)	0.0220 (3)
O214	−0.06386 (5)	0.65805 (4)	0.42358 (3)	0.0212 (3)
O314	0.08785 (5)	0.70204 (4)	0.31620 (3)	0.0200 (3)
N114	−0.01213 (5)	0.70116 (4)	0.35864 (4)	0.0165 (3)
C714	0.06001 (6)	0.70289 (4)	0.35410 (4)	0.0146 (3)
S115	0.247897 (14)	0.824999 (10)	0.331901 (10)	0.01299 (7)
O115	0.29161 (5)	0.78317 (3)	0.33230 (3)	0.0200 (3)
O215	0.28721 (4)	0.86824 (3)	0.32408 (3)	0.0179 (2)
O315	0.05536 (4)	0.81863 (3)	0.29887 (3)	0.0164 (2)
N115	0.17863 (5)	0.82098 (4)	0.29615 (4)	0.0147 (2)
C715	0.11611 (6)	0.82190 (4)	0.31870 (4)	0.0133 (3)
S116	−0.057450 (15)	0.943291 (11)	0.414126 (10)	0.01476 (7)
O116	−0.09734 (5)	0.98488 (4)	0.42638 (3)	0.0206 (3)
O216	−0.08409 (5)	0.89988 (4)	0.43266 (3)	0.0208 (3)
O316	0.03971 (5)	0.94154 (3)	0.30838 (3)	0.0181 (2)
N116	−0.05028 (5)	0.93974 (4)	0.35929 (4)	0.0165 (3)
C716	0.01976 (6)	0.94312 (4)	0.34832 (4)	0.0147 (3)
Na15	−0.1086 (2)	0.51422 (16)	0.35054 (16)	0.0191 (12)	0.1237 (8)
Na17	−0.1419 (3)	0.5805 (2)	0.23032 (19)	0.0325 (18)	0.1237 (8)
Na19	0.0361 (3)	0.5666 (2)	0.24605 (18)	0.0345 (17)	0.1237 (8)
O37w	−0.0514 (5)	0.6134 (3)	0.2799 (4)	0.037 (3)	0.1237 (8)
Hao28	−0.1042 (8)	0.9856 (6)	0.3109 (6)	0.0196*
Hbo28	−0.1385 (8)	0.9843 (6)	0.2664 (6)	0.0196*
Hao24	−0.1314 (10)	1.0487 (7)	0.3954 (7)	0.0342*
Hao27	0.1304 (10)	0.9255 (7)	0.0994 (7)	0.0337*
Hao17	0.1512 (9)	0.7221 (7)	0.1202 (6)	0.0284*
Hao22	−0.1485 (10)	0.3350 (7)	0.3860 (7)	0.0321*
Hao18	−0.1020 (8)	1.1484 (6)	0.3037 (6)	0.019*
Hbo18	−0.1388 (8)	1.1476 (6)	0.2615 (6)	0.019*
Hao33	0.0484 (8)	1.2649 (6)	0.1850 (6)	0.0206*
Hao13	−0.1459 (9)	0.8048 (6)	0.2033 (6)	0.0203*
Hao21	0.1863 (9)	0.6834 (6)	0.3023 (6)	0.0218*
Hao38	0.0488 (10)	0.4733 (7)	0.2108 (7)	0.0215*	0.8763 (8)
O43w	−0.1468 (4)	0.5847 (3)	0.3797 (3)	0.023 (2)	0.1237 (8)
Hao23	−0.2551 (9)	1.0945 (6)	0.2164 (6)	0.0214*
Hao15	−0.1365 (8)	0.8931 (6)	0.2635 (6)	0.0193*
Hbo15	−0.1034 (8)	0.8911 (6)	0.3061 (6)	0.0193*
Hao12	−0.1204 (10)	0.8004 (7)	0.3893 (7)	0.0311*
Hao34	−0.0649 (9)	0.7331 (6)	0.3060 (6)	0.0236*
Hao31	−0.1085 (9)	0.2443 (7)	0.3003 (6)	0.0277*
O41w	0.0920 (4)	0.6335 (3)	0.2157 (4)	0.028 (3)	0.1237 (8)
Hao32	0.1396 (9)	1.2063 (6)	0.2876 (6)	0.02*
Hao29	0.2430 (9)	0.9645 (6)	0.2797 (6)	0.0204*
Hbo29	0.2497 (8)	0.9192 (6)	0.2842 (6)	0.0204*
Hbo25	0.1028 (9)	0.3542 (6)	0.2553 (6)	0.0231*
Hao25	0.0469 (9)	0.3810 (6)	0.2534 (6)	0.0231*
Hao30	0.1339 (8)	1.0256 (6)	0.2335 (6)	0.0188*
Hao16	0.1205 (10)	1.2169 (7)	0.1050 (7)	0.0278*
Hao20	0.1367 (9)	1.1168 (6)	0.2290 (6)	0.0204*
Hbo20	0.0960 (8)	1.1162 (6)	0.1887 (6)	0.0204*
Hbo14	0.1022 (8)	0.8570 (6)	0.1925 (6)	0.0191*
Hao14	0.1423 (8)	0.8624 (6)	0.2344 (6)	0.0191*
Hao11	−0.0681 (9)	0.3870 (6)	0.2983 (6)	0.0219*
Hbo11	−0.0943 (9)	0.3946 (6)	0.2554 (6)	0.0219*
Hao19	0.1680 (10)	0.4713 (7)	0.1409 (7)	0.0373*
Hao26	0.1643 (8)	0.7706 (6)	0.2481 (6)	0.0208*
Hbo26	0.1535 (9)	0.7678 (6)	0.2044 (6)	0.0208*
Hbo10	−0.2280 (9)	0.3641 (6)	0.2067 (6)	0.0208*
Hbo21	0.2279 (9)	0.6495 (6)	0.2962 (6)	0.0218*
Hbo30	0.0952 (8)	1.0229 (6)	0.1907 (6)	0.0188*
Hbo17	0.1457 (9)	0.6754 (7)	0.1190 (6)	0.0284*
Hbo33	0.0232 (9)	1.2264 (6)	0.2011 (6)	0.0206*
Hao10	−0.1836 (9)	0.3294 (6)	0.2002 (6)	0.0208*
Hbo12	−0.1284 (10)	0.8439 (7)	0.3892 (7)	0.0311*
Hbo13	−0.2003 (9)	0.7766 (6)	0.2058 (6)	0.0203*
Hbo34	−0.1016 (9)	0.7280 (6)	0.2642 (6)	0.0236*
Hbo27	0.1260 (10)	0.9712 (7)	0.0982 (7)	0.0337*
Hbo23	−0.2459 (9)	1.0493 (6)	0.2152 (6)	0.0214*
Hbo22	−0.1495 (10)	0.2906 (7)	0.3813 (7)	0.0321*
Hbo19	0.1175 (10)	0.4745 (7)	0.1101 (7)	0.0373*
Hbo32	0.1719 (8)	1.2446 (6)	0.2838 (6)	0.02*
Hao35	−0.0358 (9)	0.5250 (7)	0.3046 (6)	0.03*
Hbo38	0.0365 (10)	0.4884 (7)	0.2502 (7)	0.0215*	0.8763 (8)
Hbo24	−0.1358 (10)	1.0907 (7)	0.3950 (7)	0.0342*
Hbo31	−0.1461 (10)	0.2448 (7)	0.2617 (6)	0.0277*
Hbo16	0.1209 (9)	1.1748 (7)	0.1085 (6)	0.0278*
Hbo35	−0.0659 (9)	0.4835 (7)	0.3057 (6)	0.03*
Hbo40	0.0729 (12)	0.6551 (8)	0.2585 (8)	0.0353*	0.8763 (8)
O39w	0.0966 (4)	0.4964 (3)	0.2199 (3)	0.022 (2)	0.1237 (8)
Hao40	0.0496 (12)	0.6572 (8)	0.2185 (8)	0.0353*	0.8763 (8)
Hao42	−0.1211 (11)	0.5330 (8)	0.3883 (7)	0.0278*	0.8763 (8)
Hbo42	−0.1729 (11)	0.5366 (8)	0.3614 (7)	0.0278*	0.8763 (8)
S1dia	0.20429 (2)	0.54741 (2)	0.32592 (2)	0.01310 (10)	0.8763 (8)
O1dia	0.25412 (6)	0.57836 (4)	0.30419 (4)	0.0225 (3)	0.8763 (8)
O2dia	0.22222 (19)	0.49839 (12)	0.32227 (14)	0.0146 (4)	0.8763 (8)
O3dia	0.01560 (5)	0.57816 (4)	0.33654 (4)	0.0237 (3)	0.8763 (8)
N1dia	0.12260 (7)	0.55647 (5)	0.30681 (5)	0.0180 (3)	0.8763 (8)
C7dia	0.08158 (7)	0.57008 (5)	0.34128 (5)	0.0154 (3)	0.8763 (8)
S1dib	0.1802 (3)	0.54443 (18)	0.32182 (18)	0.0252 (11)	0.1237 (8)
O1dib	0.2141 (5)	0.5787 (3)	0.2918 (3)	0.0225 (3)	0.1237 (8)
O2dib	0.2126 (15)	0.4934 (11)	0.3188 (12)	0.028 (5)	0.1237 (8)
O3dib	0.0029 (4)	0.5538 (3)	0.3655 (3)	0.0237 (3)	0.1237 (8)
N1dib	0.0966 (5)	0.5427 (4)	0.3196 (3)	0.025 (3)	0.1237 (8)
C7dib	0.0681 (5)	0.5551 (5)	0.3594 (4)	0.021 (3)	0.1237 (8)
C1a	−0.04797 (3)	1.078592 (18)	0.07310 (2)	0.0140 (12)
C2a	−0.08242 (3)	1.073767 (18)	0.11383 (2)	0.0140 (12)
C3a	−0.15674 (4)	1.077304 (18)	0.11412 (3)	0.0175 (13)
C4a	−0.19512 (4)	1.085804 (18)	0.07236 (3)	0.0203 (12)
C5a	−0.15998 (4)	1.090617 (18)	0.03149 (3)	0.0204 (12)
C6a	−0.08497 (4)	1.087048 (18)	0.03119 (3)	0.0176 (13)
H1c3a	−0.180917	1.074016	0.142099	0.020 (3)
H1c4a	−0.246577	1.088401	0.071635	0.024 (2)
H1c5a	−0.187717	1.096451	0.003249	0.024 (2)
H1c6a	−0.060379	1.090293	0.003362	0.020 (3)
C1b	−0.20518 (5)	1.20152 (7)	0.11717 (2)	0.0139 (13)
C2b	−0.13116 (5)	1.19578 (7)	0.12406 (2)	0.0138 (13)
C3b	−0.08666 (5)	1.20112 (12)	0.08791 (3)	0.0166 (14)
C4b	−0.11878 (6)	1.21237 (6)	0.04483 (3)	0.0183 (13)
C5b	−0.19338 (6)	1.21808 (7)	0.03821 (3)	0.0187 (13)
C6b	−0.23832 (5)	1.21269 (13)	0.07469 (3)	0.0171 (14)
H1c3b	−0.035508	1.19722	0.092385	0.022 (3)
H1c4b	−0.089176	1.216254	0.019265	0.024 (2)
H1c5b	−0.214047	1.225815	0.008205	0.025 (2)
H1c6b	−0.28951	1.216534	0.070499	0.023 (3)
C1c	−0.06068 (4)	0.32456 (3)	0.05970 (3)	0.0140 (13)
C2c	−0.10462 (4)	0.32457 (3)	0.09660 (3)	0.0141 (13)
C3c	−0.17811 (5)	0.33221 (4)	0.08974 (3)	0.0170 (14)
C4c	−0.20587 (5)	0.33979 (3)	0.04482 (3)	0.0194 (13)
C5c	−0.16121 (5)	0.33972 (3)	0.00786 (3)	0.0194 (13)
C6c	−0.08703 (5)	0.33202 (4)	0.01478 (3)	0.0169 (14)
H1c3c	−0.208806	0.332267	0.115029	0.022 (3)
H1c4c	−0.25652	0.345157	0.03916	0.026 (3)
H1c5c	−0.181735	0.345034	−0.022682	0.026 (3)
H1c6c	−0.055971	0.331902	−0.010324	0.022 (3)
C1d	−0.18102 (6)	0.46019 (13)	0.11645 (2)	0.0161 (14)
C2d	−0.10769 (6)	0.45066 (13)	0.11780 (2)	0.0152 (14)
C3d	−0.07094 (9)	0.4506 (3)	0.07778 (3)	0.0188 (15)
C4d	−0.11008 (7)	0.46039 (12)	0.03657 (3)	0.0230 (14)
C5d	−0.18394 (7)	0.46995 (13)	0.03552 (3)	0.0235 (14)
C6d	−0.22104 (9)	0.4700 (3)	0.07592 (4)	0.0202 (15)
H1c3d	−0.020317	0.444069	0.078424	0.025 (3)
H1c4d	−0.085921	0.460574	0.008401	0.032 (3)
H1c5d	−0.209539	0.476565	0.006691	0.033 (3)
H1c6d	−0.271658	0.47651	0.075563	0.027 (3)
C1e	−0.02684 (4)	0.57960 (4)	0.06572 (3)	0.0147 (15)
C2e	−0.07210 (4)	0.57443 (4)	0.10160 (3)	0.0150 (15)
C3e	−0.14626 (5)	0.57655 (5)	0.09351 (3)	0.0180 (17)
C4e	−0.17331 (5)	0.58398 (4)	0.04842 (3)	0.0203 (15)
C5e	−0.12732 (5)	0.58914 (4)	0.01249 (3)	0.0201 (15)
C6e	−0.05247 (5)	0.58701 (5)	0.02064 (3)	0.0176 (17)
H1c3e	−0.177865	0.573014	0.118099	0.029 (3)
H1c4e	−0.224409	0.585583	0.041921	0.033 (3)
H1c5e	−0.147395	0.594223	−0.018205	0.033 (3)
H1c6e	−0.020501	0.590508	−0.003754	0.028 (4)
C1f	−0.17907 (5)	0.69250 (8)	0.12021 (2)	0.0153 (15)
C2f	−0.10489 (5)	0.69877 (8)	0.12388 (2)	0.0147 (15)
C3f	−0.06772 (5)	0.71017 (16)	0.08555 (4)	0.0189 (16)
C4f	−0.10730 (6)	0.71505 (8)	0.04365 (3)	0.0225 (15)
C5f	−0.18201 (6)	0.70867 (9)	0.04027 (3)	0.0237 (15)
C6f	−0.21954 (5)	0.69716 (17)	0.07895 (4)	0.0207 (16)
H1c3f	−0.016512	0.714557	0.0878	0.029 (3)
H1c4f	−0.08286	0.722923	0.016625	0.035 (3)
H1c5f	−0.207899	0.712242	0.011009	0.037 (3)
H1c6f	−0.270741	0.692715	0.076991	0.032 (3)
C1g	−0.02619 (4)	0.82657 (4)	0.06962 (3)	0.0145 (17)
C2g	−0.06769 (4)	0.82642 (4)	0.10769 (3)	0.0144 (17)
C3g	−0.14183 (5)	0.83176 (4)	0.10249 (3)	0.0171 (19)
C4g	−0.17275 (5)	0.83723 (3)	0.05802 (3)	0.0206 (17)
C5g	−0.13053 (5)	0.83734 (4)	0.01987 (3)	0.0212 (17)
C6g	−0.05570 (5)	0.83195 (4)	0.02511 (3)	0.0179 (19)
H1c3g	−0.170859	0.831696	0.128597	0.032 (4)
H1c4g	−0.223917	0.840996	0.053494	0.038 (3)
H1c5g	−0.15321	0.841174	−0.010341	0.039 (3)
H1c6g	−0.02629	0.831977	−0.000825	0.033 (4)
C1h	−0.18413 (4)	0.95305 (6)	0.12044 (2)	0.0141 (14)
C2h	−0.11141 (5)	0.94886 (6)	0.13364 (2)	0.0139 (14)
C3h	−0.05968 (4)	0.95337 (11)	0.10158 (3)	0.0171 (15)
C4h	−0.08328 (6)	0.96217 (6)	0.05607 (3)	0.0193 (14)
C5h	−0.15664 (6)	0.96633 (6)	0.04307 (3)	0.0193 (14)
C6h	−0.20886 (5)	0.96178 (11)	0.07542 (3)	0.0174 (15)
H1c3h	−0.00937	0.950527	0.110425	0.024 (3)
H1c4h	−0.04857	0.965427	0.033231	0.027 (3)
H1c5h	−0.171367	0.972386	0.011516	0.027 (3)
H1c6h	−0.259274	0.964576	0.066861	0.024 (3)
C1i	0.19282 (5)	1.07538 (8)	0.37540 (2)	0.0149 (15)
C2i	0.11878 (5)	1.07404 (8)	0.36586 (2)	0.0141 (15)
C3i	0.07196 (4)	1.07885 (15)	0.40084 (3)	0.0170 (17)
C4i	0.10180 (6)	1.08503 (8)	0.44549 (3)	0.0200 (15)
C5i	0.17644 (6)	1.08634 (8)	0.45478 (3)	0.0206 (16)
C6i	0.22371 (4)	1.08149 (15)	0.41948 (4)	0.0186 (17)
H1c3i	0.020782	1.07796	0.394536	0.027 (3)
H1c4i	0.070569	1.088443	0.470291	0.032 (3)
H1c5i	0.195506	1.090637	0.485816	0.033 (3)
H1c6i	0.274953	1.082337	0.425497	0.030 (4)
C1j	0.03124 (4)	1.20016 (3)	0.42788 (3)	0.0142 (15)
C2j	0.07216 (4)	1.19644 (3)	0.38971 (3)	0.0140 (15)
C3j	0.14635 (5)	1.20184 (4)	0.39403 (3)	0.0165 (17)
C4j	0.17791 (5)	1.21105 (3)	0.43772 (3)	0.0186 (15)
C5j	0.13628 (5)	1.21474 (3)	0.47598 (3)	0.0185 (15)
C6j	0.06140 (5)	1.20930 (4)	0.47164 (3)	0.0168 (17)
H1c3j	0.174973	1.199319	0.367838	0.029 (3)
H1c4j	0.22913	1.214926	0.441619	0.033 (3)
H1c5j	0.159404	1.2211	0.505639	0.032 (3)
H1c6j	0.032393	1.211762	0.49765	0.029 (4)
C1k	0.18188 (5)	0.33507 (7)	0.39299 (2)	0.0129 (11)
C2k	0.10995 (6)	0.32247 (7)	0.38568 (2)	0.0124 (11)
C3k	0.06509 (7)	0.32098 (14)	0.42198 (3)	0.0148 (12)
C4k	0.09469 (6)	0.33251 (7)	0.46563 (3)	0.0170 (11)
C5k	0.16719 (6)	0.34516 (8)	0.47268 (3)	0.0172 (12)
C6k	0.21249 (7)	0.34666 (15)	0.43605 (3)	0.0155 (13)
H1c3k	0.015374	0.312317	0.417213	0.018 (3)
H1c4k	0.064788	0.331752	0.491311	0.022 (2)
H1c5k	0.18615	0.352924	0.503073	0.022 (2)
H1c6k	0.262262	0.35529	0.440523	0.019 (3)
C1l	0.02252 (4)	0.44110 (4)	0.43912 (3)	0.0160 (12)
C2l	0.07050 (4)	0.44132 (4)	0.40438 (3)	0.0147 (12)
C3l	0.14255 (5)	0.45207 (5)	0.41401 (3)	0.0173 (13)
C4l	0.16470 (5)	0.46253 (4)	0.45943 (3)	0.0210 (12)
C5l	0.11600 (5)	0.46221 (4)	0.49420 (3)	0.0230 (12)
C6l	0.04328 (5)	0.45137 (5)	0.48450 (3)	0.0207 (14)
H1c3l	0.176007	0.452303	0.390219	0.022 (3)
H1c4l	0.214253	0.470076	0.466982	0.028 (2)
H1c5l	0.132708	0.469544	0.525157	0.031 (2)
H1c6l	0.009482	0.45106	0.50809	0.028 (3)
C1m	0.05857 (4)	0.70639 (3)	0.43594 (3)	0.0137 (12)
C2m	0.10334 (4)	0.70601 (3)	0.39946 (3)	0.0141 (12)
C3m	0.17738 (5)	0.70980 (4)	0.40727 (3)	0.0173 (13)
C4m	0.20484 (5)	0.71396 (3)	0.45268 (3)	0.0198 (12)
C5m	0.15934 (5)	0.71432 (4)	0.48921 (3)	0.0189 (12)
C6m	0.08460 (5)	0.71049 (5)	0.48134 (3)	0.0159 (14)
H1c3m	0.208654	0.709558	0.382278	0.021 (3)
H1c4m	0.255866	0.716635	0.459	0.025 (2)
H1c5m	0.179675	0.717228	0.520116	0.023 (2)
H1c6m	0.052961	0.710703	0.506145	0.018 (3)
C1n	0.20130 (5)	0.83026 (7)	0.38256 (2)	0.0143 (14)
C2n	0.12831 (5)	0.82727 (7)	0.36973 (2)	0.0143 (14)
C3n	0.07729 (5)	0.83077 (12)	0.40236 (3)	0.0185 (16)
C4n	0.10188 (6)	0.83733 (6)	0.44806 (3)	0.0219 (14)
C5n	0.17550 (6)	0.84030 (7)	0.46068 (3)	0.0224 (14)
C6n	0.22701 (5)	0.83677 (12)	0.42775 (3)	0.0190 (16)
H1c3n	0.026803	0.828736	0.393776	0.026 (3)
H1c4n	0.067676	0.839853	0.471293	0.031 (3)
H1c5n	0.190915	0.844825	0.492378	0.032 (3)
H1c6n	0.277592	0.838768	0.436053	0.027 (3)
C1o	0.03487 (4)	0.95116 (3)	0.43006 (3)	0.0149 (15)
C2o	0.07136 (4)	0.94934 (3)	0.38988 (3)	0.0150 (15)
C3o	0.14564 (5)	0.95409 (4)	0.39123 (3)	0.0183 (16)
C4o	0.18188 (4)	0.96070 (3)	0.43404 (4)	0.0213 (15)
C5o	0.14468 (4)	0.96249 (3)	0.47433 (4)	0.0214 (15)
C6o	0.06970 (5)	0.95770 (4)	0.47299 (3)	0.0184 (17)
H1c3o	0.171234	0.952874	0.363645	0.028 (3)
H1c4o	0.233267	0.964088	0.435896	0.034 (3)
H1c5o	0.170968	0.96708	0.503323	0.034 (3)
H1c6o	0.043718	0.958873	0.500413	0.028 (4)
C1p	0.19497 (6)	0.56456 (8)	0.38341 (3)	0.0120 (14)	0.8763 (8)
C2p	0.12249 (7)	0.57482 (8)	0.38687 (3)	0.0122 (14)	0.8763 (8)
C3p	0.09723 (7)	0.58996 (15)	0.42818 (4)	0.0163 (15)	0.8763 (8)
C4p	0.14691 (7)	0.59443 (8)	0.46571 (3)	0.0194 (14)	0.8763 (8)
C5p	0.21982 (7)	0.58402 (8)	0.46191 (3)	0.0213 (14)	0.8763 (8)
C6p	0.24533 (7)	0.56874 (15)	0.42022 (4)	0.0179 (16)	0.8763 (8)
H1c3p	0.047271	0.597111	0.430854	0.021 (3)	0.8763 (8)
H1c4p	0.130799	0.604844	0.494671	0.025 (3)	0.8763 (8)
H1c5p	0.25282	0.58741	0.488284	0.029 (3)	0.8763 (8)
H1c6p	0.295197	0.561513	0.417268	0.023 (3)	0.8763 (8)
C1q	0.1895 (3)	0.5644 (4)	0.37939 (17)	0.03 (2)	0.1237 (8)
C2q	0.1220 (3)	0.5697 (4)	0.39667 (17)	0.02 (2)	0.1237 (8)
C3q	0.11516 (17)	0.5860 (7)	0.4411 (2)	0.02 (2)	0.1237 (8)
C4q	0.1781 (3)	0.5967 (4)	0.46743 (16)	0.02 (2)	0.1237 (8)
C5q	0.2459 (3)	0.5912 (4)	0.44974 (17)	0.02 (2)	0.1237 (8)
C6q	0.25275 (17)	0.5749 (7)	0.4049 (3)	0.03 (2)	0.1237 (8)
H1c3q	0.068747	0.589734	0.45326	0.06 (5)	0.1237 (8)
H1c4q	0.174854	0.607984	0.498248	0.06 (4)	0.1237 (8)
H1c5q	0.288284	0.598875	0.468625	0.06 (4)	0.1237 (8)
H1c6q	0.298962	0.571009	0.392488	0.07 (5)	0.1237 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0101 (2)	0.0193 (2)	0.0183 (2)	0.00201 (17)	0.00348 (17)	0.00084 (19)
Na2	0.0111 (2)	0.0178 (2)	0.0173 (2)	−0.00145 (17)	0.00312 (17)	−0.00012 (18)
Na3	0.0113 (2)	0.0186 (2)	0.0159 (2)	0.00063 (17)	0.00248 (17)	0.00065 (18)
Na4	0.0112 (2)	0.0173 (2)	0.0179 (2)	0.00030 (17)	0.00275 (17)	0.00009 (18)
Na5	0.0115 (2)	0.0161 (2)	0.0192 (2)	0.00089 (17)	0.00303 (17)	−0.00016 (18)
Na6	0.0117 (2)	0.0152 (2)	0.0198 (2)	−0.00024 (17)	0.00218 (17)	−0.00003 (18)
Na7	0.0106 (2)	0.0186 (2)	0.0182 (2)	0.00179 (17)	0.00176 (17)	−0.00061 (19)
Na8	0.0145 (2)	0.0196 (3)	0.0196 (2)	0.00294 (18)	0.00151 (18)	−0.0028 (2)
Na9	0.0115 (2)	0.0157 (2)	0.0198 (2)	−0.00040 (17)	0.00297 (17)	0.00040 (19)
Na10	0.0121 (2)	0.0193 (2)	0.0195 (2)	0.00000 (18)	0.00378 (17)	−0.00065 (19)
Na11	0.0114 (2)	0.0234 (3)	0.0162 (2)	0.00050 (18)	0.00146 (17)	−0.0011 (2)
Na12	0.0118 (2)	0.0266 (3)	0.0337 (3)	−0.0001 (2)	0.0017 (2)	−0.0117 (2)
Na13	0.0104 (2)	0.0215 (3)	0.0191 (2)	−0.00122 (18)	0.00393 (17)	0.0009 (2)
Na14	0.0114 (2)	0.0184 (3)	0.0176 (3)	0.0009 (2)	0.00116 (19)	−0.0016 (2)
Na16	0.0120 (3)	0.0330 (4)	0.0191 (3)	−0.0018 (2)	0.0044 (2)	−0.0060 (3)
Na18	0.0178 (3)	0.0182 (3)	0.0165 (3)	0.0009 (2)	0.0001 (2)	0.0000 (2)
O10w	0.0121 (4)	0.0191 (4)	0.0214 (4)	0.0007 (3)	0.0055 (3)	0.0014 (3)
O11w	0.0189 (4)	0.0194 (4)	0.0163 (4)	0.0006 (3)	0.0004 (3)	−0.0015 (3)
O12w	0.0303 (5)	0.0223 (5)	0.0247 (5)	0.0000 (4)	−0.0030 (4)	−0.0021 (4)
O13w	0.0112 (4)	0.0188 (4)	0.0212 (4)	0.0003 (3)	0.0044 (3)	−0.0022 (3)
O14w	0.0117 (3)	0.0185 (4)	0.0179 (4)	0.0001 (3)	0.0027 (3)	−0.0004 (3)
O15w	0.0126 (4)	0.0177 (4)	0.0181 (4)	−0.0001 (3)	0.0027 (3)	−0.0003 (3)
O16w	0.0264 (5)	0.0191 (5)	0.0236 (5)	−0.0009 (4)	−0.0030 (4)	−0.0013 (4)
O17w	0.0239 (5)	0.0221 (5)	0.0245 (5)	0.0015 (4)	−0.0028 (4)	0.0006 (4)
O18w	0.0119 (3)	0.0183 (4)	0.0172 (4)	−0.0010 (3)	0.0012 (3)	−0.0008 (3)
O19w	0.0280 (5)	0.0229 (5)	0.0407 (7)	−0.0069 (4)	−0.0129 (5)	0.0086 (5)
O20w	0.0134 (4)	0.0183 (4)	0.0194 (4)	0.0000 (3)	0.0018 (3)	0.0001 (3)
O21w	0.0132 (4)	0.0184 (4)	0.0234 (5)	−0.0010 (3)	0.0062 (3)	0.0006 (4)
O22w	0.0316 (5)	0.0213 (5)	0.0266 (5)	−0.0002 (4)	−0.0042 (4)	0.0034 (4)
O23w	0.0170 (4)	0.0177 (4)	0.0193 (4)	0.0000 (3)	0.0038 (3)	−0.0001 (3)
O24w	0.0366 (6)	0.0200 (5)	0.0278 (6)	−0.0010 (4)	−0.0079 (4)	−0.0002 (4)
O25w	0.0170 (4)	0.0233 (5)	0.0176 (4)	0.0064 (3)	0.0028 (3)	0.0007 (3)
O26w	0.0184 (4)	0.0178 (4)	0.0166 (4)	−0.0003 (3)	0.0061 (3)	0.0004 (3)
O27w	0.0359 (6)	0.0203 (5)	0.0268 (5)	0.0030 (4)	−0.0086 (4)	−0.0005 (4)
O28w	0.0125 (4)	0.0183 (4)	0.0184 (4)	0.0002 (3)	0.0028 (3)	0.0001 (3)
O29w	0.0166 (4)	0.0176 (4)	0.0171 (4)	−0.0001 (3)	0.0032 (3)	−0.0002 (3)
O30w	0.0120 (3)	0.0173 (4)	0.0179 (4)	0.0012 (3)	0.0015 (3)	−0.0002 (3)
O31w	0.0202 (5)	0.0199 (5)	0.0298 (6)	−0.0034 (4)	0.0070 (4)	0.0000 (4)
O32w	0.0124 (4)	0.0178 (4)	0.0202 (4)	−0.0009 (3)	0.0049 (3)	−0.0011 (3)
O33w	0.0129 (4)	0.0187 (4)	0.0201 (4)	0.0006 (3)	0.0029 (3)	0.0031 (3)
O34w	0.0163 (4)	0.0221 (5)	0.0201 (4)	0.0022 (3)	−0.0022 (3)	−0.0009 (4)
O35w	0.0215 (5)	0.0209 (5)	0.0326 (6)	−0.0035 (4)	0.0017 (4)	−0.0009 (4)
O36w	0.0119 (4)	0.0222 (5)	0.0184 (5)	0.0021 (4)	0.0044 (4)	0.0007 (4)
O38w	0.0156 (5)	0.0201 (5)	0.0182 (5)	−0.0003 (4)	0.0014 (4)	−0.0027 (4)
O40w	0.0385 (7)	0.0240 (6)	0.0241 (6)	0.0135 (5)	−0.0118 (6)	−0.0074 (5)
O42w	0.0216 (5)	0.0219 (6)	0.0257 (6)	−0.0025 (4)	−0.0015 (4)	0.0024 (5)
S11	0.01001 (10)	0.01620 (12)	0.01459 (12)	−0.00011 (9)	0.00217 (9)	0.00057 (10)
O11	0.0168 (4)	0.0202 (4)	0.0216 (4)	−0.0053 (3)	0.0029 (3)	0.0016 (3)
O21	0.0159 (4)	0.0197 (4)	0.0191 (4)	0.0033 (3)	0.0045 (3)	−0.0016 (3)
O31	0.0171 (4)	0.0213 (4)	0.0145 (4)	0.0019 (3)	0.0047 (3)	0.0012 (3)
N11	0.0112 (4)	0.0206 (5)	0.0147 (4)	0.0012 (3)	0.0021 (3)	0.0005 (4)
C71	0.0124 (4)	0.0145 (5)	0.0147 (5)	0.0013 (4)	0.0021 (3)	0.0001 (4)
S12	0.01240 (11)	0.01587 (13)	0.01776 (13)	0.00281 (9)	0.00463 (9)	0.00160 (10)
O12	0.0132 (4)	0.0222 (5)	0.0273 (5)	−0.0027 (3)	0.0035 (3)	0.0060 (4)
O22	0.0310 (5)	0.0224 (5)	0.0297 (6)	0.0122 (4)	0.0127 (4)	0.0003 (4)
O32	0.0120 (4)	0.0233 (5)	0.0241 (5)	−0.0013 (3)	−0.0030 (3)	0.0050 (4)
N12	0.0153 (4)	0.0213 (5)	0.0167 (5)	−0.0002 (4)	0.0021 (3)	0.0018 (4)
C72	0.0132 (5)	0.0151 (5)	0.0175 (5)	−0.0009 (4)	0.0003 (4)	0.0016 (4)
S13	0.01084 (11)	0.01675 (13)	0.01331 (12)	0.00032 (9)	0.00296 (9)	0.00053 (9)
O13	0.0137 (4)	0.0223 (5)	0.0206 (4)	−0.0046 (3)	0.0025 (3)	0.0023 (3)
O23	0.0184 (4)	0.0205 (4)	0.0177 (4)	0.0045 (3)	0.0055 (3)	−0.0014 (3)
O33	0.0121 (4)	0.0280 (5)	0.0139 (4)	0.0026 (3)	0.0041 (3)	0.0005 (3)
N13	0.0095 (4)	0.0206 (5)	0.0147 (4)	0.0018 (3)	0.0022 (3)	0.0002 (4)
C73	0.0104 (4)	0.0174 (5)	0.0143 (5)	0.0011 (4)	0.0026 (3)	−0.0001 (4)
S14	0.01073 (11)	0.01817 (13)	0.02226 (14)	0.00328 (10)	0.00680 (10)	0.00356 (11)
O14	0.0131 (4)	0.0218 (5)	0.0397 (6)	0.0006 (3)	0.0112 (4)	0.0077 (4)
O24	0.0155 (4)	0.0202 (4)	0.0248 (5)	0.0055 (3)	0.0071 (3)	−0.0003 (4)
O34	0.0117 (4)	0.0286 (5)	0.0232 (5)	0.0073 (3)	0.0023 (3)	−0.0001 (4)
N14	0.0140 (4)	0.0229 (5)	0.0195 (5)	0.0060 (4)	0.0067 (4)	0.0039 (4)
C74	0.0117 (4)	0.0180 (5)	0.0184 (5)	0.0032 (4)	0.0044 (4)	0.0004 (4)
S15	0.01051 (11)	0.02178 (14)	0.01436 (12)	0.00022 (10)	0.00236 (9)	0.00256 (10)
O15	0.0173 (4)	0.0286 (5)	0.0218 (5)	−0.0087 (4)	0.0004 (3)	0.0047 (4)
O25	0.0190 (4)	0.0297 (5)	0.0188 (4)	0.0092 (4)	0.0057 (3)	0.0023 (4)
O35	0.0206 (4)	0.0365 (6)	0.0168 (4)	0.0022 (4)	0.0078 (3)	0.0007 (4)
N15	0.0127 (4)	0.0250 (5)	0.0149 (4)	0.0000 (4)	0.0018 (3)	0.0017 (4)
C75	0.0151 (5)	0.0191 (5)	0.0156 (5)	0.0008 (4)	0.0041 (4)	−0.0013 (4)
S16	0.01154 (11)	0.01673 (13)	0.01923 (13)	−0.00247 (9)	0.00598 (9)	−0.00269 (10)
O16	0.0227 (5)	0.0195 (5)	0.0293 (5)	−0.0082 (4)	0.0128 (4)	−0.0041 (4)
O26	0.0142 (4)	0.0241 (5)	0.0289 (5)	0.0007 (3)	0.0091 (3)	−0.0064 (4)
O36	0.0110 (4)	0.0243 (5)	0.0274 (5)	0.0005 (3)	−0.0018 (3)	−0.0039 (4)
N16	0.0154 (4)	0.0200 (5)	0.0191 (5)	−0.0006 (4)	0.0025 (4)	−0.0009 (4)
C76	0.0110 (4)	0.0152 (5)	0.0207 (5)	0.0001 (4)	0.0014 (4)	−0.0021 (4)
S17	0.00936 (10)	0.01696 (13)	0.01515 (12)	−0.00045 (9)	0.00331 (9)	−0.00014 (10)
O17	0.0141 (4)	0.0208 (4)	0.0227 (4)	−0.0047 (3)	0.0051 (3)	0.0009 (3)
O27	0.0165 (4)	0.0188 (4)	0.0208 (4)	0.0035 (3)	0.0049 (3)	−0.0011 (3)
O37	0.0127 (4)	0.0255 (5)	0.0150 (4)	−0.0024 (3)	0.0048 (3)	−0.0018 (3)
N17	0.0089 (4)	0.0232 (5)	0.0163 (4)	−0.0011 (3)	0.0032 (3)	−0.0008 (4)
C77	0.0110 (4)	0.0175 (5)	0.0165 (5)	−0.0019 (4)	0.0032 (4)	−0.0013 (4)
S18	0.01005 (11)	0.01477 (12)	0.01633 (12)	−0.00053 (9)	0.00287 (9)	−0.00001 (10)
O18	0.0151 (4)	0.0186 (4)	0.0252 (5)	−0.0053 (3)	0.0021 (3)	0.0021 (4)
O28	0.0173 (4)	0.0196 (4)	0.0234 (5)	0.0040 (3)	0.0036 (3)	−0.0033 (4)
O38	0.0111 (3)	0.0189 (4)	0.0201 (4)	−0.0001 (3)	−0.0010 (3)	0.0009 (3)
N18	0.0123 (4)	0.0208 (5)	0.0154 (4)	−0.0012 (3)	0.0022 (3)	0.0008 (4)
C78	0.0114 (4)	0.0138 (5)	0.0174 (5)	−0.0003 (3)	0.0014 (4)	−0.0004 (4)
S19	0.00909 (10)	0.01484 (12)	0.01801 (13)	0.00014 (9)	0.00121 (9)	−0.00108 (10)
O19	0.0149 (4)	0.0181 (4)	0.0267 (5)	0.0052 (3)	−0.0005 (3)	−0.0039 (4)
O29	0.0149 (4)	0.0208 (5)	0.0278 (5)	−0.0057 (3)	0.0020 (3)	0.0022 (4)
O39	0.0092 (3)	0.0189 (4)	0.0194 (4)	0.0003 (3)	−0.0003 (3)	−0.0008 (3)
N19	0.0106 (4)	0.0201 (5)	0.0162 (4)	0.0005 (3)	0.0015 (3)	−0.0014 (4)
C79	0.0104 (4)	0.0142 (5)	0.0157 (5)	0.0009 (3)	0.0011 (3)	−0.0001 (4)
S110	0.01023 (11)	0.01868 (13)	0.01535 (12)	−0.00157 (9)	0.00331 (9)	−0.00193 (10)
O110	0.0151 (4)	0.0252 (5)	0.0225 (5)	0.0055 (3)	0.0029 (3)	−0.0027 (4)
O210	0.0201 (4)	0.0236 (5)	0.0214 (5)	−0.0084 (4)	0.0073 (3)	−0.0013 (4)
O310	0.0143 (4)	0.0225 (4)	0.0153 (4)	−0.0035 (3)	0.0052 (3)	−0.0032 (3)
N110	0.0106 (4)	0.0238 (5)	0.0163 (4)	−0.0031 (3)	0.0033 (3)	−0.0034 (4)
C710	0.0110 (4)	0.0164 (5)	0.0163 (5)	−0.0025 (4)	0.0034 (4)	−0.0012 (4)
S111	0.00894 (10)	0.01438 (12)	0.01471 (12)	0.00018 (9)	0.00407 (8)	−0.00019 (9)
O111	0.0111 (3)	0.0210 (4)	0.0226 (4)	0.0046 (3)	0.0052 (3)	−0.0017 (3)
O211	0.0125 (3)	0.0163 (4)	0.0214 (4)	−0.0019 (3)	0.0051 (3)	0.0024 (3)
O311	0.0118 (4)	0.0224 (4)	0.0192 (4)	−0.0036 (3)	−0.0009 (3)	0.0003 (3)
N111	0.0122 (4)	0.0180 (5)	0.0136 (4)	−0.0007 (3)	0.0030 (3)	−0.0008 (3)
C711	0.0113 (4)	0.0146 (5)	0.0137 (5)	−0.0006 (3)	0.0016 (3)	0.0008 (4)
S112	0.01244 (11)	0.01734 (13)	0.01767 (13)	0.00102 (10)	0.00671 (9)	0.00025 (10)
O112	0.0165 (4)	0.0213 (5)	0.0259 (5)	0.0058 (3)	0.0074 (3)	−0.0001 (4)
O212	0.0198 (4)	0.0190 (4)	0.0239 (5)	−0.0022 (3)	0.0094 (3)	0.0020 (4)
O312	0.0147 (4)	0.0314 (5)	0.0172 (4)	−0.0020 (4)	0.0074 (3)	−0.0015 (4)
N112	0.0104 (4)	0.0226 (5)	0.0175 (5)	−0.0007 (3)	0.0045 (3)	−0.0007 (4)
C712	0.0117 (4)	0.0173 (5)	0.0173 (5)	0.0003 (4)	0.0047 (4)	0.0002 (4)
S114	0.00924 (11)	0.02257 (14)	0.01352 (12)	0.00042 (10)	0.00286 (9)	−0.00162 (10)
O114	0.0153 (4)	0.0308 (5)	0.0203 (4)	0.0088 (4)	0.0036 (3)	−0.0033 (4)
O214	0.0179 (4)	0.0274 (5)	0.0190 (4)	−0.0088 (4)	0.0056 (3)	−0.0034 (4)
O314	0.0169 (4)	0.0278 (5)	0.0160 (4)	−0.0013 (3)	0.0068 (3)	−0.0016 (4)
N114	0.0105 (4)	0.0247 (5)	0.0146 (4)	0.0021 (3)	0.0018 (3)	−0.0008 (4)
C714	0.0129 (4)	0.0170 (5)	0.0144 (5)	0.0014 (4)	0.0039 (4)	−0.0003 (4)
S115	0.00816 (10)	0.01469 (12)	0.01629 (12)	0.00025 (9)	0.00207 (9)	0.00021 (9)
O115	0.0151 (4)	0.0191 (4)	0.0261 (5)	0.0062 (3)	0.0027 (3)	−0.0012 (4)
O215	0.0115 (3)	0.0191 (4)	0.0230 (4)	−0.0043 (3)	0.0012 (3)	0.0035 (3)
O315	0.0091 (3)	0.0190 (4)	0.0208 (4)	−0.0007 (3)	−0.0001 (3)	0.0002 (3)
N115	0.0107 (4)	0.0186 (5)	0.0149 (4)	−0.0009 (3)	0.0029 (3)	−0.0009 (3)
C715	0.0098 (4)	0.0130 (5)	0.0174 (5)	−0.0006 (3)	0.0026 (3)	0.0002 (4)
S116	0.01177 (11)	0.01743 (13)	0.01528 (12)	−0.00027 (9)	0.00256 (9)	−0.00085 (10)
O116	0.0161 (4)	0.0233 (5)	0.0225 (5)	0.0054 (3)	0.0034 (3)	−0.0025 (4)
O216	0.0211 (4)	0.0219 (5)	0.0198 (4)	−0.0065 (3)	0.0046 (3)	0.0011 (4)
O316	0.0177 (4)	0.0216 (4)	0.0156 (4)	−0.0001 (3)	0.0047 (3)	0.0005 (3)
N116	0.0115 (4)	0.0221 (5)	0.0159 (4)	−0.0008 (3)	0.0021 (3)	−0.0006 (4)
C716	0.0136 (5)	0.0151 (5)	0.0156 (5)	0.0003 (4)	0.0028 (4)	0.0005 (4)
Na15	0.0131 (18)	0.021 (2)	0.023 (2)	−0.0026 (15)	−0.0013 (15)	−0.0013 (17)
Na17	0.019 (2)	0.052 (4)	0.028 (3)	0.002 (2)	0.0078 (19)	−0.008 (3)
Na19	0.025 (2)	0.055 (4)	0.023 (3)	0.015 (2)	0.0008 (19)	0.010 (2)
O37w	0.015 (4)	0.021 (4)	0.074 (8)	0.000 (3)	−0.008 (5)	−0.015 (5)
O43w	0.015 (3)	0.020 (4)	0.035 (5)	0.003 (3)	−0.002 (3)	−0.001 (3)
O41w	0.012 (3)	0.031 (5)	0.041 (6)	−0.001 (3)	−0.001 (3)	−0.011 (4)
O39w	0.020 (4)	0.023 (4)	0.024 (4)	−0.007 (3)	0.006 (3)	0.004 (3)
S1dia	0.01156 (18)	0.01352 (17)	0.01469 (19)	0.00112 (16)	0.00468 (17)	−0.00004 (13)
O1dia	0.0230 (5)	0.0185 (5)	0.0277 (6)	0.0000 (4)	0.0159 (5)	0.0028 (4)
O2dia	0.0125 (7)	0.0119 (7)	0.0198 (9)	0.0012 (8)	0.0053 (7)	−0.0021 (6)
O3dia	0.0096 (4)	0.0281 (6)	0.0328 (6)	0.0053 (4)	−0.0038 (4)	−0.0084 (5)
N1dia	0.0155 (6)	0.0228 (6)	0.0156 (5)	0.0060 (5)	−0.0001 (4)	−0.0032 (5)
C7dia	0.0104 (5)	0.0178 (6)	0.0180 (6)	0.0024 (4)	0.0001 (4)	−0.0031 (5)
S1dib	0.043 (3)	0.0172 (14)	0.0159 (14)	−0.002 (2)	0.004 (2)	−0.0017 (10)
O1dib	0.0230 (5)	0.0185 (5)	0.0277 (6)	0.0000 (4)	0.0159 (5)	0.0028 (4)
O2dib	0.031 (10)	0.029 (9)	0.025 (7)	−0.013 (5)	−0.002 (6)	−0.008 (5)
O3dib	0.0096 (4)	0.0281 (6)	0.0328 (6)	0.0053 (4)	−0.0038 (4)	−0.0084 (5)
N1dib	0.014 (4)	0.042 (6)	0.017 (4)	0.019 (4)	−0.001 (3)	−0.003 (4)
C7dib	0.009 (4)	0.033 (6)	0.021 (5)	0.007 (4)	−0.008 (3)	−0.006 (4)
C1a	0.0125 (3)	0.015 (3)	0.0150 (4)	0.0006 (6)	0.0013 (3)	0.0012 (8)
C2a	0.0115 (3)	0.014 (3)	0.0163 (4)	0.0005 (6)	0.0023 (3)	0.0005 (8)
C3a	0.0115 (4)	0.018 (4)	0.0230 (3)	0.0006 (7)	0.0031 (3)	0.0006 (8)
C4a	0.0121 (3)	0.020 (3)	0.0284 (4)	0.0006 (6)	−0.0013 (3)	0.0024 (8)
C5a	0.0164 (3)	0.021 (3)	0.0234 (4)	−0.0005 (6)	−0.0047 (3)	0.0036 (8)
C6a	0.0169 (5)	0.019 (4)	0.0166 (3)	−0.0005 (7)	−0.0012 (3)	0.0025 (8)
H1c3a	0.0132 (9)	0.020 (8)	0.0263 (5)	0.0000 (15)	0.0065 (6)	−0.0004 (16)
H1c4a	0.0120 (6)	0.022 (7)	0.0376 (8)	0.0006 (12)	−0.0021 (5)	0.0029 (16)
H1c5a	0.0211 (6)	0.023 (7)	0.0272 (8)	−0.0019 (12)	−0.0090 (5)	0.0054 (16)
H1c6a	0.0221 (10)	0.022 (8)	0.0155 (6)	−0.0017 (15)	−0.0007 (6)	0.0029 (17)
C1b	0.0110 (4)	0.014 (4)	0.0167 (3)	0.0003 (6)	0.0022 (3)	0.0010 (7)
C2b	0.0109 (4)	0.014 (4)	0.0167 (3)	−0.0006 (6)	0.0019 (3)	0.0009 (7)
C3b	0.0125 (3)	0.018 (4)	0.0200 (5)	−0.0008 (5)	0.0046 (2)	0.0012 (8)
C4b	0.0191 (4)	0.019 (4)	0.0175 (3)	−0.0013 (6)	0.0057 (3)	0.0009 (7)
C5b	0.0200 (4)	0.020 (4)	0.0163 (3)	−0.0008 (6)	0.0007 (3)	0.0019 (7)
C6b	0.0136 (3)	0.019 (4)	0.0189 (5)	0.0007 (5)	−0.0002 (2)	0.0024 (8)
H1c3b	0.0123 (3)	0.027 (9)	0.0270 (11)	−0.0003 (10)	0.0061 (3)	0.0034 (17)
H1c4b	0.0258 (8)	0.027 (7)	0.0202 (5)	−0.0018 (12)	0.0099 (5)	0.0018 (14)
H1c5b	0.0278 (8)	0.029 (7)	0.0174 (5)	−0.0012 (12)	−0.0016 (5)	0.0042 (14)
H1c6b	0.0141 (3)	0.029 (9)	0.0251 (11)	0.0021 (10)	−0.0020 (3)	0.0053 (18)
C1c	0.0125 (4)	0.015 (4)	0.0146 (4)	−0.0003 (9)	0.0017 (3)	0.0007 (7)
C2c	0.0107 (4)	0.016 (4)	0.0153 (4)	0.0003 (9)	0.0015 (3)	0.0003 (7)
C3c	0.0107 (4)	0.021 (4)	0.0195 (3)	0.0002 (9)	0.0008 (3)	0.0009 (8)
C4c	0.0129 (4)	0.023 (4)	0.0222 (4)	−0.0013 (9)	−0.0026 (3)	0.0035 (7)
C5c	0.0172 (4)	0.022 (4)	0.0185 (4)	−0.0036 (9)	−0.0032 (3)	0.0042 (7)
C6c	0.0169 (5)	0.019 (4)	0.0150 (4)	−0.0028 (10)	0.0005 (3)	0.0020 (8)
H1c3c	0.0108 (9)	0.034 (9)	0.0224 (6)	0.002 (2)	0.0026 (7)	0.0010 (16)
H1c4c	0.0134 (7)	0.037 (8)	0.0284 (8)	0.0001 (17)	−0.0042 (5)	0.0063 (14)
H1c5c	0.0221 (7)	0.036 (8)	0.0204 (8)	−0.0050 (17)	−0.0058 (5)	0.0077 (14)
H1c6c	0.0212 (9)	0.031 (9)	0.0149 (6)	−0.003 (2)	0.0022 (7)	0.0029 (16)
C1d	0.0116 (4)	0.015 (4)	0.0216 (3)	0.0009 (9)	0.0028 (3)	0.0010 (5)
C2d	0.0118 (4)	0.016 (4)	0.0179 (3)	0.0014 (9)	0.0039 (3)	0.0000 (5)
C3d	0.0173 (3)	0.021 (4)	0.0186 (5)	0.0029 (9)	0.0062 (2)	−0.0009 (6)
C4d	0.0274 (5)	0.025 (4)	0.0174 (3)	0.0043 (9)	0.0042 (3)	−0.0016 (5)
C5d	0.0265 (5)	0.023 (4)	0.0204 (3)	0.0031 (9)	−0.0030 (3)	−0.0016 (5)
C6d	0.0160 (3)	0.019 (5)	0.0255 (5)	0.0012 (10)	−0.0022 (2)	0.0002 (6)
H1c3d	0.0183 (5)	0.035 (9)	0.0228 (11)	0.0060 (19)	0.0097 (4)	0.0009 (13)
H1c4d	0.0389 (9)	0.041 (8)	0.0181 (4)	0.0092 (18)	0.0081 (5)	−0.0002 (10)
H1c5d	0.0369 (9)	0.038 (8)	0.0226 (4)	0.0069 (18)	−0.0074 (5)	−0.0009 (10)
H1c6d	0.0161 (5)	0.030 (10)	0.0344 (11)	0.003 (2)	−0.0043 (4)	0.0028 (13)
C1e	0.0124 (3)	0.016 (5)	0.0157 (4)	−0.0003 (6)	0.0025 (3)	0.0012 (10)
C2e	0.0120 (3)	0.016 (5)	0.0177 (4)	−0.0001 (6)	0.0039 (3)	−0.0008 (10)
C3e	0.0120 (4)	0.019 (5)	0.0232 (4)	−0.0001 (6)	0.0037 (3)	−0.0014 (11)
C4e	0.0128 (3)	0.022 (5)	0.0260 (4)	−0.0004 (6)	0.0002 (3)	0.0005 (10)
C5e	0.0150 (3)	0.023 (5)	0.0221 (4)	−0.0009 (6)	−0.0017 (3)	0.0027 (10)
C6e	0.0146 (4)	0.021 (5)	0.0172 (4)	−0.0008 (6)	0.0004 (3)	0.0031 (11)
H1c3e	0.0124 (8)	0.048 (10)	0.0268 (7)	0.0007 (13)	0.0060 (6)	0.002 (2)
H1c4e	0.0130 (6)	0.054 (9)	0.0323 (8)	0.0004 (11)	−0.0008 (5)	0.0049 (19)
H1c5e	0.0177 (6)	0.056 (9)	0.0246 (8)	−0.0008 (11)	−0.0042 (5)	0.0087 (19)
H1c6e	0.0167 (8)	0.052 (11)	0.0167 (8)	−0.0006 (13)	0.0005 (7)	0.009 (2)
C1f	0.0108 (4)	0.017 (4)	0.0185 (3)	−0.0007 (7)	0.0028 (3)	−0.0018 (7)
C2f	0.0108 (4)	0.015 (4)	0.0187 (3)	−0.0007 (7)	0.0035 (3)	−0.0015 (7)
C3f	0.0161 (3)	0.019 (5)	0.0227 (5)	−0.0024 (7)	0.0083 (2)	−0.0020 (8)
C4f	0.0280 (4)	0.021 (4)	0.0193 (3)	−0.0018 (7)	0.0083 (3)	−0.0003 (7)
C5f	0.0273 (4)	0.025 (4)	0.0184 (3)	0.0014 (7)	−0.0004 (3)	−0.0003 (7)
C6f	0.0153 (3)	0.025 (5)	0.0216 (5)	0.0008 (7)	−0.0012 (2)	−0.0023 (9)
H1c3f	0.0167 (3)	0.039 (10)	0.0319 (11)	−0.0065 (14)	0.0113 (3)	−0.0014 (18)
H1c4f	0.0416 (9)	0.041 (9)	0.0226 (5)	−0.0062 (14)	0.0137 (5)	0.0028 (14)
H1c5f	0.0399 (9)	0.049 (9)	0.0207 (5)	0.0011 (14)	−0.0054 (5)	0.0031 (14)
H1c6f	0.0154 (3)	0.050 (10)	0.0300 (11)	−0.0012 (15)	−0.0045 (4)	−0.0018 (18)
C1g	0.0110 (4)	0.016 (5)	0.0163 (4)	−0.0008 (9)	0.0030 (3)	0.0003 (7)
C2g	0.0102 (4)	0.017 (5)	0.0167 (4)	−0.0007 (9)	0.0030 (3)	−0.0010 (7)
C3g	0.0103 (4)	0.021 (6)	0.0207 (3)	0.0001 (10)	0.0032 (3)	−0.0003 (8)
C4g	0.0114 (4)	0.027 (5)	0.0236 (4)	−0.0003 (9)	0.0002 (3)	0.0030 (7)
C5g	0.0150 (4)	0.028 (5)	0.0199 (4)	−0.0021 (9)	−0.0010 (3)	0.0037 (8)
C6g	0.0148 (5)	0.022 (6)	0.0166 (3)	−0.0017 (10)	0.0021 (3)	0.0017 (8)
H1c3g	0.0117 (9)	0.060 (12)	0.0237 (5)	0.005 (2)	0.0057 (6)	0.0019 (16)
H1c4g	0.0120 (7)	0.073 (10)	0.0301 (8)	0.0042 (18)	−0.0006 (5)	0.0087 (15)
H1c5g	0.0196 (7)	0.076 (10)	0.0220 (8)	0.0003 (18)	−0.0033 (5)	0.0096 (15)
H1c6g	0.0192 (9)	0.063 (12)	0.0168 (6)	0.001 (2)	0.0038 (7)	0.0053 (17)
C1h	0.0112 (4)	0.015 (4)	0.0163 (3)	−0.0003 (5)	0.0017 (3)	−0.0002 (6)
C2h	0.0108 (4)	0.014 (4)	0.0166 (3)	−0.0007 (5)	0.0024 (3)	−0.0004 (6)
C3h	0.0126 (3)	0.020 (4)	0.0192 (5)	−0.0016 (4)	0.0045 (2)	−0.0005 (7)
C4h	0.0182 (4)	0.022 (4)	0.0179 (3)	−0.0030 (5)	0.0057 (2)	−0.0003 (6)
C5h	0.0200 (4)	0.022 (4)	0.0160 (3)	−0.0022 (5)	0.0021 (3)	0.0006 (6)
C6h	0.0149 (3)	0.020 (5)	0.0170 (5)	−0.0004 (4)	0.0001 (2)	0.0006 (8)
H1c3h	0.0121 (3)	0.036 (9)	0.0238 (10)	−0.0011 (8)	0.0053 (3)	0.0012 (16)
H1c4h	0.0226 (8)	0.039 (8)	0.0206 (5)	−0.0041 (10)	0.0090 (5)	0.0012 (12)
H1c5h	0.0266 (8)	0.037 (8)	0.0165 (5)	−0.0026 (10)	0.0012 (5)	0.0032 (12)
H1c6h	0.0158 (3)	0.036 (10)	0.0201 (10)	0.0009 (8)	−0.0020 (3)	0.0031 (16)
C1i	0.0121 (4)	0.016 (5)	0.0168 (3)	0.0006 (4)	0.0002 (2)	−0.0010 (6)
C2i	0.0117 (4)	0.015 (5)	0.0157 (3)	0.0009 (4)	0.0013 (2)	−0.0003 (6)
C3i	0.0148 (2)	0.019 (5)	0.0180 (5)	0.0010 (4)	0.0040 (2)	0.0003 (7)
C4i	0.0227 (4)	0.021 (5)	0.0165 (3)	0.0010 (4)	0.0046 (2)	−0.0001 (6)
C5i	0.0242 (4)	0.022 (5)	0.0159 (3)	0.0003 (4)	−0.0009 (3)	−0.0011 (6)
C6i	0.0166 (2)	0.020 (5)	0.0186 (5)	0.0001 (4)	−0.0027 (2)	−0.0015 (7)
H1c3i	0.0142 (3)	0.044 (10)	0.0232 (10)	0.0011 (5)	0.0056 (3)	−0.0021 (14)
H1c4i	0.0296 (8)	0.049 (9)	0.0189 (4)	0.0013 (9)	0.0088 (5)	−0.0030 (11)
H1c5i	0.0329 (8)	0.049 (9)	0.0169 (5)	−0.0001 (9)	−0.0032 (5)	−0.0048 (11)
H1c6i	0.0173 (3)	0.047 (11)	0.0242 (11)	−0.0006 (5)	−0.0056 (3)	−0.0052 (15)
C1j	0.0123 (4)	0.015 (5)	0.0153 (4)	−0.0002 (8)	0.0023 (3)	−0.0006 (10)
C2j	0.0110 (4)	0.015 (5)	0.0160 (4)	−0.0006 (8)	0.0023 (3)	−0.0009 (10)
C3j	0.0108 (4)	0.020 (5)	0.0190 (4)	0.0001 (9)	0.0018 (3)	−0.0010 (11)
C4j	0.0123 (4)	0.022 (5)	0.0208 (4)	0.0007 (8)	−0.0008 (3)	−0.0013 (10)
C5j	0.0156 (4)	0.021 (5)	0.0182 (4)	0.0015 (8)	−0.0016 (3)	−0.0018 (10)
C6j	0.0155 (4)	0.019 (5)	0.0157 (4)	0.0013 (9)	0.0011 (4)	−0.0013 (11)
H1c3j	0.0112 (9)	0.054 (10)	0.0217 (7)	−0.0030 (19)	0.0037 (7)	−0.006 (2)
H1c4j	0.0127 (7)	0.059 (9)	0.0259 (9)	−0.0026 (16)	−0.0016 (6)	−0.006 (2)
H1c5j	0.0194 (7)	0.056 (9)	0.0203 (9)	−0.0009 (17)	−0.0033 (6)	−0.008 (2)
H1c6j	0.0190 (9)	0.053 (11)	0.0162 (7)	−0.001 (2)	0.0026 (7)	−0.006 (2)
C1k	0.0100 (5)	0.014 (3)	0.0147 (3)	−0.0004 (10)	0.0028 (3)	−0.0003 (5)
C2k	0.0097 (5)	0.014 (3)	0.0137 (3)	0.0001 (10)	0.0028 (3)	0.0007 (5)
C3k	0.0114 (4)	0.018 (4)	0.0158 (4)	0.0002 (10)	0.0047 (3)	0.0014 (6)
C4k	0.0176 (5)	0.020 (3)	0.0143 (3)	0.0004 (10)	0.0055 (3)	0.0010 (5)
C5k	0.0188 (5)	0.019 (3)	0.0138 (3)	−0.0001 (10)	0.0012 (3)	−0.0002 (5)
C6k	0.0129 (4)	0.017 (4)	0.0164 (4)	−0.0008 (10)	0.0004 (3)	−0.0009 (6)
H1c3k	0.0113 (6)	0.023 (8)	0.0206 (9)	−0.001 (2)	0.0059 (4)	0.0015 (13)
H1c4k	0.0238 (9)	0.026 (7)	0.0163 (4)	−0.0002 (19)	0.0092 (5)	0.0010 (10)
H1c5k	0.0262 (9)	0.024 (7)	0.0145 (4)	−0.0009 (19)	−0.0006 (5)	−0.0012 (10)
H1c6k	0.0137 (6)	0.022 (8)	0.0215 (9)	−0.002 (2)	−0.0013 (4)	−0.0023 (14)
C1l	0.0161 (5)	0.016 (4)	0.0166 (4)	0.0017 (10)	0.0050 (3)	0.0004 (9)
C2l	0.0125 (5)	0.015 (4)	0.0168 (4)	0.0003 (10)	0.0035 (3)	0.0005 (9)
C3l	0.0133 (5)	0.017 (4)	0.0216 (4)	−0.0007 (11)	0.0014 (4)	0.0010 (10)
C4l	0.0197 (5)	0.018 (4)	0.0247 (4)	−0.0007 (10)	−0.0031 (3)	−0.0017 (9)
C5l	0.0274 (5)	0.021 (4)	0.0203 (4)	0.0028 (10)	−0.0019 (4)	−0.0043 (9)
C6l	0.0248 (5)	0.021 (4)	0.0169 (4)	0.0044 (11)	0.0041 (4)	−0.0017 (10)
H1c3l	0.0121 (9)	0.028 (8)	0.0254 (8)	−0.002 (2)	0.0029 (8)	0.002 (2)
H1c4l	0.0217 (9)	0.028 (7)	0.0323 (8)	−0.004 (2)	−0.0067 (7)	−0.0025 (18)
H1c5l	0.0370 (9)	0.034 (7)	0.0225 (8)	0.003 (2)	−0.0051 (7)	−0.0085 (18)
H1c6l	0.0312 (10)	0.035 (8)	0.0176 (8)	0.006 (2)	0.0075 (8)	−0.002 (2)
C1m	0.0103 (3)	0.016 (4)	0.0153 (4)	−0.0001 (6)	0.0024 (3)	−0.0001 (6)
C2m	0.0106 (3)	0.016 (4)	0.0164 (4)	−0.0002 (6)	0.0032 (3)	0.0000 (6)
C3m	0.0106 (4)	0.020 (4)	0.0218 (3)	−0.0012 (6)	0.0040 (3)	−0.0017 (6)
C4m	0.0109 (3)	0.024 (4)	0.0247 (4)	−0.0009 (6)	0.0003 (3)	−0.0040 (6)
C5m	0.0141 (4)	0.023 (4)	0.0196 (4)	0.0005 (6)	−0.0015 (3)	−0.0030 (6)
C6m	0.0136 (4)	0.019 (4)	0.0157 (3)	0.0002 (7)	0.0015 (3)	−0.0009 (6)
H1c3m	0.0123 (8)	0.024 (8)	0.0257 (6)	−0.0020 (14)	0.0071 (6)	−0.0022 (12)
H1c4m	0.0111 (6)	0.032 (7)	0.0321 (7)	−0.0013 (12)	−0.0009 (5)	−0.0070 (11)
H1c5m	0.0187 (7)	0.029 (7)	0.0214 (7)	0.0018 (12)	−0.0044 (5)	−0.0048 (11)
H1c6m	0.0173 (8)	0.022 (9)	0.0154 (6)	0.0005 (14)	0.0029 (6)	−0.0008 (12)
C1n	0.0127 (4)	0.014 (4)	0.0159 (3)	−0.0001 (5)	0.0016 (2)	0.0005 (5)
C2n	0.0117 (4)	0.014 (4)	0.0173 (3)	0.0004 (5)	0.0034 (2)	0.0006 (5)
C3n	0.0159 (3)	0.019 (5)	0.0214 (5)	0.0008 (4)	0.0076 (2)	0.0010 (6)
C4n	0.0254 (4)	0.022 (4)	0.0193 (3)	0.0018 (5)	0.0094 (2)	0.0015 (5)
C5n	0.0281 (4)	0.023 (4)	0.0159 (3)	0.0018 (5)	0.0034 (3)	0.0002 (5)
C6n	0.0195 (3)	0.021 (5)	0.0166 (5)	0.0002 (4)	−0.0004 (2)	−0.0004 (6)
H1c3n	0.0148 (3)	0.035 (10)	0.0282 (10)	0.0005 (7)	0.0094 (3)	−0.0012 (13)
H1c4n	0.0326 (8)	0.039 (8)	0.0230 (5)	0.0026 (10)	0.0148 (5)	0.0004 (10)
H1c5n	0.0383 (8)	0.042 (8)	0.0161 (5)	0.0029 (10)	0.0022 (5)	−0.0023 (10)
H1c6n	0.0209 (3)	0.038 (10)	0.0202 (10)	−0.0005 (7)	−0.0040 (3)	−0.0035 (14)
C1o	0.0134 (4)	0.015 (4)	0.0167 (4)	0.0003 (8)	0.0016 (3)	−0.0012 (8)
C2o	0.0128 (4)	0.015 (4)	0.0177 (4)	0.0001 (8)	0.0023 (3)	0.0001 (8)
C3o	0.0130 (5)	0.019 (5)	0.0232 (3)	−0.0009 (9)	0.0031 (3)	0.0003 (8)
C4o	0.0134 (4)	0.023 (4)	0.0272 (4)	−0.0008 (8)	−0.0007 (3)	−0.0015 (8)
C5o	0.0169 (4)	0.024 (4)	0.0228 (4)	0.0004 (8)	−0.0032 (3)	−0.0024 (8)
C6o	0.0172 (5)	0.020 (5)	0.0177 (3)	0.0004 (9)	−0.0002 (3)	−0.0021 (8)
H1c3o	0.0148 (9)	0.044 (10)	0.0265 (5)	−0.0039 (19)	0.0063 (6)	−0.0015 (16)
H1c4o	0.0137 (6)	0.052 (9)	0.0352 (8)	−0.0038 (16)	−0.0011 (5)	−0.0052 (15)
H1c5o	0.0213 (7)	0.053 (9)	0.0258 (8)	−0.0012 (16)	−0.0064 (5)	−0.0066 (15)
H1c6o	0.0218 (10)	0.046 (11)	0.0173 (5)	−0.002 (2)	0.0009 (6)	−0.0055 (16)
C1p	0.0066 (5)	0.014 (4)	0.0157 (4)	0.0004 (9)	0.0019 (3)	−0.0001 (10)
C2p	0.0075 (5)	0.014 (4)	0.0154 (4)	0.0010 (9)	0.0042 (3)	−0.0007 (10)
C3p	0.0156 (4)	0.018 (4)	0.0167 (6)	0.0020 (9)	0.0077 (3)	−0.0005 (11)
C4p	0.0270 (5)	0.017 (4)	0.0143 (4)	0.0032 (9)	0.0042 (3)	−0.0001 (10)
C5p	0.0244 (5)	0.021 (4)	0.0176 (4)	0.0030 (9)	−0.0041 (3)	−0.0025 (10)
C6p	0.0120 (4)	0.021 (5)	0.0203 (6)	0.0012 (10)	−0.0029 (3)	−0.0023 (11)
H1c3p	0.0171 (5)	0.024 (9)	0.0223 (13)	0.0037 (19)	0.0119 (6)	−0.002 (2)
H1c4p	0.0401 (10)	0.020 (8)	0.0145 (7)	0.0062 (19)	0.0067 (6)	0.0003 (19)
H1c5p	0.0349 (10)	0.029 (8)	0.0217 (7)	0.0059 (19)	−0.0107 (7)	−0.0056 (19)
H1c6p	0.0112 (5)	0.030 (10)	0.0284 (13)	0.0024 (19)	−0.0059 (6)	−0.005 (2)
C1q	0.041 (4)	0.02 (6)	0.024 (7)	−0.009 (5)	0.001 (3)	−0.011 (19)
C2q	0.027 (4)	0.02 (6)	0.026 (7)	−0.010 (5)	−0.014 (3)	0.005 (19)
C3q	0.010 (3)	0.02 (7)	0.026 (8)	0.002 (4)	−0.006 (3)	0.01 (2)
C4q	0.011 (4)	0.02 (6)	0.016 (7)	0.002 (5)	−0.002 (3)	0.000 (19)
C5q	0.010 (4)	0.03 (6)	0.025 (7)	0.000 (5)	−0.002 (3)	−0.006 (19)
C6q	0.024 (3)	0.03 (7)	0.033 (8)	−0.001 (4)	0.009 (3)	−0.01 (2)
H1c3q	0.010 (4)	0.11 (14)	0.054 (17)	0.001 (8)	0.000 (5)	−0.01 (4)
H1c4q	0.024 (9)	0.12 (12)	0.027 (13)	−0.002 (10)	0.004 (6)	−0.03 (4)
H1c5q	0.012 (9)	0.13 (12)	0.047 (13)	−0.008 (10)	−0.005 (6)	−0.04 (4)
H1c6q	0.033 (4)	0.12 (14)	0.065 (17)	−0.003 (8)	0.025 (6)	−0.05 (4)

Geometric parameters (Å, º) top

Na1—Na2	3.4831 (7)	C712—C2l	1.5045 (14)
Na1—Na12	3.3954 (8)	S114—O114	1.4503 (11)
Na1—O14w	2.3763 (10)	S114—O214	1.4479 (11)
Na1—O15w	2.3743 (10)	S114—N114	1.6151 (11)
Na1—O38	2.3095 (10)	S114—C1m	1.7660 (7)
Na1—O315	2.3786 (10)	O314—C714	1.2491 (15)
Na1—O316	2.4410 (11)	N114—C714	1.3585 (15)
Na2—Na3	3.5291 (7)	C714—C2m	1.5101 (14)
Na2—O28w	2.4140 (10)	S115—O115	1.4418 (10)
Na2—O30w	2.4135 (10)	S115—O215	1.4571 (10)
Na2—O31	2.4435 (10)	S115—N115	1.6132 (10)
Na2—O38	2.3570 (10)	S115—C1n	1.7642 (8)
Na2—O39	2.3442 (10)	O315—C715	1.2427 (13)
Na3—O18w	2.3431 (10)	N115—C715	1.3715 (15)
Na3—O20w	2.4347 (10)	C715—C2n	1.4994 (14)
Na3—O32	2.3578 (11)	S116—O116	1.4534 (10)
Na3—O39	2.3901 (10)	S116—O216	1.4482 (10)
Na3—O310	2.4399 (10)	S116—N116	1.6159 (11)
Na4—Na8ⁱ	3.6547 (7)	S116—C1o	1.7678 (7)
Na4—O16w	2.3635 (12)	O316—C716	1.2445 (15)
Na4—O21wⁱ	2.3518 (10)	N116—C716	1.3650 (15)
Na4—O32w	2.4290 (11)	C716—C2o	1.5110 (14)
Na4—O33w	2.3819 (10)	Na15—Na17	3.992 (7)
Na4—O115ⁱ	2.4119 (11)	Na15—O43w	2.305 (10)
Na5—Na13ⁱ	3.2567 (7)	Na15—Hao35	1.986 (19)
Na5—O14w	2.3675 (11)	Na15—Hbo35	1.803 (19)
Na5—O27w	2.3304 (13)	Na15—Hao42	1.27 (2)
Na5—O29w	2.4466 (11)	Na15—Hbo42	1.41 (2)
Na5—O30w	2.3296 (11)	Na15—O3dib	2.382 (9)
Na5—O211ⁱ	2.4311 (10)	Na17—Na19	3.342 (7)
Na6—Na16ⁱⁱ	3.5370 (8)	Na17—O37w	2.343 (11)
Na6—O18w	2.3337 (10)	Na19—O37w	2.370 (12)
Na6—O23w	2.4192 (11)	Na19—O41w	2.364 (11)
Na6—O24w	2.3350 (13)	Na19—Hbo38	2.23 (2)
Na6—O28w	2.4095 (11)	Na19—O39w	2.435 (10)
Na6—O24ⁱⁱ	2.4499 (10)	Na19—N1dia	2.340 (5)
Na6—O16ⁱⁱ	2.4190 (11)	Na19—N1dib	2.456 (11)
Na6—Na17ⁱⁱ	3.340 (5)	S1dia—O1dia	1.4503 (15)
Na7—Na13	3.9158 (7)	S1dia—O2dia	1.440 (4)
Na7—O19w	2.3392 (13)	S1dia—N1dia	1.6094 (14)
Na7—O25w	2.3683 (11)	S1dia—S1dib	0.456 (5)
Na7—N13	2.7012 (12)	S1dia—O1dib	1.360 (10)
Na7—O34	2.3328 (10)	S1dia—C1p	1.7648 (13)
Na7—O215ⁱⁱⁱ	2.3937 (9)	S1dia—C1q	1.671 (6)
Na8—Na18	3.8894 (8)	O1dia—O1dib	0.831 (13)
Na8—O17w	2.3577 (12)	O2dia—S1dib	1.522 (6)
Na8—O21w	2.4189 (12)	O2dia—O2dib	0.24 (3)
Na8—O26w	2.3460 (11)	O3dia—C7dia	1.2490 (17)
Na8—O32wⁱⁱⁱ	2.3946 (10)	O3dia—O3dib	1.127 (12)
Na8—O29ⁱⁱⁱ	2.3240 (11)	O3dia—C7dib	1.324 (11)
Na9—Na10ⁱⁱ	3.7397 (7)	N1dia—C7dia	1.355 (2)
Na9—O10wⁱⁱ	2.3592 (10)	N1dia—S1dib	1.193 (5)
Na9—O12w	2.3727 (12)	N1dia—N1dib	0.736 (11)
Na9—O15w	2.3691 (11)	C7dia—N1dib	1.052 (11)
Na9—O34w	2.4160 (11)	C7dia—C7dib	0.734 (12)
Na9—O22^iv	2.3240 (12)	C7dia—C2p	1.4982 (18)
Na10—Na11	3.5817 (7)	S1dib—O1dib	1.471 (12)
Na10—O10w	2.4032 (11)	S1dib—N1dib	1.562 (11)
Na10—O13w^iv	2.4133 (10)	S1dib—C1q	1.770 (8)
Na10—O22w	2.3385 (13)	O3dib—C7dib	1.237 (13)
Na10—O18^iv	2.4019 (11)	N1dib—C7dib	1.355 (16)
Na11—O11w	2.4392 (11)	C7dib—C2p	1.371 (11)
Na11—O31w	2.3258 (12)	C7dib—C2q	1.491 (13)
Na11—O33w^v	2.4395 (11)	C1a—C2a	1.3905 (9)
Na11—O33	2.3574 (10)	C1a—C6a	1.3874 (10)
Na11—O311	2.2946 (10)	C2a—C3a	1.3881 (9)
Na12—O26w	2.3227 (11)	C3a—C4a	1.3956 (11)
Na12—O34w	2.3138 (11)	C3a—H1c3a	0.96
Na12—O36	2.3869 (12)	C4a—C5a	1.4005 (12)
Na12—O315	2.4079 (11)	C4a—H1c4a	0.96
Na13—O29wⁱⁱⁱ	2.3412 (11)	C5a—C6a	1.4011 (10)
Na13—O38w	2.3861 (12)	C5a—H1c5a	0.96
Na13—O312	2.2143 (11)	C6a—H1c6a	0.96
Na13—O2dia	2.430 (4)	C1b—C2b	1.3905 (13)
Na13—O2dib	2.19 (3)	C1b—C6b	1.3874 (15)
Na14—Na16	3.9352 (9)	C2b—C3b	1.3881 (13)
Na14—O36w	2.3294 (13)	C3b—C4b	1.3956 (15)
Na14—O42w	2.2947 (14)	C3b—H1c3b	0.96
Na14—O12^iv	2.4247 (10)	C4b—C5b	1.4005 (16)
Na14—O214	2.4464 (11)	C4b—H1c4b	0.96
Na14—N114	2.7584 (12)	C5b—C6b	1.4011 (15)
Na14—Na15	3.025 (5)	C5b—H1c5b	0.96
Na14—Na17	3.717 (6)	C6b—H1c6b	0.96
Na14—O37w	2.225 (12)	C1c—C2c	1.3905 (11)
Na14—O43w	1.705 (8)	C1c—C6c	1.3874 (12)
Na14—O3dia	2.3905 (12)	C2c—C3c	1.3881 (11)
Na16—O23w^iv	2.4028 (11)	C3c—C4c	1.3956 (13)
Na16—O35w	2.3379 (13)	C3c—H1c3c	0.96
Na16—O36w	2.4232 (14)	C4c—C5c	1.4005 (14)
Na16—O24	2.3327 (11)	C4c—H1c4c	0.96
Na16—O35	2.2387 (12)	C5c—C6c	1.4011 (13)
Na16—Na15	3.452 (5)	C5c—H1c5c	0.96
Na16—Na17	0.977 (7)	C6c—H1c6c	0.96
Na16—Na19	3.248 (5)	C1d—C2d	1.3905 (19)
Na18—O38w	2.3815 (13)	C1d—C6d	1.387 (2)
Na18—O40w	2.3321 (16)	C2d—C3d	1.3881 (15)
Na18—N15	2.4234 (12)	C3d—C4d	1.396 (2)
Na18—Na19	1.537 (5)	C3d—H1c3d	0.96
Na18—O41w	1.959 (10)	C4d—C5d	1.401 (2)
Na18—O39w	1.964 (8)	C4d—H1c4d	0.96
Na18—N1dia	2.5917 (15)	C5d—C6d	1.4011 (16)
O10w—Hbo10	0.760 (18)	C5d—H1c5d	0.96
O10w—Hao10	0.818 (17)	C6d—H1c6d	0.96
O11w—Hao11	0.827 (17)	C1e—C2e	1.3905 (11)
O11w—Hbo11	0.829 (17)	C1e—C6e	1.3874 (12)
O12w—Hao12	0.784 (19)	C2e—C3e	1.3881 (11)
O12w—Hbo12	0.791 (19)	C3e—C4e	1.3956 (13)
O13w—Hao13	0.868 (17)	C3e—H1c3e	0.96
O13w—Hbo13	0.756 (17)	C4e—C5e	1.4005 (14)
O14w—Hbo14	0.894 (17)	C4e—H1c4e	0.96
O14w—Hao14	0.843 (16)	C5e—C6e	1.4011 (13)
O15w—Hao15	0.848 (16)	C5e—H1c5e	0.96
O15w—Hbo15	0.798 (17)	C6e—H1c6e	0.96
O16w—Hao16	0.716 (19)	C1f—C2f	1.3905 (14)
O16w—Hbo16	0.819 (19)	C1f—C6f	1.3874 (13)
O17w—Hao17	0.818 (19)	C2f—C3f	1.3881 (18)
O17w—Hbo17	0.860 (18)	C3f—C4f	1.3956 (14)
O18w—Hao18	0.813 (17)	C3f—H1c3f	0.96
O18w—Hbo18	0.866 (16)	C4f—C5f	1.4005 (17)
O19w—Hao19	0.798 (19)	C4f—H1c4f	0.96
O19w—Hbo19	0.83 (2)	C5f—C6f	1.4011 (19)
O20w—Hao20	0.814 (16)	C5f—H1c5f	0.96
O20w—Hbo20	0.865 (17)	C6f—H1c6f	0.96
O21w—Hao21	0.806 (17)	C1g—C2g	1.3905 (11)
O21w—Hbo21	0.750 (18)	C1g—C6g	1.3874 (11)
O22w—Hao22	0.812 (19)	C2g—C3g	1.3881 (11)
O22w—Hbo22	0.818 (19)	C3g—C4g	1.3956 (13)
O23w—Na17ⁱⁱ	2.292 (5)	C3g—H1c3g	0.96
O23w—Hao23	0.794 (18)	C4g—C5g	1.4005 (14)
O23w—Hbo23	0.847 (18)	C4g—H1c4g	0.96
O24w—Hao24	0.76 (2)	C5g—C6g	1.4011 (13)
O24w—Hbo24	0.76 (2)	C5g—H1c5g	0.96
O25w—Hbo25	0.802 (17)	C6g—H1c6g	0.96
O25w—Hao25	0.865 (17)	C1h—C2h	1.3905 (12)
O26w—Hao26	0.880 (17)	C1h—C6h	1.3874 (13)
O26w—Hbo26	0.735 (18)	C2h—C3h	1.3881 (13)
O27w—Hao27	0.85 (2)	C3h—C4h	1.3956 (14)
O27w—Hbo27	0.75 (2)	C3h—H1c3h	0.96
O28w—Hao28	0.871 (17)	C4h—C5h	1.4005 (15)
O28w—Hbo28	0.850 (16)	C4h—H1c4h	0.96
O29w—Hao29	0.775 (18)	C5h—C6h	1.4011 (14)
O29w—Hbo29	0.882 (17)	C5h—H1c5h	0.96
O30w—Hao30	0.899 (16)	C6h—H1c6h	0.96
O30w—Hbo30	0.817 (17)	C1i—C2i	1.3905 (13)
O31w—Hao31	0.854 (18)	C1i—C6i	1.3874 (13)
O31w—Hbo31	0.764 (18)	C2i—C3i	1.3881 (13)
O32w—Hao32	0.814 (17)	C3i—C4i	1.3956 (14)
O32w—Hbo32	0.803 (18)	C3i—H1c3i	0.96
O33w—Hao33	0.817 (17)	C4i—C5i	1.4005 (15)
O33w—Hbo33	0.816 (17)	C4i—H1c4i	0.96
O34w—Hao34	0.880 (17)	C5i—C6i	1.4011 (15)
O34w—Hbo34	0.816 (17)	C5i—H1c5i	0.96
O35w—Na15	2.171 (5)	C6i—H1c6i	0.96
O35w—Hao35	0.825 (18)	C1j—C2j	1.3905 (11)
O35w—Hbo35	0.869 (19)	C1j—C6j	1.3874 (12)
O36w—Na17	1.873 (6)	C2j—C3j	1.3881 (11)
O36w—O37w	0.659 (9)	C3j—C4j	1.3956 (13)
O38w—Na19	2.384 (6)	C3j—H1c3j	0.96
O38w—Hao38	0.81 (2)	C4j—C5j	1.4005 (14)
O38w—Hbo38	0.78 (2)	C4j—H1c4j	0.96
O38w—O39w	0.732 (9)	C5j—C6j	1.4011 (13)
O40w—Na19	2.286 (6)	C5j—H1c5j	0.96
O40w—O41w	0.743 (11)	C6j—H1c6j	0.96
O40w—Hbo40	0.74 (2)	C1k—C2k	1.3905 (16)
O40w—Hao40	0.78 (2)	C1k—C6k	1.3874 (16)
O42w—Na15	1.476 (5)	C2k—C3k	1.3881 (14)
O42w—O43w	0.931 (9)	C3k—C4k	1.3956 (16)
O42w—Hao42	0.78 (2)	C3k—H1c3k	0.96
O42w—Hbo42	0.78 (2)	C4k—C5k	1.4005 (18)
S11—O11	1.4492 (10)	C4k—H1c4k	0.96
S11—O21	1.4520 (10)	C5k—C6k	1.4011 (15)
S11—N11	1.6148 (11)	C5k—H1c5k	0.96
S11—C1a	1.7611 (6)	C6k—H1c6k	0.96
O31—C71	1.2413 (15)	C1l—C2l	1.3905 (11)
N11—C71	1.3690 (15)	C1l—C6l	1.3874 (12)
C71—C2a	1.5139 (13)	C2l—C3l	1.3881 (12)
S12—O12	1.4571 (10)	C3l—C4l	1.3956 (13)
S12—O22	1.4376 (11)	C3l—H1c3l	0.96
S12—N12	1.6101 (10)	C4l—C5l	1.4005 (14)
S12—C1b	1.7642 (8)	C4l—H1c4l	0.96
O32—C72	1.2473 (14)	C5l—C6l	1.4011 (13)
N12—C72	1.3631 (16)	C5l—H1c5l	0.96
C72—C2b	1.5044 (14)	C6l—H1c6l	0.96
S13—O13	1.4526 (10)	C1m—C2m	1.3905 (11)
S13—O23	1.4495 (10)	C1m—C6m	1.3874 (12)
S13—N13	1.6115 (11)	C2m—C3m	1.3881 (11)
S13—C1c	1.7737 (7)	C3m—C4m	1.3956 (13)
O33—C73	1.2425 (15)	C3m—H1c3m	0.96
N13—C73	1.3645 (14)	C4m—C5m	1.4005 (14)
C73—C2c	1.5017 (14)	C4m—H1c4m	0.96
S14—O14	1.4490 (10)	C5m—C6m	1.4011 (12)
S14—O24	1.4563 (10)	C5m—H1c5m	0.96
S14—N14	1.6171 (11)	C6m—H1c6m	0.96
S14—C1d	1.7577 (8)	C1n—C2n	1.3905 (12)
O34—C74	1.2470 (14)	C1n—C6n	1.3874 (13)
N14—C74	1.3625 (16)	C2n—C3n	1.3881 (13)
C74—C2d	1.4928 (16)	C3n—C4n	1.3956 (13)
S15—O15	1.4516 (11)	C3n—H1c3n	0.96
S15—O25	1.4525 (11)	C4n—C5n	1.4005 (15)
S15—N15	1.5992 (11)	C4n—H1c4n	0.96
S15—C1e	1.7696 (7)	C5n—C6n	1.4011 (14)
O35—C75	1.2359 (16)	C5n—H1c5n	0.96
O35—Na17	2.214 (6)	C6n—H1c6n	0.96
O35—Na19	2.435 (5)	C1o—C2o	1.3905 (11)
N15—C75	1.3651 (15)	C1o—C6o	1.3874 (12)
C75—C2e	1.5098 (14)	C2o—C3o	1.3881 (11)
S16—O16	1.4434 (10)	C3o—C4o	1.3956 (13)
S16—O26	1.4463 (10)	C3o—H1c3o	0.96
S16—C1f	1.7677 (10)	C4o—C5o	1.4005 (14)
O36—C76	1.2502 (14)	C4o—H1c4o	0.96
N16—C76	1.3618 (16)	C5o—C6o	1.4011 (13)
C76—C2f	1.4910 (14)	C5o—H1c5o	0.96
S17—O17	1.4520 (10)	C6o—H1c6o	0.96
S17—O27	1.4473 (10)	C1p—C2p	1.3905 (18)
S17—C1g	1.7675 (7)	C1p—C6p	1.3874 (16)
O37—C77	1.2546 (15)	C1p—C1q	0.147 (5)
N17—C77	1.3527 (15)	C1p—C2q	1.439 (6)
C77—C2g	1.5089 (14)	C1p—C6q	1.252 (7)
S18—O18	1.4384 (10)	C2p—C3p	1.388 (2)
S18—O28	1.4560 (10)	C2p—C1q	1.318 (7)
S18—N18	1.6178 (10)	C2p—C2q	0.314 (7)
S18—C1h	1.7760 (8)	C3p—C4p	1.3956 (17)
O38—C78	1.2449 (14)	C3p—H1c3p	0.96
N18—C78	1.3669 (15)	C3p—C2q	1.204 (8)
C78—C2h	1.4881 (14)	C3p—C3q	0.494 (7)
S19—O19	1.4589 (10)	C3p—H1c3q	0.9223
S19—O29	1.4476 (10)	C4p—C5p	1.401 (2)
S19—N19	1.6073 (10)	C4p—H1c4p	0.96
S19—C1i	1.7713 (8)	C4p—C3q	0.939 (8)
O39—C79	1.2419 (13)	C4p—C4q	0.579 (6)
N19—C79	1.3695 (15)	C5p—C6p	1.401 (2)
C79—C2i	1.4960 (14)	C5p—H1c5p	0.96
S110—O110	1.4499 (10)	C5p—C4q	0.884 (8)
S110—O210	1.4529 (11)	C5p—C5q	0.646 (7)
S110—N110	1.6125 (11)	C6p—H1c6p	0.96
S110—C1j	1.7633 (7)	C6p—C1q	1.534 (5)
O310—C710	1.2454 (15)	C6p—C5q	1.076 (9)
N110—C710	1.3637 (15)	C6p—C6q	0.500 (10)
C710—C2j	1.5169 (14)	H1c3p—H1c3q	0.7625
S111—O111	1.4436 (9)	H1c4p—H1c4q	0.8173
S111—O211	1.4573 (10)	H1c6p—C6q	0.9237
S111—N111	1.6152 (10)	H1c6p—H1c6q	0.7677
S111—C1k	1.7618 (8)	C1q—C2q	1.390 (9)
O311—C711	1.2313 (14)	C1q—C6q	1.387 (9)
N111—C711	1.3777 (15)	C2q—C3q	1.388 (11)
C711—C2k	1.4978 (14)	C3q—C4q	1.396 (9)
S112—O112	1.4519 (10)	C3q—H1c3q	0.96
S112—O212	1.4511 (10)	C4q—C5q	1.401 (9)
S112—N112	1.6110 (11)	C4q—H1c4q	0.96
S112—C1l	1.7747 (8)	C5q—C6q	1.401 (12)
O112—Na15	2.395 (5)	C5q—H1c5q	0.96
O312—C712	1.2371 (15)	C6q—H1c6q	0.96
N112—C712	1.3630 (15)

Na2—Na1—Na12	171.10 (2)	Na16—Na15—O43w	95.2 (3)
Na2—Na1—O14w	93.60 (3)	Na16—Na15—Hao35	51.5 (5)
Na2—Na1—O15w	91.28 (3)	Na16—Na15—Hbo35	58.5 (6)
Na2—Na1—O38	42.24 (3)	Na16—Na15—Hao42	134.4 (10)
Na2—Na1—O315	139.41 (3)	Na16—Na15—Hbo42	91.1 (9)
Na2—Na1—O316	46.04 (2)	Na16—Na15—O3dib	97.1 (3)
Na12—Na1—O14w	78.80 (3)	O35w—Na15—O42w	137.3 (3)
Na12—Na1—O15w	95.85 (3)	O35w—Na15—O112	132.5 (2)
Na12—Na1—O38	132.40 (3)	O35w—Na15—Na17	49.81 (13)
Na12—Na1—O315	45.17 (3)	O35w—Na15—O43w	125.2 (3)
Na12—Na1—O316	138.99 (3)	O35w—Na15—Hao35	22.3 (5)
O14w—Na1—O15w	172.56 (4)	O35w—Na15—Hbo35	22.9 (6)
O14w—Na1—O38	91.21 (4)	O35w—Na15—Hao42	156.1 (10)
O14w—Na1—O315	84.36 (3)	O35w—Na15—Hbo42	132.9 (9)
O14w—Na1—O316	97.53 (4)	O35w—Na15—O3dib	76.7 (3)
O15w—Na1—O38	88.62 (4)	O42w—Na15—O112	89.4 (2)
O15w—Na1—O315	95.57 (4)	O42w—Na15—Na17	91.6 (2)
O15w—Na1—O316	89.90 (4)	O42w—Na15—O43w	13.2 (2)
O38—Na1—O315	175.32 (4)	O42w—Na15—Hao35	123.7 (6)
O38—Na1—O316	88.18 (4)	O42w—Na15—Hbo35	159.9 (7)
O315—Na1—O316	93.91 (4)	O42w—Na15—Hao42	31.9 (10)
Na1—Na2—Na3	179.334 (18)	O42w—Na15—Hbo42	31.3 (9)
Na1—Na2—O28w	90.21 (3)	O42w—Na15—O3dib	88.6 (3)
Na1—Na2—O30w	91.87 (3)	O112—Na15—Na17	167.67 (18)
Na1—Na2—O31	133.81 (3)	O112—Na15—O43w	99.8 (3)
Na1—Na2—O38	41.20 (2)	O112—Na15—Hao35	134.0 (6)
Na1—Na2—O39	137.47 (3)	O112—Na15—Hbo35	110.7 (6)
Na3—Na2—O28w	90.42 (3)	O112—Na15—Hao42	60.9 (10)
Na3—Na2—O30w	87.51 (3)	O112—Na15—Hbo42	90.4 (9)
Na3—Na2—O31	46.38 (2)	O112—Na15—O3dib	100.9 (3)
Na3—Na2—O38	139.01 (3)	Na17—Na15—O43w	83.1 (3)
Na3—Na2—O39	42.30 (2)	Na17—Na15—Hao35	53.9 (5)
O28w—Na2—O30w	176.90 (4)	Na17—Na15—Hbo35	69.0 (6)
O28w—Na2—O31	91.94 (3)	Na17—Na15—Hao42	122.5 (10)
O28w—Na2—O38	90.14 (3)	Na17—Na15—Hbo42	84.1 (9)
O28w—Na2—O39	90.31 (3)	Na17—Na15—O3dib	91.4 (3)
O30w—Na2—O31	84.96 (3)	O43w—Na15—Hao35	110.5 (6)
O30w—Na2—O38	89.90 (4)	O43w—Na15—Hbo35	148.2 (7)
O30w—Na2—O39	89.72 (3)	O43w—Na15—Hao42	39.5 (10)
O31—Na2—O38	92.64 (4)	O43w—Na15—Hbo42	40.3 (9)
O31—Na2—O39	88.66 (3)	O43w—Na15—O3dib	78.8 (3)
O38—Na2—O39	178.60 (4)	Hao35—Na15—Hbo35	40.1 (8)
Na2—Na3—O18w	93.62 (3)	Hao35—Na15—Hao42	134.0 (11)
Na2—Na3—O20w	93.50 (3)	Hao35—Na15—Hbo42	134.8 (11)
Na2—Na3—O32	126.76 (3)	Hao35—Na15—O3dib	54.9 (6)
Na2—Na3—O39	41.31 (2)	Hbo35—Na15—Hao42	163.4 (11)
Na2—Na3—O310	125.33 (3)	Hbo35—Na15—Hbo42	143.6 (10)
O18w—Na3—O20w	172.84 (4)	Hbo35—Na15—O3dib	86.7 (6)
O18w—Na3—O32	91.41 (4)	Hao42—Na15—Hbo42	53.1 (13)
O18w—Na3—O39	92.81 (4)	Hao42—Na15—O3dib	81.3 (10)
O18w—Na3—O310	89.79 (3)	Hbo42—Na15—O3dib	119.0 (9)
O20w—Na3—O32	83.77 (3)	Na6^iv—Na17—Na14	120.39 (15)
O20w—Na3—O39	93.00 (3)	Na6^iv—Na17—Na16	93.5 (3)
O20w—Na3—O310	86.66 (3)	Na6^iv—Na17—O23w^iv	46.42 (9)
O32—Na3—O39	167.60 (4)	Na6^iv—Na17—O36w	139.4 (3)
O32—Na3—O310	107.63 (4)	Na6^iv—Na17—O35	119.5 (2)
O39—Na3—O310	84.05 (3)	Na6^iv—Na17—Na15	109.16 (16)
Na8ⁱ—Na4—O16w	141.28 (3)	Na6^iv—Na17—Na19	163.7 (2)
Na8ⁱ—Na4—O21wⁱ	40.68 (3)	Na6^iv—Na17—O37w	151.0 (3)
Na8ⁱ—Na4—O32w	40.39 (2)	Na14—Na17—Na16	95.7 (3)
Na8ⁱ—Na4—O33w	123.69 (3)	Na14—Na17—O23w^iv	76.17 (15)
Na8ⁱ—Na4—O115ⁱ	101.77 (3)	Na14—Na17—O36w	31.30 (11)
O16w—Na4—O21wⁱ	100.63 (4)	Na14—Na17—O35	120.09 (18)
O16w—Na4—O32w	174.92 (4)	Na14—Na17—Na15	46.03 (9)
O16w—Na4—O33w	94.94 (4)	Na14—Na17—Na19	73.78 (14)
O16w—Na4—O115ⁱ	79.10 (4)	Na14—Na17—O37w	34.5 (3)
O21wⁱ—Na4—O32w	81.00 (4)	Na16—Na17—O23w^iv	84.4 (3)
O21wⁱ—Na4—O33w	164.34 (4)	Na16—Na17—O36w	112.6 (4)
O21wⁱ—Na4—O115ⁱ	95.08 (4)	Na16—Na17—O35	78.7 (3)
O32w—Na4—O33w	83.35 (4)	Na16—Na17—Na15	50.4 (3)
O32w—Na4—O115ⁱ	105.62 (4)	Na16—Na17—Na19	76.0 (3)
O33w—Na4—O115ⁱ	89.42 (4)	Na16—Na17—O37w	101.9 (4)
Na13ⁱ—Na5—O14w	111.80 (3)	O23w^iv—Na17—O36w	103.9 (3)
Na13ⁱ—Na5—O27w	118.95 (4)	O23w^iv—Na17—O35	157.5 (3)
Na13ⁱ—Na5—O29w	45.80 (3)	O23w^iv—Na17—Na15	68.42 (15)
Na13ⁱ—Na5—O30w	117.35 (3)	O23w^iv—Na17—Na19	142.0 (2)
Na13ⁱ—Na5—O211ⁱ	49.39 (2)	O23w^iv—Na17—O37w	110.5 (4)
O14w—Na5—O27w	106.85 (4)	O36w—Na17—O35	96.4 (2)
O14w—Na5—O29w	86.37 (4)	O36w—Na17—Na15	70.85 (18)
O14w—Na5—O30w	104.38 (4)	O36w—Na17—Na19	56.87 (16)
O14w—Na5—O211ⁱ	83.19 (3)	O36w—Na17—O37w	12.7 (2)
O27w—Na5—O29w	163.93 (4)	O35—Na17—Na15	110.3 (2)
O27w—Na5—O30w	95.48 (4)	O35—Na17—Na19	46.74 (13)
O27w—Na5—O211ⁱ	92.61 (4)	O35—Na17—O37w	87.7 (3)
O29w—Na5—O30w	89.84 (4)	Na15—Na17—Na19	74.05 (15)
O29w—Na5—O211ⁱ	79.67 (3)	Na15—Na17—O37w	65.4 (3)
O30w—Na5—O211ⁱ	166.74 (4)	Na19—Na17—O37w	45.2 (3)
Na16ⁱⁱ—Na6—O18w	124.10 (3)	Na16—Na19—Na18	142.1 (3)
Na16ⁱⁱ—Na6—O23w	42.64 (3)	Na16—Na19—O38w	94.13 (18)
Na16ⁱⁱ—Na6—O24w	121.92 (4)	Na16—Na19—O40w	117.3 (2)
Na16ⁱⁱ—Na6—O28w	106.69 (3)	Na16—Na19—O35	43.54 (9)
Na16ⁱⁱ—Na6—O24ⁱⁱ	41.04 (3)	Na16—Na19—Na17	16.96 (12)
Na16ⁱⁱ—Na6—O16ⁱⁱ	64.62 (3)	Na16—Na19—O37w	55.3 (3)
Na16ⁱⁱ—Na6—Na17ⁱⁱ	15.99 (12)	Na16—Na19—O41w	124.2 (3)
O18w—Na6—O23w	88.94 (4)	Na16—Na19—Hbo38	80.3 (5)
O18w—Na6—O24w	99.82 (4)	Na16—Na19—O39w	107.6 (3)
O18w—Na6—O28w	102.35 (4)	Na16—Na19—N1dia	132.2 (2)
O18w—Na6—O24ⁱⁱ	164.59 (4)	Na16—Na19—N1dib	115.0 (3)
O18w—Na6—O16ⁱⁱ	84.74 (4)	Na18—Na19—O38w	71.1 (2)
O18w—Na6—Na17ⁱⁱ	112.02 (12)	Na18—Na19—O40w	72.2 (2)
O23w—Na6—O24w	163.23 (4)	Na18—Na19—O35	100.2 (3)
O23w—Na6—O28w	94.64 (4)	Na18—Na19—Na17	140.4 (3)
O23w—Na6—O24ⁱⁱ	75.99 (4)	Na18—Na19—O37w	147.2 (4)
O23w—Na6—O16ⁱⁱ	80.03 (4)	Na18—Na19—O41w	55.5 (3)
O23w—Na6—Na17ⁱⁱ	43.35 (10)	Na18—Na19—Hbo38	90.1 (6)
O24w—Na6—O28w	97.38 (4)	Na18—Na19—O39w	53.7 (3)
O24w—Na6—O24ⁱⁱ	94.02 (4)	Na18—Na19—N1dia	81.0 (2)
O24w—Na6—O16ⁱⁱ	86.51 (4)	Na18—Na19—N1dib	95.8 (3)
O24w—Na6—Na17ⁱⁱ	119.89 (10)	O38w—Na19—O40w	143.1 (2)
O28w—Na6—O24ⁱⁱ	82.38 (3)	O38w—Na19—O35	89.8 (2)
O28w—Na6—O16ⁱⁱ	171.13 (4)	O38w—Na19—Na17	109.9 (2)
O28w—Na6—Na17ⁱⁱ	121.83 (12)	O38w—Na19—O37w	141.7 (4)
O24ⁱⁱ—Na6—O16ⁱⁱ	89.42 (4)	O38w—Na19—O41w	126.4 (3)
O24ⁱⁱ—Na6—Na17ⁱⁱ	54.30 (12)	O38w—Na19—Hbo38	19.2 (5)
O16ⁱⁱ—Na6—Na17ⁱⁱ	49.72 (12)	O38w—Na19—O39w	17.4 (2)
Na13—Na7—O19w	85.10 (4)	O38w—Na19—N1dia	80.58 (19)
Na13—Na7—O25w	40.63 (3)	O38w—Na19—N1dib	76.7 (3)
Na13—Na7—N13	131.23 (3)	O40w—Na19—O35	99.8 (2)
Na13—Na7—O34	80.83 (3)	O40w—Na19—Na17	100.3 (2)
Na13—Na7—O215ⁱⁱⁱ	69.87 (3)	O40w—Na19—O37w	75.1 (3)
O19w—Na7—O25w	125.53 (5)	O40w—Na19—O41w	18.3 (3)
O19w—Na7—N13	143.24 (4)	O40w—Na19—Hbo38	161.4 (6)
O19w—Na7—O34	91.04 (4)	O40w—Na19—O39w	125.8 (3)
O19w—Na7—O215ⁱⁱⁱ	82.93 (4)	O40w—Na19—N1dia	90.6 (2)
O25w—Na7—N13	90.60 (4)	O40w—Na19—N1dib	104.0 (3)
O25w—Na7—O34	78.31 (4)	O35—Na19—Na17	41.47 (13)
O25w—Na7—O215ⁱⁱⁱ	81.80 (4)	O35—Na19—O37w	82.2 (3)
N13—Na7—O34	90.08 (4)	O35—Na19—O41w	94.6 (3)
N13—Na7—O215ⁱⁱⁱ	111.89 (4)	O35—Na19—Hbo38	88.9 (5)
O34—Na7—O215ⁱⁱⁱ	150.45 (4)	O35—Na19—O39w	92.2 (3)
Na4ⁱⁱⁱ—Na8—Na18	115.435 (18)	O35—Na19—N1dia	169.4 (3)
Na4ⁱⁱⁱ—Na8—O17w	144.88 (3)	O35—Na19—N1dib	154.5 (4)
Na4ⁱⁱⁱ—Na8—O21w	39.33 (2)	Na17—Na19—O37w	44.5 (3)
Na4ⁱⁱⁱ—Na8—O26w	89.34 (3)	Na17—Na19—O41w	108.1 (3)
Na4ⁱⁱⁱ—Na8—O32wⁱⁱⁱ	41.09 (3)	Na17—Na19—Hbo38	97.1 (5)
Na4ⁱⁱⁱ—Na8—O29ⁱⁱⁱ	106.25 (3)	Na17—Na19—O39w	121.6 (3)
Na18—Na8—O17w	96.51 (3)	Na17—Na19—N1dia	138.6 (2)
Na18—Na8—O21w	82.87 (3)	Na17—Na19—N1dib	123.4 (3)
Na18—Na8—O26w	119.67 (3)	O37w—Na19—O41w	91.7 (4)
Na18—Na8—O32wⁱⁱⁱ	140.21 (3)	O37w—Na19—Hbo38	122.7 (6)
Na18—Na8—O29ⁱⁱⁱ	42.48 (3)	O37w—Na19—O39w	159.0 (4)
O17w—Na8—O21w	172.38 (4)	O37w—Na19—N1dia	102.5 (3)
O17w—Na8—O26w	86.93 (4)	O37w—Na19—N1dib	95.0 (4)
O17w—Na8—O32wⁱⁱⁱ	104.54 (4)	O41w—Na19—Hbo38	145.6 (6)
O17w—Na8—O29ⁱⁱⁱ	87.10 (4)	O41w—Na19—O39w	109.0 (4)
O21w—Na8—O26w	86.80 (4)	O41w—Na19—N1dia	94.7 (3)
O21w—Na8—O32wⁱⁱⁱ	80.35 (4)	O41w—Na19—N1dib	110.9 (4)
O21w—Na8—O29ⁱⁱⁱ	97.39 (4)	Hbo38—Na19—O39w	36.6 (6)
O26w—Na8—O32wⁱⁱⁱ	95.16 (4)	Hbo38—Na19—N1dia	80.6 (5)
O26w—Na8—O29ⁱⁱⁱ	160.10 (4)	Hbo38—Na19—N1dib	71.2 (6)
O32wⁱⁱⁱ—Na8—O29ⁱⁱⁱ	104.71 (4)	O39w—Na19—N1dia	80.0 (3)
Na10ⁱⁱ—Na9—O10wⁱⁱ	38.68 (3)	O39w—Na19—N1dib	81.4 (4)
Na10ⁱⁱ—Na9—O12w	137.83 (3)	N1dia—Na19—N1dib	17.4 (2)
Na10ⁱⁱ—Na9—O15w	88.48 (3)	Na14—O37w—O36w	90.8 (11)
Na10ⁱⁱ—Na9—O34w	117.24 (3)	Na14—O37w—Na17	108.9 (4)
Na10ⁱⁱ—Na9—O22^iv	91.42 (3)	Na14—O37w—Na19	135.1 (5)
O10wⁱⁱ—Na9—O12w	99.48 (4)	O36w—O37w—Na17	38.5 (7)
O10wⁱⁱ—Na9—O15w	90.62 (4)	O36w—O37w—Na19	124.8 (12)
O10wⁱⁱ—Na9—O34w	152.54 (4)	Na17—O37w—Na19	90.3 (4)
O10wⁱⁱ—Na9—O22^iv	88.19 (4)	Na14—O43w—O42w	118.0 (7)
O12w—Na9—O15w	86.73 (4)	Na14—O43w—Na15	96.8 (4)
O12w—Na9—O34w	104.59 (4)	O42w—O43w—Na15	21.2 (4)
O12w—Na9—O22^iv	92.16 (4)	Na18—O41w—O40w	111.1 (9)
O15w—Na9—O34w	103.65 (4)	Na18—O41w—Na19	40.3 (2)
O15w—Na9—O22^iv	178.21 (4)	O40w—O41w—Na19	75.0 (8)
O34w—Na9—O22^iv	77.98 (4)	O35w—Hao35—Na15	91.5 (14)
Na9^iv—Na10—Na11	105.872 (17)	O38w—Hbo38—Na19	91.5 (16)
Na9^iv—Na10—O10w	37.84 (2)	O35w—Hbo35—Na15	103.0 (15)
Na9^iv—Na10—O13w^iv	40.21 (3)	Na18—O39w—O38w	116.4 (8)
Na9^iv—Na10—O22w	135.81 (3)	Na18—O39w—Na19	39.1 (2)
Na9^iv—Na10—O18^iv	108.47 (3)	O38w—O39w—Na19	77.4 (7)
Na11—Na10—O10w	77.73 (3)	O42w—Hao42—Na15	89.0 (19)
Na11—Na10—O13w^iv	133.75 (3)	O42w—Hbo42—Na15	79.2 (16)
Na11—Na10—O22w	101.57 (3)	O1dia—S1dia—O2dia	113.53 (16)
Na11—Na10—O18^iv	128.14 (3)	O1dia—S1dia—N1dia	111.59 (8)
O10w—Na10—O13w^iv	77.98 (3)	O1dia—S1dia—S1dib	129.1 (7)
O10w—Na10—O22w	170.75 (5)	O1dia—S1dia—O1dib	34.2 (6)
O10w—Na10—O18^iv	108.78 (4)	O1dia—S1dia—C1p	110.36 (9)
O13w^iv—Na10—O22w	96.46 (4)	O1dia—S1dia—C1q	111.9 (3)
O13w^iv—Na10—O18^iv	96.86 (4)	O2dia—S1dia—N1dia	110.37 (15)
O22w—Na10—O18^iv	79.04 (4)	O2dia—S1dia—S1dib	91.6 (7)
Na10—Na11—O11w	44.23 (3)	O2dia—S1dia—O1dib	122.7 (5)
Na10—Na11—O31w	44.42 (3)	O2dia—S1dia—C1p	111.96 (18)
Na10—Na11—O33w^v	151.47 (3)	O2dia—S1dia—C1q	113.6 (4)
Na10—Na11—O33	82.62 (3)	N1dia—S1dia—S1dib	20.5 (6)
Na10—Na11—O311	92.01 (3)	N1dia—S1dia—O1dib	78.0 (6)
O11w—Na11—O31w	88.32 (4)	N1dia—S1dia—C1p	98.02 (7)
O11w—Na11—O33w^v	159.88 (4)	N1dia—S1dia—C1q	94.2 (2)
O11w—Na11—O33	86.16 (4)	S1dib—S1dia—O1dib	94.9 (9)
O11w—Na11—O311	87.76 (4)	S1dib—S1dia—C1p	98.4 (7)
O31w—Na11—O33w^v	109.85 (4)	S1dib—S1dia—C1q	94.9 (7)
O31w—Na11—O33	89.41 (4)	O1dib—S1dia—C1p	123.1 (4)
O31w—Na11—O311	88.95 (4)	O1dib—S1dia—C1q	122.4 (6)
O33w^v—Na11—O33	85.51 (4)	C1p—S1dia—C1q	3.8 (2)
O33w^v—Na11—O311	100.72 (4)	S1dia—O1dia—O1dib	66.9 (7)
O33—Na11—O311	173.75 (4)	Na13—O2dia—S1dia	125.6 (2)
Na1—Na12—O26w	103.06 (3)	Na13—O2dia—S1dib	109.3 (3)
Na1—Na12—O34w	92.53 (3)	Na13—O2dia—O2dib	14 (7)
Na1—Na12—O36	138.72 (3)	S1dia—O2dia—S1dib	17.41 (19)
Na1—Na12—O315	44.47 (3)	S1dia—O2dia—O2dib	114 (7)
O26w—Na12—O34w	153.05 (5)	S1dib—O2dia—O2dib	97 (7)
O26w—Na12—O36	92.33 (4)	Na14—O3dia—C7dia	155.12 (11)
O26w—Na12—O315	89.65 (4)	Na14—O3dia—O3dib	88.2 (4)
O34w—Na12—O36	90.10 (4)	Na14—O3dia—C7dib	140.4 (5)
O34w—Na12—O315	86.26 (4)	C7dia—O3dia—O3dib	93.0 (4)
O36—Na12—O315	175.38 (4)	C7dia—O3dia—C7dib	33.0 (5)
Na5ⁱⁱⁱ—Na13—Na7	120.847 (19)	O3dib—O3dia—C7dib	60.0 (6)
Na5ⁱⁱⁱ—Na13—O29wⁱⁱⁱ	48.52 (3)	Na18—N1dia—Na19	35.87 (13)
Na5ⁱⁱⁱ—Na13—O38w	138.67 (4)	Na18—N1dia—S1dia	115.33 (7)
Na5ⁱⁱⁱ—Na13—O312	125.00 (3)	Na18—N1dia—C7dia	131.44 (10)
Na5ⁱⁱⁱ—Na13—O2dia	49.30 (9)	Na18—N1dia—S1dib	117.3 (3)
Na5ⁱⁱⁱ—Na13—O2dib	50.8 (8)	Na18—N1dia—N1dib	119.8 (8)
Na7—Na13—O29wⁱⁱⁱ	76.30 (3)	Na19—N1dia—S1dia	151.10 (16)
Na7—Na13—O38w	64.81 (3)	Na19—N1dia—C7dia	97.67 (16)
Na7—Na13—O312	105.13 (3)	Na19—N1dia—S1dib	151.9 (3)
Na7—Na13—O2dia	149.77 (9)	Na19—N1dia—N1dib	90.2 (8)
Na7—Na13—O2dib	150.2 (9)	S1dia—N1dia—C7dia	110.63 (11)
O29wⁱⁱⁱ—Na13—O38w	104.30 (4)	S1dia—N1dia—S1dib	7.7 (2)
O29wⁱⁱⁱ—Na13—O312	168.86 (4)	S1dia—N1dia—N1dib	112.0 (8)
O29wⁱⁱⁱ—Na13—O2dia	80.56 (10)	C7dia—N1dia—S1dib	110.3 (3)
O29wⁱⁱⁱ—Na13—O2dib	81.9 (8)	C7dia—N1dia—N1dib	50.4 (9)
O38w—Na13—O312	86.05 (4)	S1dib—N1dia—N1dib	105.7 (8)
O38w—Na13—O2dia	103.21 (9)	O3dia—C7dia—N1dia	124.39 (14)
O38w—Na13—O2dib	102.2 (8)	O3dia—C7dia—N1dib	111.5 (5)
O312—Na13—O2dia	101.34 (10)	O3dia—C7dia—C7dib	79.1 (8)
O312—Na13—O2dib	100.2 (8)	O3dia—C7dia—C2p	121.73 (14)
O2dia—Na13—O2dib	1.5 (8)	N1dia—C7dia—N1dib	32.6 (6)
Na16—Na14—O36w	34.88 (3)	N1dia—C7dia—C7dib	126.9 (10)
Na16—Na14—O42w	75.94 (4)	N1dia—C7dia—C2p	113.87 (12)
Na16—Na14—O12^iv	82.12 (3)	N1dib—C7dia—C7dib	97.1 (12)
Na16—Na14—O214	174.30 (3)	N1dib—C7dia—C2p	117.5 (5)
Na16—Na14—N114	127.37 (3)	C7dib—C7dia—C2p	65.8 (9)
Na16—Na14—Na15	57.72 (9)	S1dia—S1dib—O2dia	71.0 (6)
Na16—Na14—Na17	14.30 (11)	S1dia—S1dib—N1dia	151.8 (9)
Na16—Na14—O37w	41.9 (2)	S1dia—S1dib—O1dib	67.1 (8)
Na16—Na14—O43w	91.2 (3)	S1dia—S1dib—N1dib	164.7 (9)
Na16—Na14—O3dia	74.68 (3)	S1dia—S1dib—C1q	70.2 (7)
O36w—Na14—O42w	110.80 (5)	O2dia—S1dib—N1dia	134.3 (4)
O36w—Na14—O12^iv	84.46 (4)	O2dia—S1dib—O1dib	110.3 (6)
O36w—Na14—O214	149.70 (5)	O2dia—S1dib—N1dib	118.7 (6)
O36w—Na14—N114	92.72 (4)	O2dia—S1dib—C1q	104.5 (5)
O36w—Na14—Na15	89.86 (9)	N1dia—S1dib—O1dib	89.1 (6)
O36w—Na14—Na17	24.70 (10)	N1dia—S1dib—N1dib	27.0 (4)
O36w—Na14—O37w	16.4 (2)	N1dia—S1dib—C1q	106.9 (4)
O36w—Na14—O43w	125.1 (3)	O1dib—S1dib—N1dib	116.0 (7)
O36w—Na14—O3dia	73.79 (4)	O1dib—S1dib—C1q	110.0 (6)
O42w—Na14—O12^iv	88.54 (4)	N1dib—S1dib—C1q	95.2 (5)
O42w—Na14—O214	99.20 (5)	S1dia—O1dib—O1dia	78.9 (7)
O42w—Na14—N114	155.14 (5)	S1dia—O1dib—S1dib	18.0 (2)
O42w—Na14—Na15	28.19 (9)	O1dia—O1dib—S1dib	96.8 (8)
O42w—Na14—Na17	87.84 (11)	Na13—O2dib—O2dia	165 (8)
O42w—Na14—O37w	113.5 (2)	Na15—O3dib—O3dia	112.0 (6)
O42w—Na14—O43w	21.0 (3)	Na15—O3dib—C7dib	147.1 (10)
O42w—Na14—O3dia	90.45 (5)	O3dia—O3dib—C7dib	67.9 (8)
O12^iv—Na14—O214	100.90 (4)	Na19—N1dib—N1dia	72.3 (7)
O12^iv—Na14—N114	102.11 (4)	Na19—N1dib—C7dia	101.4 (7)
O12^iv—Na14—Na15	105.54 (8)	Na19—N1dib—S1dib	115.9 (6)
O12^iv—Na14—Na17	74.18 (9)	Na19—N1dib—C7dib	119.6 (8)
O12^iv—Na14—O37w	100.7 (2)	N1dia—N1dib—C7dia	96.9 (12)
O12^iv—Na14—O43w	76.2 (3)	N1dia—N1dib—S1dib	47.3 (6)
O12^iv—Na14—O3dia	156.30 (5)	N1dia—N1dib—C7dib	126.7 (14)
O214—Na14—N114	56.98 (3)	C7dia—N1dib—S1dib	104.7 (8)
O214—Na14—Na15	116.64 (9)	C7dia—N1dib—C7dib	32.5 (6)
O214—Na14—Na17	171.39 (11)	S1dib—N1dib—C7dib	113.4 (8)
O214—Na14—O37w	140.9 (2)	O3dia—C7dib—C7dia	67.9 (9)
O214—Na14—O43w	84.9 (3)	O3dia—C7dib—O3dib	52.1 (7)
O214—Na14—O3dia	102.64 (4)	O3dia—C7dib—N1dib	90.7 (8)
N114—Na14—Na15	152.35 (8)	O3dia—C7dib—C2p	126.1 (10)
N114—Na14—Na17	116.56 (10)	O3dia—C7dib—C2q	132.2 (11)
N114—Na14—O37w	86.8 (2)	C7dia—C7dib—O3dib	120.0 (13)
N114—Na14—O43w	141.2 (3)	C7dia—C7dib—N1dib	50.4 (9)
N114—Na14—O3dia	88.46 (4)	C7dia—C7dib—C2p	85.0 (10)
Na15—Na14—Na17	71.79 (14)	C7dia—C7dib—C2q	96.6 (11)
Na15—Na14—O37w	88.0 (3)	O3dib—C7dib—N1dib	123.7 (11)
Na15—Na14—O43w	49.2 (3)	O3dib—C7dib—C2p	128.6 (11)
Na15—Na14—O3dia	65.87 (8)	O3dib—C7dib—C2q	121.9 (11)
Na17—Na14—O37w	36.6 (3)	N1dib—C7dib—C2p	107.0 (8)
Na17—Na14—O43w	100.5 (3)	N1dib—C7dib—C2q	114.4 (8)
Na17—Na14—O3dia	82.12 (9)	C2p—C7dib—C2q	11.7 (4)
O37w—Na14—O43w	131.9 (4)	S11—C1a—C2a	107.78 (4)
O37w—Na14—O3dia	58.3 (2)	S11—C1a—C6a	129.55 (5)
O43w—Na14—O3dia	108.6 (3)	C2a—C1a—C6a	122.66 (5)
Na6^iv—Na16—Na14	110.02 (2)	C71—C2a—C1a	110.30 (6)
Na6^iv—Na16—O23w^iv	43.00 (3)	C71—C2a—C3a	129.06 (7)
Na6^iv—Na16—O35w	149.55 (4)	C1a—C2a—C3a	120.62 (6)
Na6^iv—Na16—O36w	109.73 (4)	C2a—C3a—C4a	117.76 (7)
Na6^iv—Na16—O24	43.60 (3)	C2a—C3a—H1c3a	121.12
Na6^iv—Na16—O35	111.54 (3)	C4a—C3a—H1c3a	121.12
Na6^iv—Na16—Na15	117.86 (7)	C3a—C4a—C5a	121.24 (7)
Na6^iv—Na16—Na17	70.5 (3)	C3a—C4a—H1c4a	119.38
Na6^iv—Na16—Na19	154.20 (11)	C5a—C4a—H1c4a	119.38
Na14—Na16—O23w^iv	70.66 (3)	C4a—C5a—C6a	121.02 (7)
Na14—Na16—O35w	69.52 (3)	C4a—C5a—H1c5a	119.49
Na14—Na16—O36w	33.35 (3)	C6a—C5a—H1c5a	119.49
Na14—Na16—O24	148.76 (3)	C1a—C6a—C5a	116.70 (7)
Na14—Na16—O35	111.56 (4)	C1a—C6a—H1c6a	121.65
Na14—Na16—Na15	47.79 (8)	C5a—C6a—H1c6a	121.65
Na14—Na16—Na17	70.0 (3)	S12—C1b—C2b	106.69 (6)
Na14—Na16—Na19	71.79 (10)	S12—C1b—C6b	130.65 (7)
O23w^iv—Na16—O35w	116.76 (5)	C2b—C1b—C6b	122.66 (8)
O23w^iv—Na16—O36w	85.95 (4)	C72—C2b—C1b	110.99 (8)
O23w^iv—Na16—O24	78.53 (4)	C72—C2b—C3b	128.39 (9)
O23w^iv—Na16—O35	144.41 (5)	C1b—C2b—C3b	120.62 (8)
O23w^iv—Na16—Na15	78.77 (7)	C2b—C3b—C4b	117.76 (9)
O23w^iv—Na16—Na17	71.7 (3)	C2b—C3b—H1c3b	121.12
O23w^iv—Na16—Na19	141.29 (11)	C4b—C3b—H1c3b	121.12
O35w—Na16—O36w	86.55 (4)	C3b—C4b—C5b	121.24 (9)
O35w—Na16—O24	122.71 (5)	C3b—C4b—H1c4b	119.38
O35w—Na16—O35	95.78 (4)	C5b—C4b—H1c4b	119.38
O35w—Na16—Na15	38.27 (8)	C4b—C5b—C6b	121.02 (9)
O35w—Na16—Na17	131.8 (3)	C4b—C5b—H1c5b	119.49
O35w—Na16—Na19	56.13 (11)	C6b—C5b—H1c5b	119.49
O36w—Na16—O24	150.61 (5)	C1b—C6b—C5b	116.70 (9)
O36w—Na16—O35	81.85 (5)	C1b—C6b—H1c6b	121.65
O36w—Na16—Na15	78.80 (8)	C5b—C6b—H1c6b	121.65
O36w—Na16—Na17	45.5 (3)	S13—C1c—C2c	106.74 (5)
O36w—Na16—Na19	56.95 (11)	S13—C1c—C6c	130.59 (6)
O24—Na16—O35	96.43 (4)	C2c—C1c—C6c	122.66 (7)
O24—Na16—Na15	121.49 (8)	C73—C2c—C1c	111.28 (7)
O24—Na16—Na17	105.4 (3)	C73—C2c—C3c	128.10 (8)
O24—Na16—Na19	139.45 (11)	C1c—C2c—C3c	120.62 (7)
O35—Na16—Na15	130.47 (7)	C2c—C3c—C4c	117.76 (8)
O35—Na16—Na17	75.9 (3)	C2c—C3c—H1c3c	121.12
O35—Na16—Na19	48.52 (10)	C4c—C3c—H1c3c	121.12
Na15—Na16—Na17	117.0 (3)	C3c—C4c—C5c	121.24 (8)
Na15—Na16—Na19	83.10 (12)	C3c—C4c—H1c4c	119.38
Na17—Na16—Na19	87.0 (3)	C5c—C4c—H1c4c	119.38
Na8—Na18—O38w	166.91 (4)	C4c—C5c—C6c	121.02 (8)
Na8—Na18—O40w	47.03 (4)	C4c—C5c—H1c5c	119.49
Na8—Na18—N15	95.80 (3)	C6c—C5c—H1c5c	119.49
Na8—Na18—Na19	115.2 (2)	C1c—C6c—C5c	116.70 (8)
Na8—Na18—O41w	35.4 (2)	C1c—C6c—H1c6c	121.65
Na8—Na18—O39w	155.2 (2)	C5c—C6c—H1c6c	121.65
Na8—Na18—N1dia	96.75 (4)	S14—C1d—C2d	106.32 (6)
O38w—Na18—O40w	140.10 (6)	S14—C1d—C6d	130.85 (13)
O38w—Na18—N15	94.55 (4)	C2d—C1d—C6d	122.66 (10)
O38w—Na18—Na19	71.3 (2)	C74—C2d—C1d	111.25 (8)
O38w—Na18—O41w	154.9 (3)	C74—C2d—C3d	128.10 (15)
O38w—Na18—O39w	16.0 (3)	C1d—C2d—C3d	120.62 (12)
O38w—Na18—N1dia	75.68 (5)	C2d—C3d—C4d	117.76 (17)
O40w—Na18—N15	93.48 (5)	C2d—C3d—H1c3d	121.12
O40w—Na18—Na19	69.0 (2)	C4d—C3d—H1c3d	121.12
O40w—Na18—O41w	17.3 (3)	C3d—C4d—C5d	121.24 (11)
O40w—Na18—O39w	156.1 (3)	C3d—C4d—H1c4d	119.38
O40w—Na18—N1dia	83.67 (5)	C5d—C4d—H1c4d	119.38
N15—Na18—Na19	97.19 (19)	C4d—C5d—C6d	121.02 (13)
N15—Na18—O41w	83.3 (3)	C4d—C5d—H1c5d	119.49
N15—Na18—O39w	91.6 (2)	C6d—C5d—H1c5d	119.49
N15—Na18—N1dia	159.82 (5)	C1d—C6d—C5d	116.70 (17)
Na19—Na18—O41w	84.2 (4)	C1d—C6d—H1c6d	121.65
Na19—Na18—O39w	87.2 (3)	C5d—C6d—H1c6d	121.65
Na19—Na18—N1dia	63.10 (19)	S15—C1e—C2e	106.52 (5)
O41w—Na18—O39w	169.3 (3)	S15—C1e—C6e	130.80 (6)
O41w—Na18—N1dia	98.1 (3)	C2e—C1e—C6e	122.66 (7)
O39w—Na18—N1dia	83.5 (2)	C75—C2e—C1e	110.92 (7)
Na9^iv—O10w—Na10	103.48 (4)	C75—C2e—C3e	128.46 (8)
Na9^iv—O10w—Hbo10	99.7 (12)	C1e—C2e—C3e	120.62 (7)
Na9^iv—O10w—Hao10	122.6 (12)	C2e—C3e—C4e	117.76 (8)
Na10—O10w—Hbo10	110.2 (13)	C2e—C3e—H1c3e	121.12
Na10—O10w—Hao10	108.3 (11)	C4e—C3e—H1c3e	121.12
Hbo10—O10w—Hao10	111.9 (18)	C3e—C4e—C5e	121.24 (8)
Na11—O11w—Hao11	122.2 (12)	C3e—C4e—H1c4e	119.38
Na11—O11w—Hbo11	123.0 (12)	C5e—C4e—H1c4e	119.38
Hao11—O11w—Hbo11	107.7 (17)	C4e—C5e—C6e	121.02 (9)
Na9—O12w—Hao12	112.0 (14)	C4e—C5e—H1c5e	119.49
Na9—O12w—Hbo12	130.6 (14)	C6e—C5e—H1c5e	119.49
Hao12—O12w—Hbo12	104.5 (19)	C1e—C6e—C5e	116.70 (8)
Na10ⁱⁱ—O13w—Hao13	139.9 (11)	C1e—C6e—H1c6e	121.65
Na10ⁱⁱ—O13w—Hbo13	93.0 (12)	C5e—C6e—H1c6e	121.65
Hao13—O13w—Hbo13	106.3 (17)	S16—C1f—C2f	106.84 (6)
Na1—O14w—Na5	124.43 (4)	S16—C1f—C6f	130.48 (9)
Na1—O14w—Hbo14	100.4 (10)	C2f—C1f—C6f	122.66 (10)
Na1—O14w—Hao14	103.6 (11)	C76—C2f—C1f	111.15 (8)
Na5—O14w—Hbo14	111.6 (11)	C76—C2f—C3f	128.05 (10)
Na5—O14w—Hao14	107.8 (11)	C1f—C2f—C3f	120.62 (8)
Hbo14—O14w—Hao14	107.8 (15)	C2f—C3f—C4f	117.76 (10)
Na1—O15w—Na9	121.45 (4)	C2f—C3f—H1c3f	121.12
Na1—O15w—Hao15	102.4 (11)	C4f—C3f—H1c3f	121.12
Na1—O15w—Hbo15	100.1 (11)	C3f—C4f—C5f	121.24 (10)
Na9—O15w—Hao15	111.3 (11)	C3f—C4f—H1c4f	119.38
Na9—O15w—Hbo15	110.3 (12)	C5f—C4f—H1c4f	119.38
Hao15—O15w—Hbo15	110.5 (17)	C4f—C5f—C6f	121.02 (9)
Na4—O16w—Hao16	116.7 (15)	C4f—C5f—H1c5f	119.49
Na4—O16w—Hbo16	118.2 (13)	C6f—C5f—H1c5f	119.49
Hao16—O16w—Hbo16	102.8 (19)	C1f—C6f—C5f	116.70 (10)
Na8—O17w—Hao17	126.4 (13)	C1f—C6f—H1c6f	121.65
Na8—O17w—Hbo17	111.8 (12)	C5f—C6f—H1c6f	121.65
Hao17—O17w—Hbo17	105.4 (17)	S17—C1g—C2g	107.38 (5)
Na3—O18w—Na6	127.11 (4)	S17—C1g—C6g	129.95 (6)
Na3—O18w—Hao18	96.3 (11)	C2g—C1g—C6g	122.66 (7)
Na3—O18w—Hbo18	98.6 (11)	C77—C2g—C1g	110.44 (7)
Na6—O18w—Hao18	112.9 (12)	C77—C2g—C3g	128.90 (8)
Na6—O18w—Hbo18	110.7 (11)	C1g—C2g—C3g	120.62 (7)
Hao18—O18w—Hbo18	109.5 (16)	C2g—C3g—C4g	117.76 (8)
Na7—O19w—Hao19	124.2 (15)	C2g—C3g—H1c3g	121.12
Na7—O19w—Hbo19	127.2 (13)	C4g—C3g—H1c3g	121.12
Hao19—O19w—Hbo19	102 (2)	C3g—C4g—C5g	121.24 (8)
Na3—O20w—Hao20	103.7 (12)	C3g—C4g—H1c4g	119.38
Na3—O20w—Hbo20	95.4 (11)	C5g—C4g—H1c4g	119.38
Hao20—O20w—Hbo20	108.3 (16)	C4g—C5g—C6g	121.02 (8)
Na4ⁱⁱⁱ—O21w—Na8	99.99 (4)	C4g—C5g—H1c5g	119.49
Na4ⁱⁱⁱ—O21w—Hao21	126.3 (12)	C6g—C5g—H1c5g	119.49
Na4ⁱⁱⁱ—O21w—Hbo21	107.7 (13)	C1g—C6g—C5g	116.70 (8)
Na8—O21w—Hao21	106.2 (12)	C1g—C6g—H1c6g	121.65
Na8—O21w—Hbo21	107.8 (13)	C5g—C6g—H1c6g	121.65
Hao21—O21w—Hbo21	107.5 (18)	S18—C1h—C2h	106.14 (5)
Na10—O22w—Hao22	110.9 (14)	S18—C1h—C6h	131.18 (7)
Na10—O22w—Hbo22	122.8 (14)	C2h—C1h—C6h	122.66 (7)
Hao22—O22w—Hbo22	102.7 (19)	C78—C2h—C1h	111.77 (8)
Na6—O23w—Na16ⁱⁱ	94.36 (4)	C78—C2h—C3h	127.53 (8)
Na6—O23w—Na17ⁱⁱ	90.24 (14)	C1h—C2h—C3h	120.62 (7)
Na6—O23w—Hao23	124.1 (12)	C2h—C3h—C4h	117.76 (8)
Na6—O23w—Hbo23	113.8 (11)	C2h—C3h—H1c3h	121.12
Na16ⁱⁱ—O23w—Na17ⁱⁱ	23.86 (18)	C4h—C3h—H1c3h	121.12
Na16ⁱⁱ—O23w—Hao23	117.7 (12)	C3h—C4h—C5h	121.24 (9)
Na16ⁱⁱ—O23w—Hbo23	99.9 (11)	C3h—C4h—H1c4h	119.38
Na17ⁱⁱ—O23w—Hao23	101.7 (12)	C5h—C4h—H1c4h	119.38
Na17ⁱⁱ—O23w—Hbo23	122.7 (11)	C4h—C5h—C6h	121.02 (8)
Hao23—O23w—Hbo23	104.7 (17)	C4h—C5h—H1c5h	119.49
Na6—O24w—Hao24	120.4 (15)	C6h—C5h—H1c5h	119.49
Na6—O24w—Hbo24	118.3 (15)	C1h—C6h—C5h	116.70 (8)
Hao24—O24w—Hbo24	104 (2)	C1h—C6h—H1c6h	121.65
Na7—O25w—Hbo25	134.5 (13)	C5h—C6h—H1c6h	121.65
Na7—O25w—Hao25	123.8 (11)	S19—C1i—C2i	106.29 (5)
Hbo25—O25w—Hao25	101.2 (17)	S19—C1i—C6i	131.05 (7)
Na8—O26w—Na12	126.51 (5)	C2i—C1i—C6i	122.66 (7)
Na8—O26w—Hao26	114.0 (11)	C79—C2i—C1i	111.42 (8)
Na8—O26w—Hbo26	97.6 (13)	C79—C2i—C3i	127.95 (9)
Na12—O26w—Hao26	100.7 (11)	C1i—C2i—C3i	120.62 (7)
Na12—O26w—Hbo26	112.1 (13)	C2i—C3i—C4i	117.76 (8)
Hao26—O26w—Hbo26	104.6 (17)	C2i—C3i—H1c3i	121.12
Na5—O27w—Hao27	111.6 (13)	C4i—C3i—H1c3i	121.12
Na5—O27w—Hbo27	130.8 (15)	C3i—C4i—C5i	121.24 (9)
Hao27—O27w—Hbo27	109.1 (19)	C3i—C4i—H1c4i	119.38
Na2—O28w—Na6	126.49 (4)	C5i—C4i—H1c4i	119.38
Na2—O28w—Hao28	101.0 (10)	C4i—C5i—C6i	121.02 (8)
Na2—O28w—Hbo28	98.6 (11)	C4i—C5i—H1c5i	119.49
Na6—O28w—Hao28	108.2 (11)	C6i—C5i—H1c5i	119.49
Na6—O28w—Hbo28	110.8 (11)	C1i—C6i—C5i	116.70 (8)
Hao28—O28w—Hbo28	110.9 (16)	C1i—C6i—H1c6i	121.65
Na5—O29w—Na13ⁱ	85.69 (4)	C5i—C6i—H1c6i	121.65
Na5—O29w—Hao29	119.0 (12)	S110—C1j—C2j	107.22 (5)
Na5—O29w—Hbo29	129.5 (11)	S110—C1j—C6j	130.10 (6)
Na13ⁱ—O29w—Hao29	111.3 (12)	C2j—C1j—C6j	122.66 (7)
Na13ⁱ—O29w—Hbo29	104.5 (11)	C710—C2j—C1j	110.59 (7)
Hao29—O29w—Hbo29	103.2 (17)	C710—C2j—C3j	128.79 (8)
Na2—O30w—Na5	125.63 (4)	C1j—C2j—C3j	120.62 (7)
Na2—O30w—Hao30	96.8 (10)	C2j—C3j—C4j	117.76 (8)
Na2—O30w—Hbo30	97.1 (11)	C2j—C3j—H1c3j	121.12
Na5—O30w—Hao30	113.9 (10)	C4j—C3j—H1c3j	121.12
Na5—O30w—Hbo30	111.4 (12)	C3j—C4j—C5j	121.24 (8)
Hao30—O30w—Hbo30	110.0 (16)	C3j—C4j—H1c4j	119.38
Na11—O31w—Hao31	111.1 (12)	C5j—C4j—H1c4j	119.38
Na11—O31w—Hbo31	124.1 (14)	C4j—C5j—C6j	121.02 (8)
Hao31—O31w—Hbo31	106.0 (19)	C4j—C5j—H1c5j	119.49
Na4—O32w—Na8ⁱ	98.52 (4)	C6j—C5j—H1c5j	119.49
Na4—O32w—Hao32	100.9 (11)	C1j—C6j—C5j	116.70 (8)
Na4—O32w—Hbo32	101.4 (12)	C1j—C6j—H1c6j	121.65
Na8ⁱ—O32w—Hao32	129.4 (12)	C5j—C6j—H1c6j	121.65
Na8ⁱ—O32w—Hbo32	119.4 (11)	S111—C1k—C2k	106.73 (5)
Hao32—O32w—Hbo32	101.8 (17)	S111—C1k—C6k	130.43 (10)
Na4—O33w—Na11^vi	151.03 (5)	C2k—C1k—C6k	122.66 (9)
Na4—O33w—Hao33	99.8 (12)	C711—C2k—C1k	111.41 (8)
Na4—O33w—Hbo33	100.2 (12)	C711—C2k—C3k	127.94 (12)
Na11^vi—O33w—Hao33	91.7 (12)	C1k—C2k—C3k	120.62 (9)
Na11^vi—O33w—Hbo33	102.5 (12)	C2k—C3k—C4k	117.76 (13)
Hao33—O33w—Hbo33	104.6 (16)	C2k—C3k—H1c3k	121.12
Na9—O34w—Na12	124.53 (5)	C4k—C3k—H1c3k	121.12
Na9—O34w—Hao34	104.5 (11)	C3k—C4k—C5k	121.24 (10)
Na9—O34w—Hbo34	100.8 (12)	C3k—C4k—H1c4k	119.38
Na12—O34w—Hao34	111.1 (11)	C5k—C4k—H1c4k	119.38
Na12—O34w—Hbo34	107.0 (12)	C4k—C5k—C6k	121.02 (10)
Hao34—O34w—Hbo34	107.6 (17)	C4k—C5k—H1c5k	119.49
Na16—O35w—Na15	99.89 (12)	C6k—C5k—H1c5k	119.49
Na16—O35w—Hao35	107.9 (13)	C1k—C6k—C5k	116.70 (13)
Na16—O35w—Hbo35	126.9 (11)	C1k—C6k—H1c6k	121.65
Na15—O35w—Hao35	66.2 (13)	C5k—C6k—H1c6k	121.65
Na15—O35w—Hbo35	54.1 (13)	S112—C1l—C2l	106.62 (6)
Hao35—O35w—Hbo35	101.4 (18)	S112—C1l—C6l	130.70 (7)
Na14—O36w—Na16	111.77 (5)	C2l—C1l—C6l	122.66 (8)
Na14—O36w—Na17	124.00 (18)	C712—C2l—C1l	110.95 (8)
Na14—O36w—O37w	72.8 (11)	C712—C2l—C3l	128.43 (8)
Na16—O36w—Na17	21.8 (2)	C1l—C2l—C3l	120.62 (8)
Na16—O36w—O37w	109.9 (9)	C2l—C3l—C4l	117.76 (8)
Na17—O36w—O37w	128.8 (9)	C2l—C3l—H1c3l	121.12
Na13—O38w—Na18	115.53 (5)	C4l—C3l—H1c3l	121.12
Na13—O38w—Na19	127.29 (13)	C3l—C4l—C5l	121.24 (9)
Na13—O38w—Hao38	114.5 (14)	C3l—C4l—H1c4l	119.38
Na13—O38w—Hbo38	100.8 (14)	C5l—C4l—H1c4l	119.38
Na13—O38w—O39w	90.7 (6)	C4l—C5l—C6l	121.02 (9)
Na18—O38w—Na19	37.64 (13)	C4l—C5l—H1c5l	119.49
Na18—O38w—Hao38	114.1 (14)	C6l—C5l—H1c5l	119.49
Na18—O38w—Hbo38	106.6 (15)	C1l—C6l—C5l	116.70 (8)
Na18—O38w—O39w	47.6 (7)	C1l—C6l—H1c6l	121.65
Na19—O38w—Hao38	118.2 (14)	C5l—C6l—H1c6l	121.65
Na19—O38w—Hbo38	69.3 (15)	S114—C1m—C2m	106.87 (5)
Na19—O38w—O39w	85.2 (7)	S114—C1m—C6m	130.45 (6)
Hao38—O38w—Hbo38	103 (2)	C2m—C1m—C6m	122.66 (7)
Hao38—O38w—O39w	92.8 (16)	C714—C2m—C1m	110.94 (7)
Hbo38—O38w—O39w	154.0 (16)	C714—C2m—C3m	128.41 (8)
Na18—O40w—Na19	38.87 (14)	C1m—C2m—C3m	120.62 (7)
Na18—O40w—O41w	51.6 (8)	C2m—C3m—C4m	117.76 (8)
Na18—O40w—Hbo40	132.2 (18)	C2m—C3m—H1c3m	121.12
Na18—O40w—Hao40	120.0 (17)	C4m—C3m—H1c3m	121.12
Na19—O40w—O41w	86.7 (8)	C3m—C4m—C5m	121.24 (8)
Na19—O40w—Hbo40	109.6 (18)	C3m—C4m—H1c4m	119.38
Na19—O40w—Hao40	115.4 (16)	C5m—C4m—H1c4m	119.38
O41w—O40w—Hbo40	152.0 (18)	C4m—C5m—C6m	121.02 (8)
O41w—O40w—Hao40	86.1 (19)	C4m—C5m—H1c5m	119.49
Hbo40—O40w—Hao40	106 (2)	C6m—C5m—H1c5m	119.49
Na14—O42w—Na15	104.56 (19)	C1m—C6m—C5m	116.70 (8)
Na14—O42w—O43w	41.0 (5)	C1m—C6m—H1c6m	121.65
Na14—O42w—Hao42	121.6 (15)	C5m—C6m—H1c6m	121.65
Na14—O42w—Hbo42	127.0 (16)	S115—C1n—C2n	106.95 (5)
Na15—O42w—O43w	145.5 (6)	S115—C1n—C6n	130.39 (7)
Na15—O42w—Hao42	59.1 (16)	C2n—C1n—C6n	122.66 (7)
Na15—O42w—Hbo42	69.5 (16)	C715—C2n—C1n	111.14 (7)
O43w—O42w—Hao42	130.2 (17)	C715—C2n—C3n	128.21 (8)
O43w—O42w—Hbo42	126.7 (16)	C1n—C2n—C3n	120.62 (7)
Hao42—O42w—Hbo42	101 (2)	C2n—C3n—C4n	117.76 (8)
O11—S11—O21	113.99 (6)	C2n—C3n—H1c3n	121.12
O11—S11—N11	111.40 (6)	C4n—C3n—H1c3n	121.12
O11—S11—C1a	110.33 (4)	C3n—C4n—C5n	121.24 (9)
O21—S11—N11	111.38 (6)	C3n—C4n—H1c4n	119.38
O21—S11—C1a	111.20 (4)	C5n—C4n—H1c4n	119.38
N11—S11—C1a	97.36 (4)	C4n—C5n—C6n	121.02 (8)
Na2—O31—C71	129.16 (8)	C4n—C5n—H1c5n	119.49
S11—N11—C71	111.29 (8)	C6n—C5n—H1c5n	119.49
O31—C71—N11	123.86 (10)	C1n—C6n—C5n	116.70 (8)
O31—C71—C2a	122.89 (9)	C1n—C6n—H1c6n	121.65
N11—C71—C2a	113.25 (9)	C5n—C6n—H1c6n	121.65
O12—S12—O22	114.24 (6)	S116—C1o—C2o	106.89 (5)
O12—S12—N12	110.17 (6)	S116—C1o—C6o	130.45 (6)
O12—S12—C1b	110.54 (7)	C2o—C1o—C6o	122.66 (7)
O22—S12—N12	111.83 (6)	C716—C2o—C1o	111.16 (7)
O22—S12—C1b	111.00 (8)	C716—C2o—C3o	128.21 (8)
N12—S12—C1b	97.89 (5)	C1o—C2o—C3o	120.62 (7)
Na14ⁱⁱ—O12—S12	145.63 (6)	C2o—C3o—C4o	117.76 (8)
Na9ⁱⁱ—O22—S12	173.14 (7)	C2o—C3o—H1c3o	121.12
Na3—O32—C72	128.76 (8)	C4o—C3o—H1c3o	121.12
S12—N12—C72	110.91 (9)	C3o—C4o—C5o	121.24 (8)
O32—C72—N12	124.01 (11)	C3o—C4o—H1c4o	119.38
O32—C72—C2b	122.50 (11)	C5o—C4o—H1c4o	119.38
N12—C72—C2b	113.49 (9)	C4o—C5o—C6o	121.02 (9)
O13—S13—O23	114.90 (5)	C4o—C5o—H1c5o	119.49
O13—S13—N13	109.08 (6)	C6o—C5o—H1c5o	119.49
O13—S13—C1c	111.45 (5)	C1o—C6o—C5o	116.70 (8)
O23—S13—N13	112.17 (6)	C1o—C6o—H1c6o	121.65
O23—S13—C1c	110.62 (5)	C5o—C6o—H1c6o	121.65
N13—S13—C1c	97.26 (4)	S1dia—C1p—C2p	106.17 (7)
Na11—O33—C73	124.62 (7)	S1dia—C1p—C6p	131.16 (11)
Na7—N13—S13	91.27 (5)	S1dia—C1p—C1q	49 (3)
Na7—N13—C73	114.52 (8)	S1dia—C1p—C2q	115.4 (2)
S13—N13—C73	111.57 (8)	S1dia—C1p—C6q	114.4 (4)
O33—C73—N13	123.31 (10)	C2p—C1p—C6p	122.66 (12)
O33—C73—C2c	123.58 (9)	C2p—C1p—C1q	58 (3)
N13—C73—C2c	113.11 (9)	C2p—C1p—C2q	12.6 (3)
O14—S14—O24	113.98 (6)	C2p—C1p—C6q	136.5 (6)
O14—S14—N14	111.83 (6)	C6p—C1p—C1q	176 (4)
O14—S14—C1d	111.40 (10)	C6p—C1p—C2q	113.0 (2)
O24—S14—N14	110.47 (6)	C6p—C1p—C6q	21.1 (5)
O24—S14—C1d	110.09 (13)	C1q—C1p—C2q	68 (2)
N14—S14—C1d	97.96 (7)	C1q—C1p—C6q	156 (3)
Na6^iv—O24—Na16	95.36 (4)	C2q—C1p—C6q	129.7 (5)
Na6^iv—O24—S14	145.75 (6)	C7dia—C2p—C7dib	29.2 (5)
Na16—O24—S14	117.42 (5)	C7dia—C2p—C1p	111.15 (10)
Na7—O34—C74	152.53 (9)	C7dia—C2p—C3p	128.13 (12)
S14—N14—C74	110.25 (9)	C7dia—C2p—C1q	105.7 (2)
O34—C74—N14	124.05 (11)	C7dia—C2p—C2q	135.6 (16)
O34—C74—C2d	122.16 (11)	C7dib—C2p—C1p	123.9 (5)
N14—C74—C2d	113.79 (10)	C7dib—C2p—C3p	110.9 (5)
O15—S15—O25	113.56 (6)	C7dib—C2p—C1q	119.2 (6)
O15—S15—N15	111.91 (6)	C7dib—C2p—C2q	106.4 (16)
O15—S15—C1e	110.44 (5)	C1p—C2p—C3p	120.62 (10)
O25—S15—N15	111.20 (6)	C1p—C2p—C1q	5.4 (2)
O25—S15—C1e	110.64 (5)	C1p—C2p—C2q	92.4 (12)
N15—S15—C1e	98.06 (5)	C3p—C2p—C1q	126.0 (3)
Na16—O35—C75	162.66 (9)	C3p—C2p—C2q	48.7 (19)
Na16—O35—Na17	25.33 (18)	C1q—C2p—C2q	96.7 (13)
Na16—O35—Na19	87.94 (13)	C2p—C3p—C4p	117.76 (13)
C75—O35—Na17	148.64 (18)	C2p—C3p—H1c3p	121.12
C75—O35—Na19	109.34 (15)	C2p—C3p—C2q	11.3 (5)
Na17—O35—Na19	91.79 (19)	C2p—C3p—C3q	109.4 (12)
Na18—N15—S15	139.32 (6)	C2p—C3p—H1c3q	156.93
Na18—N15—C75	109.15 (8)	C4p—C3p—H1c3p	121.12
S15—N15—C75	111.22 (8)	C4p—C3p—C2q	112.2 (3)
O35—C75—N15	122.99 (11)	C4p—C3p—C3q	18 (2)
O35—C75—C2e	123.74 (10)	C4p—C3p—H1c3q	77.01
N15—C75—C2e	113.27 (10)	H1c3p—C3p—C2q	125.67
O16—S16—O26	115.34 (6)	H1c3p—C3p—C3q	126.68
O16—S16—C1f	111.67 (9)	H1c3p—C3p—H1c3q	47.74
O26—S16—C1f	110.39 (8)	C2q—C3p—C3q	101.3 (15)
Na6^iv—O16—S16	152.04 (6)	C2q—C3p—H1c3q	150.15
Na12—O36—C76	122.22 (8)	C3q—C3p—H1c3q	79.04
O36—C76—N16	123.79 (12)	C3p—C4p—C5p	121.24 (12)
O36—C76—C2f	122.39 (11)	C3p—C4p—H1c4p	119.38
N16—C76—C2f	113.80 (10)	C3p—C4p—C3q	9.5 (12)
O17—S17—O27	114.50 (6)	C3p—C4p—C4q	133.3 (5)
O17—S17—C1g	109.72 (5)	C5p—C4p—H1c4p	119.38
O27—S17—C1g	111.00 (5)	C5p—C4p—C3q	117.1 (6)
O37—C77—N17	122.82 (10)	C5p—C4p—C4q	20.8 (11)
O37—C77—C2g	123.50 (9)	H1c4p—C4p—C3q	122.74
N17—C77—C2g	113.69 (10)	H1c4p—C4p—C4q	104.65
O18—S18—O28	114.41 (5)	C3q—C4p—C4q	132.3 (7)
O18—S18—N18	111.77 (6)	C4p—C5p—C6p	121.02 (10)
O18—S18—C1h	112.10 (6)	C4p—C5p—H1c5p	119.49
O28—S18—N18	110.10 (6)	C4p—C5p—C4q	13.5 (6)
O28—S18—C1h	109.56 (7)	C4p—C5p—C5q	137.5 (8)
N18—S18—C1h	97.65 (5)	C6p—C5p—H1c5p	119.49
Na10ⁱⁱ—O18—S18	147.78 (6)	C6p—C5p—C4q	129.3 (3)
Na1—O38—Na2	96.55 (4)	C6p—C5p—C5q	47.5 (9)
Na1—O38—C78	127.04 (8)	H1c5p—C5p—C4q	110.14
Na2—O38—C78	116.14 (8)	H1c5p—C5p—C5q	86.44
S18—N18—C78	110.59 (8)	C4q—C5p—C5q	132.0 (12)
O38—C78—N18	123.73 (11)	C1p—C6p—C5p	116.70 (13)
O38—C78—C2h	122.44 (10)	C1p—C6p—H1c6p	121.65
N18—C78—C2h	113.83 (9)	C1p—C6p—C1q	0.4 (4)
O19—S19—O29	111.83 (5)	C1p—C6p—C5q	130.3 (5)
O19—S19—N19	110.64 (6)	C1p—C6p—C6q	64.1 (8)
O19—S19—C1i	111.08 (8)	C5p—C6p—H1c6p	121.65
O29—S19—N19	112.37 (6)	C5p—C6p—C1q	116.7 (3)
O29—S19—C1i	112.27 (8)	C5p—C6p—C5q	26.3 (4)
N19—S19—C1i	97.91 (5)	C5p—C6p—C6q	142 (2)
Na8ⁱ—O29—S19	152.33 (6)	H1c6p—C6p—C1q	121.61
Na2—O39—Na3	96.39 (4)	H1c6p—C6p—C5q	103.82
Na2—O39—C79	122.20 (8)	H1c6p—C6p—C6q	70.62
Na3—O39—C79	117.31 (8)	C1q—C6p—C5q	130.1 (6)
S19—N19—C79	110.75 (8)	C1q—C6p—C6q	63.8 (8)
O39—C79—N19	123.38 (11)	C5q—C6p—C6q	121 (2)
O39—C79—C2i	123.13 (10)	C3p—H1c3p—H1c3q	63.54
N19—C79—C2i	113.50 (9)	C4p—H1c4p—H1c4q	77.53
O110—S110—O210	113.68 (6)	C6p—H1c6p—C6q	30.72
O110—S110—N110	111.82 (6)	C6p—H1c6p—H1c6q	99.11
O110—S110—C1j	110.49 (5)	C6q—H1c6p—H1c6q	68.45
O210—S110—N110	111.64 (6)	S1dia—C1q—S1dib	14.86 (17)
O210—S110—C1j	110.44 (5)	S1dia—C1q—C1p	128 (3)
N110—S110—C1j	97.67 (4)	S1dia—C1q—C2p	115.3 (4)
Na3—O310—C710	126.67 (8)	S1dia—C1q—C6p	127.4 (4)
S110—N110—C710	111.28 (8)	S1dia—C1q—C2q	124.5 (5)
O310—C710—N110	123.65 (10)	S1dia—C1q—C6q	112.7 (5)
O310—C710—C2j	123.21 (9)	S1dib—C1q—C1p	141 (3)
N110—C710—C2j	113.13 (10)	S1dib—C1q—C2p	101.0 (4)
O111—S111—O211	114.48 (5)	S1dib—C1q—C6p	141.5 (5)
O111—S111—N111	112.20 (5)	S1dib—C1q—C2q	109.7 (5)
O111—S111—C1k	110.29 (6)	S1dib—C1q—C6q	127.6 (5)
O211—S111—N111	110.34 (5)	C1p—C1q—C2p	117 (3)
O211—S111—C1k	110.73 (8)	C1p—C1q—C6p	4 (4)
N111—S111—C1k	97.55 (5)	C1p—C1q—C2q	106 (2)
Na5ⁱⁱⁱ—O211—S111	144.54 (5)	C1p—C1q—C6q	22 (3)
Na11—O311—C711	130.52 (8)	C2p—C1q—C6p	117.2 (4)
S111—N111—C711	110.81 (8)	C2p—C1q—C2q	13.0 (3)
O311—C711—N111	123.87 (11)	C2p—C1q—C6q	130.3 (7)
O311—C711—C2k	123.23 (10)	C6p—C1q—C2q	107.3 (4)
N111—C711—C2k	112.89 (9)	C6p—C1q—C6q	18.9 (4)
O112—S112—O212	114.14 (6)	C2q—C1q—C6q	122.7 (6)
O112—S112—N112	111.45 (6)	C7dib—C2q—C1p	112.6 (6)
O112—S112—C1l	109.84 (5)	C7dib—C2q—C2p	61.9 (14)
O212—S112—N112	111.75 (6)	C7dib—C2q—C3p	114.6 (6)
O212—S112—C1l	110.80 (5)	C7dib—C2q—C1q	107.2 (6)
N112—S112—C1l	97.67 (5)	C7dib—C2q—C3q	132.2 (6)
S112—O112—Na15	107.79 (12)	C1p—C2q—C2p	75.0 (11)
Na13—O312—C712	154.19 (9)	C1p—C2q—C3p	131.8 (6)
S112—N112—C712	110.94 (8)	C1p—C2q—C1q	5.6 (2)
O312—C712—N112	122.99 (11)	C1p—C2q—C3q	115.2 (4)
O312—C712—C2l	123.30 (10)	C2p—C2q—C3p	120 (2)
N112—C712—C2l	113.71 (10)	C2p—C2q—C1q	70.3 (12)
O114—S114—O214	114.28 (6)	C2p—C2q—C3q	134 (3)
O114—S114—N114	112.55 (6)	C3p—C2q—C1q	136.6 (7)
O114—S114—C1m	110.21 (5)	C3p—C2q—C3q	20.4 (4)
O214—S114—N114	109.16 (6)	C1q—C2q—C3q	120.6 (5)
O214—S114—C1m	111.88 (5)	C3p—C3q—C4p	152 (4)
N114—S114—C1m	97.58 (4)	C3p—C3q—C2q	58.3 (12)
Na14—O214—S114	104.63 (5)	C3p—C3q—C4q	150 (3)
Na14—N114—S114	87.77 (5)	C3p—C3q—H1c3q	70.6
Na14—N114—C714	123.77 (8)	C4p—C3q—C2q	135.5 (5)
S114—N114—C714	111.26 (8)	C4p—C3q—C4q	17.9 (3)
O314—C714—N114	123.43 (11)	C4p—C3q—H1c3q	103.36
O314—C714—C2m	123.24 (10)	C2q—C3q—C4q	117.8 (5)
N114—C714—C2m	113.33 (10)	C2q—C3q—H1c3q	121.12
O115—S115—O215	114.20 (5)	C4q—C3q—H1c3q	121.12
O115—S115—N115	112.07 (6)	C4p—C4q—C5p	145.7 (17)
O115—S115—C1n	111.67 (7)	C4p—C4q—C3q	29.8 (5)
O215—S115—N115	110.39 (5)	C4p—C4q—C5q	150.8 (10)
O215—S115—C1n	109.67 (7)	C4p—C4q—H1c4q	89.7
N115—S115—C1n	97.63 (5)	C5p—C4q—C3q	122.1 (9)
Na4ⁱⁱⁱ—O115—S115	156.18 (6)	C5p—C4q—C5q	20.0 (5)
Na7ⁱ—O215—S115	130.03 (5)	C5p—C4q—H1c4q	114.55
Na1—O315—Na12	90.37 (4)	C3q—C4q—C5q	121.2 (6)
Na1—O315—C715	121.90 (8)	C3q—C4q—H1c4q	119.38
Na12—O315—C715	124.43 (8)	C5q—C4q—H1c4q	119.38
S115—N115—C715	110.94 (8)	C5p—C5q—C6p	106.3 (12)
O315—C715—N115	123.39 (11)	C5p—C5q—C4q	28.0 (7)
O315—C715—C2n	123.30 (10)	C5p—C5q—C6q	121.1 (12)
N115—C715—C2n	113.31 (9)	C5p—C5q—H1c5q	111.88
O116—S116—O216	114.30 (6)	C6p—C5q—C4q	113.4 (7)
O116—S116—N116	111.61 (6)	C6p—C5q—C6q	17.8 (8)
O116—S116—C1o	109.60 (5)	C6p—C5q—H1c5q	124.35
O216—S116—N116	111.50 (6)	C4q—C5q—C6q	121.0 (5)
O216—S116—C1o	111.07 (5)	C4q—C5q—H1c5q	119.49
N116—S116—C1o	97.54 (5)	C6q—C5q—H1c5q	119.49
Na1—O316—C716	124.43 (8)	C1p—C6q—C6p	94.9 (11)
S116—N116—C716	111.38 (8)	C1p—C6q—H1c6p	141.98
O316—C716—N116	124.05 (11)	C1p—C6q—C1q	2.5 (3)
O316—C716—C2o	122.95 (10)	C1p—C6q—C5q	114.9 (5)
N116—C716—C2o	113.00 (10)	C1p—C6q—H1c6q	123.39
Na14—Na15—Na16	74.50 (10)	C6p—C6q—H1c6p	78.66
Na14—Na15—O35w	92.86 (16)	C6p—C6q—C1q	97.3 (11)
Na14—Na15—O42w	47.25 (14)	C6p—C6q—C5q	41.1 (16)
Na14—Na15—O112	125.74 (18)	C6p—C6q—H1c6q	126.6
Na14—Na15—Na17	62.18 (13)	H1c6p—C6q—C1q	142.73
Na14—Na15—O43w	34.0 (2)	H1c6p—C6q—C5q	84.59
Na14—Na15—Hao35	76.5 (6)	H1c6p—C6q—H1c6q	48.05
Na14—Na15—Hbo35	115.3 (6)	C1q—C6q—C5q	116.7 (5)
Na14—Na15—Hao42	66.9 (10)	C1q—C6q—H1c6q	121.65
Na14—Na15—Hbo42	68.6 (9)	C5q—C6q—H1c6q	121.65
Na14—Na15—O3dib	56.2 (3)	C3p—H1c3q—H1c3p	68.72
Na16—Na15—O35w	41.84 (9)	C3p—H1c3q—C3q	30.36
Na16—Na15—O42w	102.8 (2)	H1c3p—H1c3q—C3q	99.02
Na16—Na15—O112	158.43 (18)	H1c4p—H1c4q—C4q	88.11
Na16—Na15—Na17	12.58 (10)	H1c6p—H1c6q—C6q	63.5

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O28w—Hao28···N116	0.871 (17)	2.128 (16)	2.9682 (14)	162.0 (15)
O28w—Hbo28···N18	0.850 (16)	2.164 (17)	2.9772 (14)	160.2 (15)
O24w—Hao24···O116	0.76 (2)	2.11 (2)	2.8492 (15)	165 (2)
O27w—Hao27···O17	0.85 (2)	1.99 (2)	2.8356 (15)	172.9 (18)
O17w—Hao17···O27	0.818 (19)	2.243 (18)	3.0412 (14)	165.4 (18)
O22w—Hao22···O212	0.812 (19)	2.129 (19)	2.9344 (15)	171.6 (19)
O18w—Hao18···N110	0.813 (17)	2.046 (16)	2.8464 (14)	167.8 (16)
O18w—Hbo18···N12	0.866 (16)	2.071 (17)	2.9085 (14)	162.5 (15)
O33w—Hao33···N13^vi	0.817 (17)	2.028 (17)	2.8143 (14)	161.5 (16)
O13w—Hao13···O37	0.868 (17)	1.998 (16)	2.8556 (12)	169.3 (15)
O21w—Hao21···O314	0.806 (17)	1.979 (17)	2.7738 (13)	168.3 (16)
O38w—Hao38···O34	0.81 (2)	2.021 (19)	2.7968 (15)	159 (2)
O39w—Hao38···O34	1.12 (2)	2.021 (19)	3.093 (8)	158.8 (17)
O23w—Hao23···O12	0.794 (18)	2.170 (17)	2.9453 (14)	165.3 (16)
O15w—Hao15···N18	0.848 (16)	2.157 (17)	2.9626 (14)	158.5 (15)
O15w—Hbo15···N116	0.798 (17)	2.261 (17)	3.0266 (14)	160.8 (16)
O12w—Hao12···O114	0.784 (19)	2.087 (19)	2.8678 (15)	174.5 (19)
O34w—Hao34···N114	0.880 (17)	1.991 (17)	2.8499 (14)	164.8 (16)
O32w—Hao32···O310	0.814 (17)	2.008 (17)	2.8209 (13)	176.6 (16)
O29w—Hao29···O19	0.775 (18)	2.097 (17)	2.8527 (14)	165.0 (16)
O29w—Hbo29···O215	0.882 (17)	1.962 (17)	2.8259 (13)	165.8 (15)
O25w—Hbo25···N111	0.802 (17)	2.063 (17)	2.8584 (14)	171.4 (17)
O25w—Hao25···O11w	0.865 (17)	2.476 (17)	3.2453 (14)	148.5 (15)
O25w—Hao25···O312	0.865 (17)	2.400 (17)	2.9748 (14)	124.4 (13)
O30w—Hao30···N19	0.899 (16)	2.032 (16)	2.9040 (14)	162.9 (15)
O16w—Hao16···O23^vi	0.716 (19)	2.236 (19)	2.9520 (14)	178 (2)
O20w—Hao20···N19	0.814 (16)	2.313 (17)	3.0538 (14)	151.6 (16)
O20w—Hbo20···N11	0.865 (17)	2.203 (17)	3.0443 (14)	164.3 (16)
O14w—Hbo14···N17	0.894 (17)	1.974 (16)	2.8486 (14)	165.7 (15)
O14w—Hao14···N115	0.843 (16)	2.223 (17)	3.0259 (14)	159.4 (15)
O11w—Hao11···N112	0.827 (17)	2.124 (17)	2.9513 (15)	177.9 (16)
O11w—Hbo11···N14	0.829 (17)	2.254 (17)	3.0769 (15)	172.0 (17)
O19w—Hao19···O19ⁱⁱⁱ	0.798 (19)	2.14 (2)	2.9220 (15)	169 (2)
O26w—Hao26···N115	0.880 (17)	2.011 (17)	2.8512 (14)	159.5 (15)
O26w—Hbo26···O111ⁱ	0.735 (18)	2.109 (17)	2.7996 (14)	156.6 (17)
O10w—Hbo10···O14	0.760 (18)	2.048 (18)	2.8030 (14)	171.8 (17)
O21w—Hbo21···O1dia	0.750 (18)	2.088 (18)	2.8315 (17)	171.2 (18)
O21w—Hbo21···O1dib	0.750 (18)	2.03 (2)	2.750 (9)	160.2 (17)
O30w—Hbo30···N11	0.817 (17)	2.101 (16)	2.9098 (14)	170.6 (16)
O17w—Hbo17···O15	0.860 (18)	2.036 (18)	2.8888 (15)	171.4 (17)
O33w—Hbo33···O32	0.816 (17)	1.994 (17)	2.8095 (13)	177.3 (17)
O10w—Hao10···O33	0.818 (17)	1.961 (17)	2.7687 (13)	169.2 (16)
O12w—Hbo12···O216	0.791 (19)	2.171 (19)	2.9534 (15)	170.4 (19)
O13w—Hbo13···O26	0.756 (17)	2.161 (17)	2.9029 (14)	167.3 (17)
O34w—Hbo34···N16	0.816 (17)	2.216 (18)	2.9696 (15)	153.7 (17)
O27w—Hbo27···O21	0.75 (2)	2.17 (2)	2.9233 (15)	176 (2)
O23w—Hbo23···O28	0.847 (18)	1.984 (17)	2.7820 (14)	156.7 (15)
O22w—Hbo22···O110^v	0.818 (19)	2.062 (19)	2.8686 (15)	168.7 (19)
O19w—Hbo19···O25	0.83 (2)	2.06 (2)	2.8524 (16)	159.7 (18)
O32w—Hbo32···N111^vi	0.803 (18)	2.203 (18)	2.9907 (14)	167.1 (17)
O35w—Hao35···Na15	0.825 (18)	1.986 (19)	2.171 (5)	91.5 (14)
O35w—Hao35···O3dia	0.825 (18)	1.988 (19)	2.8012 (16)	168.7 (19)
O35w—Hao35···O3dib	0.825 (18)	2.04 (2)	2.829 (11)	158.8 (19)
O38w—Hbo38···O35w	0.78 (2)	2.13 (2)	2.9038 (16)	167 (2)
O38w—Hbo38···Na19	0.78 (2)	2.23 (2)	2.384 (6)	91.5 (16)
O24w—Hbo24···O210	0.76 (2)	2.14 (2)	2.8949 (15)	176 (2)
O16w—Hbo16···O11	0.819 (19)	2.046 (19)	2.8537 (14)	168.7 (18)
O35w—Hbo35···N112	0.869 (19)	2.393 (19)	3.2035 (16)	155.4 (15)
O35w—Hbo35···Na15	0.869 (19)	1.803 (19)	2.171 (5)	103.0 (15)
O40w—Hbo40···O314	0.74 (2)	2.16 (2)	2.8876 (17)	168 (2)
O40w—Hao40···O36	0.78 (2)	1.97 (2)	2.7402 (17)	169 (2)
O41w—Hao40···O36	1.04 (2)	1.97 (2)	2.880 (9)	144 (2)
O42w—Hao42···O112	0.78 (2)	2.09 (2)	2.7999 (16)	151 (2)
Na15—Hao42···O43w	1.27 (2)	1.55 (2)	2.305 (10)	109.2 (15)
O42w—Hbo42···O28^iv	0.78 (2)	2.08 (2)	2.8538 (16)	169 (2)
C4d—H1c4d···O25^vii	0.96	2.37	3.2119 (13)	146.17
C6d—H1c6d···O116^iv	0.96	2.45	3.405 (2)	174.42
C4f—H1c4f···O23^vii	0.96	2.47	3.3845 (13)	160.12
C6h—H1c6h···O112ⁱⁱ	0.96	2.46	3.3511 (12)	154.21
C3p—H1c3p···O3dib	0.96	2.37	2.662 (10)	96.71
C3q—H1c3p···O3dib	1.32	2.37	3.078 (13)	109.70
C4p—H1c4p···O212^viii	0.96	2.41	3.3564 (15)	170.51
C4q—H1c4p···O212^viii	1.24	2.41	3.558 (6)	153.39

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

Sodium Saccharinate 1.875-Hydrate (II) top

Crystal data top

C₇H₄NNaO_4.875S	F(000) = 1904
M_r = 235.2	D_x = 1.661 Mg m⁻³
Monoclinic, C2/c(0β0)s0†	Ag Kα radiation, λ = 0.56089 Å
q = 0.750000b*	Cell parameters from 86894 reflections
a = 18.6212 (1) Å	θ = 2.8–29.8°
b = 7.11555 (5) Å	µ = 0.20 mm⁻¹
c = 29.1642 (2) Å	T = 95 K
β = 93.4511 (6)°	Prism, white translucent
V = 3857.25 (4) Å³	0.45 × 0.35 × 0.22 mm
Z = 16

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) −x₁, x₂+1/2, −x₃+1/2, x₄+1/2; (3) −x₁, −x₂, −x₃, −x₄; (4) x₁, −x₂+1/2, x₃+1/2, −x₄+1/2; (5) x₁+1/2, x₂+1/2, x₃, x₄; (6) −x₁+1/2, x₂, −x₃+1/2, x₄+1/2; (7) −x₁+1/2, −x₂+1/2, −x₃, −x₄; (8) x₁+1/2, −x₂, x₃+1/2, −x₄+1/2.

Data collection top

Mar dtb diffractometer	88532 independent reflections
Radiation source: X-ray tube	59317 reflections with I > 3σ(I)
Equatorial mounted graphite monochromator	R_int = 0.086
φ scans	θ_max = 29.9°, θ_min = 2.8°
Absorption correction: empirical (using intensity measurements) CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −32→32
T_min = 0.912, T_max = 1	k = −15→14
651280 measured reflections	l = −51→51

Refinement top

Refinement on F	146 constraints
R[F² > 2σ(F²)] = 0.054	H-atom parameters constrained
wR(F²) = 0.065	Weighting scheme based on measured s.u.'s w = 1/(σ²(F) + 0.0001F²)
S = 1.87	(Δ/σ)_max = 0.006
88532 reflections	Δρ_max = 0.48 e Å⁻³
1734 parameters	Δρ_min = −0.21 e Å⁻³
0 restraints

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
S1a	−0.051378 (6)	0.774301 (19)	0.412309 (4)	0.01458 (3)
O1a	−0.09281 (2)	0.94098 (6)	0.421285 (15)	0.02064 (11)
O2a	−0.08111 (2)	0.60253 (6)	0.429721 (14)	0.02027 (11)
O3a	0.05950 (2)	0.75096 (6)	0.313632 (14)	0.01925 (11)
N1a	−0.03675 (2)	0.75623 (7)	0.358753 (16)	0.01640 (11)
C7a	0.03458 (3)	0.76565 (7)	0.351979 (18)	0.01482 (12)
S1b	−0.220778 (9)	0.77689 (3)	0.172867 (7)	0.01537 (4)	0.875
S1b'	−0.20444 (3)	0.68935 (6)	0.174131 (15)	0.01307 (9)	0.11045 (10)
S1b''	−0.1799 (2)	0.6783 (5)	0.17754 (13)	0.01307 (9)	0.01455 (10)
O1b	−0.26345 (3)	0.61265 (8)	0.17443 (2)	0.02211 (16)	0.875
O1b'	−0.22205 (16)	0.4934 (4)	0.17836 (10)	0.0156 (5)	0.11045 (10)
O1b''	−0.2143 (5)	0.8168 (13)	0.2082 (3)	0.0156 (5)	0.01455 (10)
O2b	−0.25533 (3)	0.94392 (8)	0.18655 (2)	0.02233 (16)	0.875
O2b'	−0.25410 (7)	0.81336 (19)	0.19572 (5)	0.0227 (4)	0.11045 (10)
O2b''	−0.2151 (17)	0.477 (4)	0.1743 (11)	0.0227 (4)	0.01455 (10)
O3b	−0.02813 (3)	0.74498 (8)	0.18734 (2)	0.01982 (15)	0.875
O3b'	−0.01547 (6)	0.8124 (2)	0.16341 (5)	0.0241 (4)	0.11045 (10)
O3b''	−0.0021 (5)	0.7148 (16)	0.1345 (4)	0.0241 (4)	0.01455 (10)
N1b	−0.14630 (3)	0.74976 (10)	0.20180 (2)	0.01764 (16)	0.875
N1b'	−0.12252 (8)	0.7257 (2)	0.19314 (5)	0.0182 (4)	0.11045 (10)
N1b''	−0.0968 (6)	0.6675 (17)	0.1802 (4)	0.0182 (4)	0.01455 (10)
C7b	−0.09133 (4)	0.76035 (10)	0.17387 (3)	0.01533 (17)	0.875
C7b'	−0.08162 (8)	0.7802 (2)	0.15869 (6)	0.0159 (4)	0.11045 (10)
C7b''	−0.0675 (6)	0.7180 (19)	0.1400 (5)	0.0159 (4)	0.01455 (10)
O28w	0.09339 (2)	0.51822 (6)	0.221566 (15)	0.02104 (15)	0.875
O28w'	0.09339 (2)	0.51822 (6)	0.221566 (15)	0.0290 (4)	0.11045 (10)
O28w''	0.0903 (6)	0.5460 (17)	0.2184 (4)	0.025 (2)*	0.01455 (10)
O18w	−0.09530 (2)	0.49866 (6)	0.278892 (14)	0.0183 (8)	0.75
O18w'	−0.09530 (2)	0.49866 (6)	0.278892 (14)	0.0182 (2)	0.2209 (2)
O18w''	−0.0988 (6)	0.4812 (17)	0.2782 (5)	0.026 (2)	0.0291 (2)
O24w	0.15022 (3)	0.78020 (7)	0.122161 (17)	0.02629 (18)	0.875
O24w'	0.15022 (3)	0.78020 (7)	0.122161 (17)	0.0236 (4)	0.11045 (10)
O24w''	0.1474 (5)	0.8363 (15)	0.1213 (4)	0.023 (2)*	0.01455 (10)
O23w	0.23860 (7)	0.8068 (2)	0.27618 (5)	0.0174 (3)	0.75
Na6	0.19724 (4)	0.81167 (10)	0.19827 (3)	0.01728 (18)	0.75
Na2	0.00275 (8)	0.7026 (2)	0.25644 (6)	0.0236 (4)	0.625
Na2'	−0.10396 (4)	0.76082 (10)	0.28157 (3)	0.01800 (19)	0.11045 (10)
Na2''	−0.0358 (3)	0.7665 (11)	0.2537 (2)	0.030 (2)	0.01455 (10)
Na16'	0.13582 (4)	0.68727 (13)	0.26322 (3)	0.0218 (2)	0.11045 (10)
Na16''	0.1414 (3)	0.8248 (11)	0.2697 (2)	0.028 (2)	0.01455 (10)
Na16	0.15301 (3)	0.76094 (9)	0.27748 (2)	0.01699 (16)	0.125
Na14'	0.09263 (3)	0.97995 (10)	0.15045 (2)	0.01633 (18)	0.11045 (10)
Na14''	0.1085 (3)	0.5571 (8)	0.14943 (19)	0.0163 (14)	0.01455 (10)
Na14	0.08910 (3)	0.54926 (9)	0.15799 (2)	0.01582 (16)	0.125
C1a	0.038545 (17)	0.80383 (3)	0.432924 (13)	0.0146 (6)
C2a	0.08073 (2)	0.79595 (3)	0.395629 (18)	0.0145 (6)
C3a	0.15420 (3)	0.81753 (3)	0.40100 (2)	0.0174 (6)
C4a	0.18437 (3)	0.84743 (3)	0.44511 (2)	0.0202 (6)
C5a	0.14191 (3)	0.85537 (3)	0.48268 (2)	0.0204 (6)
C6a	0.06753 (3)	0.83349 (3)	0.47718 (2)	0.0178 (7)
H1c3a	0.183631	0.812103	0.375114	0.0229 (13)
H1c4a	0.235503	0.862899	0.449754	0.0277 (11)
H1c5a	0.16413	0.876204	0.512811	0.0280 (12)
H1c6a	0.037736	0.838739	0.502892	0.0235 (14)
C1b	−0.18765 (3)	0.8071 (2)	0.118756 (15)	0.0149 (8)	0.875
C2b	−0.11370 (4)	0.79418 (19)	0.124733 (15)	0.0145 (8)	0.875
C3b	−0.07090 (4)	0.8153 (4)	0.08822 (3)	0.0178 (8)	0.875
C4b	−0.10457 (4)	0.84994 (19)	0.04526 (2)	0.0207 (8)	0.875
C5b	−0.17904 (4)	0.8629 (2)	0.03922 (2)	0.0213 (8)	0.875
C6b	−0.22229 (4)	0.8415 (4)	0.07623 (3)	0.0190 (8)	0.875
H1c3b	−0.019473	0.806386	0.092301	0.0271 (17)	0.875
H1c4b	−0.075889	0.865193	0.019243	0.0318 (15)	0.875
H1c5b	−0.200952	0.886982	0.009156	0.0328 (15)	0.875
H1c6b	−0.27375	0.850233	0.072429	0.0291 (18)	0.875
C1c	−0.19477 (6)	0.7565 (3)	0.11664 (3)	0.0129 (15)	0.11045 (10)
C2c	−0.12290 (7)	0.7978 (3)	0.11296 (3)	0.0127 (15)	0.11045 (10)
C3c	−0.09788 (7)	0.8585 (6)	0.07205 (4)	0.0163 (16)	0.11045 (10)
C4c	−0.14727 (7)	0.8767 (3)	0.03470 (3)	0.0204 (15)	0.11045 (10)
C5c	−0.21965 (7)	0.8351 (3)	0.03839 (3)	0.0226 (15)	0.11045 (10)
C6c	−0.24489 (7)	0.7737 (6)	0.07984 (4)	0.0187 (16)	0.11045 (10)
H1c3c	−0.047928	0.887316	0.069414	0.019 (3)	0.11045 (10)
H1c4c	−0.131139	0.918823	0.005781	0.024 (3)	0.11045 (10)
H1c5c	−0.252669	0.848932	0.012034	0.029 (3)	0.11045 (10)
H1c6c	−0.294756	0.744628	0.082744	0.023 (3)	0.11045 (10)
C1d	−0.1910 (4)	0.775 (2)	0.11637 (18)	0.0129 (15)	0.01455 (10)
C2d	−0.1234 (4)	0.797 (2)	0.10003 (18)	0.0127 (15)	0.01455 (10)
C3d	−0.11505 (18)	0.857 (4)	0.0558 (3)	0.0163 (16)	0.01455 (10)
C4d	−0.1768 (4)	0.895 (2)	0.02828 (18)	0.0204 (15)	0.01455 (10)
C5d	−0.2448 (4)	0.874 (2)	0.04473 (19)	0.0226 (15)	0.01455 (10)
C6d	−0.25321 (19)	0.813 (4)	0.0895 (3)	0.0187 (16)	0.01455 (10)
H1c3d	−0.068102	0.871616	0.044385	0.019 (3)	0.01455 (10)
H1c4d	−0.172318	0.937386	−0.002687	0.024 (3)	0.01455 (10)
H1c5d	−0.286598	0.901459	0.024978	0.029 (3)	0.01455 (10)
H1c6d	−0.299964	0.797807	0.101186	0.023 (3)	0.01455 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
S1a	0.01061 (5)	0.01849 (6)	0.01494 (5)	−0.00004 (4)	0.00325 (4)	−0.00099 (4)
O1a	0.01580 (16)	0.0241 (2)	0.02232 (19)	0.00621 (14)	0.00358 (14)	−0.00237 (15)
O2a	0.01884 (17)	0.02258 (19)	0.01997 (18)	−0.00584 (14)	0.00603 (14)	0.00013 (15)
O3a	0.01588 (17)	0.0268 (2)	0.01559 (17)	−0.00143 (14)	0.00564 (13)	−0.00074 (15)
N1a	0.01068 (16)	0.0230 (2)	0.01574 (18)	−0.00058 (15)	0.00278 (13)	−0.00094 (16)
C7a	0.01220 (19)	0.0169 (2)	0.0157 (2)	−0.00025 (15)	0.00344 (15)	0.00023 (16)
S1b	0.01124 (7)	0.01644 (8)	0.01893 (8)	0.00076 (6)	0.00507 (6)	0.00065 (6)
S1b'	0.01004 (17)	0.01422 (16)	0.01544 (16)	−0.00105 (15)	0.00474 (15)	−0.00016 (12)
S1b''	0.01004 (17)	0.01422 (16)	0.01544 (16)	−0.00105 (15)	0.00474 (15)	−0.00016 (12)
O1b	0.0161 (2)	0.0206 (3)	0.0303 (3)	−0.0042 (2)	0.0073 (2)	0.0029 (2)
O1b'	0.0151 (9)	0.0132 (8)	0.0193 (8)	−0.0012 (5)	0.0070 (5)	0.0004 (6)
O1b''	0.0151 (9)	0.0132 (8)	0.0193 (8)	−0.0012 (5)	0.0070 (5)	0.0004 (6)
O2b	0.0194 (3)	0.0216 (3)	0.0267 (3)	0.0056 (2)	0.0078 (2)	−0.0025 (2)
O2b'	0.0231 (6)	0.0190 (6)	0.0277 (7)	0.0003 (5)	0.0153 (5)	−0.0025 (5)
O2b''	0.0231 (6)	0.0190 (6)	0.0277 (7)	0.0003 (5)	0.0153 (5)	−0.0025 (5)
O3b	0.0113 (2)	0.0241 (3)	0.0238 (3)	0.00150 (19)	−0.00094 (19)	0.0003 (2)
O3b'	0.0099 (5)	0.0286 (7)	0.0332 (7)	−0.0057 (5)	−0.0041 (5)	0.0087 (6)
O3b''	0.0099 (5)	0.0286 (7)	0.0332 (7)	−0.0057 (5)	−0.0041 (5)	0.0087 (6)
N1b	0.0142 (3)	0.0214 (3)	0.0176 (3)	0.0009 (2)	0.0034 (2)	0.0015 (2)
N1b'	0.0155 (6)	0.0230 (7)	0.0161 (6)	−0.0059 (5)	0.0002 (5)	0.0031 (5)
N1b''	0.0155 (6)	0.0230 (7)	0.0161 (6)	−0.0059 (5)	0.0002 (5)	0.0031 (5)
C7b	0.0119 (3)	0.0158 (3)	0.0184 (3)	0.0005 (2)	0.0018 (2)	−0.0003 (2)
C7b'	0.0103 (6)	0.0182 (7)	0.0190 (7)	−0.0025 (5)	−0.0005 (5)	0.0037 (6)
C7b''	0.0103 (6)	0.0182 (7)	0.0190 (7)	−0.0025 (5)	−0.0005 (5)	0.0037 (6)
O28w	0.0165 (2)	0.0207 (3)	0.0263 (3)	0.0002 (2)	0.0037 (2)	0.0006 (2)
O28w'	0.0371 (8)	0.0239 (7)	0.0248 (7)	0.0114 (6)	−0.0088 (6)	−0.0067 (6)
O18w	0.0175 (12)	0.0182 (14)	0.0198 (14)	−0.0026 (10)	0.0051 (10)	−0.0001 (11)
O18w'	0.0146 (4)	0.0210 (4)	0.0193 (4)	0.0014 (3)	0.0026 (3)	0.0010 (3)
O18w''	0.019 (3)	0.017 (3)	0.039 (5)	−0.002 (3)	−0.014 (3)	−0.002 (3)
O24w	0.0278 (3)	0.0224 (3)	0.0278 (3)	−0.0008 (2)	−0.0051 (2)	0.0014 (2)
O24w'	0.0223 (6)	0.0227 (7)	0.0257 (7)	0.0019 (5)	0.0009 (5)	−0.0018 (5)
O23w	0.0144 (5)	0.0198 (6)	0.0185 (6)	−0.0004 (5)	0.0043 (4)	−0.0012 (5)
Na6	0.0132 (3)	0.0197 (3)	0.0192 (3)	0.0022 (2)	0.0026 (2)	−0.0012 (3)
Na2	0.0127 (7)	0.0274 (8)	0.0307 (8)	−0.0013 (6)	0.0004 (6)	0.0095 (6)
Na2'	0.0185 (3)	0.0184 (3)	0.0169 (3)	−0.0011 (3)	−0.0001 (2)	0.0001 (3)
Na2''	0.019 (3)	0.050 (4)	0.021 (3)	−0.014 (3)	0.003 (2)	−0.010 (3)
Na16'	0.0124 (3)	0.0340 (5)	0.0194 (4)	0.0020 (3)	0.0043 (3)	0.0063 (3)
Na16''	0.019 (3)	0.042 (4)	0.024 (3)	−0.002 (3)	0.006 (2)	0.007 (3)
Na16	0.0108 (2)	0.0214 (3)	0.0191 (3)	−0.0012 (2)	0.0037 (2)	0.0008 (2)
Na14'	0.0121 (3)	0.0190 (3)	0.0179 (3)	−0.0009 (2)	0.0013 (2)	0.0017 (3)
Na14''	0.010 (2)	0.018 (2)	0.020 (3)	0.0022 (17)	−0.0014 (17)	0.000 (2)
Na14	0.0107 (2)	0.0188 (3)	0.0181 (3)	0.0019 (2)	0.0018 (2)	−0.0005 (2)
C1a	0.01275 (16)	0.0155 (17)	0.01581 (18)	0.0003 (3)	0.00252 (13)	−0.0006 (3)
C2a	0.01156 (16)	0.0153 (17)	0.01677 (18)	−0.0001 (3)	0.00278 (13)	0.0001 (3)
C3a	0.01158 (19)	0.0192 (19)	0.02163 (15)	−0.0004 (4)	0.00262 (14)	−0.0001 (4)
C4a	0.01319 (16)	0.0224 (17)	0.02478 (18)	0.0001 (3)	−0.00099 (12)	−0.0023 (3)
C5a	0.01720 (16)	0.0229 (17)	0.02070 (18)	0.0017 (3)	−0.00236 (13)	−0.0033 (3)
C6a	0.01687 (19)	0.0200 (19)	0.01652 (16)	0.0016 (4)	0.00101 (14)	−0.0019 (4)
H1c3a	0.0122 (4)	0.032 (4)	0.0248 (3)	−0.0015 (8)	0.0050 (3)	−0.0005 (8)
H1c4a	0.0135 (3)	0.037 (3)	0.0317 (4)	−0.0013 (6)	−0.0023 (2)	−0.0047 (7)
H1c5a	0.0219 (3)	0.038 (3)	0.0230 (4)	0.0021 (6)	−0.0053 (2)	−0.0067 (7)
H1c6a	0.0211 (4)	0.033 (4)	0.0162 (3)	0.0018 (8)	0.0023 (3)	−0.0035 (8)
C1b	0.0116 (2)	0.015 (2)	0.01814 (16)	0.0001 (3)	0.00241 (14)	0.0002 (4)
C2b	0.0116 (2)	0.015 (2)	0.01701 (16)	0.0000 (3)	0.00269 (14)	−0.0001 (4)
C3b	0.01430 (15)	0.020 (2)	0.0200 (3)	−0.0004 (2)	0.00578 (12)	−0.0006 (4)
C4b	0.0232 (2)	0.022 (2)	0.01758 (16)	−0.0006 (3)	0.00647 (14)	−0.0002 (4)
C5b	0.0243 (2)	0.022 (2)	0.01706 (17)	0.0005 (3)	−0.00023 (14)	0.0003 (4)
C6b	0.01537 (15)	0.021 (2)	0.0207 (3)	0.0007 (2)	−0.00128 (12)	0.0003 (4)
H1c3b	0.01404 (15)	0.041 (5)	0.0275 (6)	0.0004 (4)	0.00786 (17)	0.0017 (9)
H1c4b	0.0324 (4)	0.044 (4)	0.0206 (2)	−0.0003 (6)	0.0116 (3)	0.0027 (7)
H1c5b	0.0347 (4)	0.044 (4)	0.0187 (3)	0.0022 (6)	−0.0034 (3)	0.0037 (7)
H1c6b	0.01579 (15)	0.042 (5)	0.0287 (6)	0.0024 (4)	−0.00397 (17)	0.0032 (9)
C1c	0.0086 (6)	0.013 (4)	0.0171 (5)	−0.0006 (10)	0.0027 (4)	0.0010 (10)
C2c	0.0088 (6)	0.016 (4)	0.0140 (5)	−0.0002 (10)	0.0039 (4)	0.0032 (10)
C3c	0.0167 (4)	0.019 (5)	0.0142 (7)	−0.0007 (10)	0.0071 (4)	0.0018 (12)
C4c	0.0302 (6)	0.018 (4)	0.0129 (5)	−0.0019 (10)	0.0022 (4)	0.0012 (10)
C5c	0.0268 (6)	0.020 (4)	0.0199 (5)	−0.0006 (10)	−0.0073 (4)	0.0024 (10)
C6c	0.0130 (4)	0.018 (5)	0.0246 (7)	0.0002 (10)	−0.0036 (4)	0.0007 (12)
H1c3c	0.0183 (5)	0.020 (10)	0.0189 (15)	−0.001 (2)	0.0125 (6)	0.000 (2)
H1c4c	0.0467 (12)	0.015 (8)	0.0117 (7)	−0.005 (2)	0.0048 (7)	−0.001 (2)
H1c5c	0.0392 (12)	0.021 (9)	0.0258 (8)	−0.001 (2)	−0.0159 (7)	0.003 (2)
H1c6c	0.0120 (6)	0.018 (10)	0.0364 (15)	0.000 (2)	−0.0055 (6)	−0.002 (3)
C1d	0.0104 (5)	0.013 (4)	0.0156 (6)	0.0000 (6)	0.0048 (3)	0.0006 (13)
C2d	0.0112 (5)	0.015 (4)	0.0121 (6)	0.0012 (6)	0.0051 (3)	0.0027 (13)
C3d	0.0197 (4)	0.019 (5)	0.0110 (7)	−0.0003 (5)	0.0057 (3)	0.0015 (14)
C4d	0.0285 (5)	0.019 (4)	0.0135 (6)	−0.0026 (6)	−0.0024 (3)	0.0022 (13)
C5d	0.0216 (5)	0.020 (4)	0.0252 (6)	0.0000 (6)	−0.0074 (3)	0.0035 (13)
C6d	0.0118 (4)	0.018 (5)	0.0265 (7)	0.0011 (5)	0.0004 (3)	0.0006 (14)
H1c3d	0.0239 (5)	0.020 (10)	0.0127 (15)	−0.0020 (8)	0.0108 (6)	−0.001 (3)
H1c4d	0.0434 (10)	0.017 (9)	0.0122 (10)	−0.0081 (12)	−0.0052 (6)	0.001 (2)
H1c5d	0.0282 (10)	0.021 (9)	0.0365 (10)	−0.0014 (12)	−0.0163 (7)	0.005 (3)
H1c6d	0.0107 (5)	0.018 (10)	0.0386 (15)	0.0004 (9)	0.0019 (6)	−0.002 (3)

Acknowledgements

We thank Professor Carolyn Brock for bringing this system to our attention. We acknowledge the Faculty of Chemistry, University of Latvia, for providing access to the GAUSSIAN09 software. Open access funding enabled and organized by Projekt DEAL.

Funding information

Funding for this research was provided by the Deutsche Forschungsgemeinschaft (DFG; German Research Foundation) – 389490692.

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