A new polymorph of white phospho­rus at ambient conditions

Dedicated to Professor George Sheldrick on the occasion of his 80th birthday.

Phospho­rus exists in several different allotropes: white, red, violet and black. For industrial and academic applications, white phospho­rus is the most important. So far, three polymorphs of white phospho­rus, all consisting of P₄ tetrahedra, have been described. Among these, β-P₄ crystallizes in the space group P1 and γ-P₄ in the space group C2/m. α-P₄ forms soft plastic crystals with a proposed structure in the cubic space group I43m with the lattice constant a = 18.51 (3) Å, consisting of 58 rotationally disordered tetrahedra and thus is similar to the structure of α-Mn. Here we present a new polymorph, δ-P₄. It crystallizes as a sixfold twin with the cell dimensions a = 18.302 (2), b = 18.302 (2), c = 36.441 (3) Å in the space group P2₁2₁2₁ with 29 P₄ tetrahedra in the asymmetric unit. The arrangement resembles the structure of α-Mn, but δ-P₄ differs from α-P₄. DFT calculations show δ-P₄ to be metastable at a similar energy level to that of γ-P₄.

1. Introduction

Phospho­rus exists in several different modifications: white, red, violet and black (Fig. 1). Its affinity for oxygen is high, so it exists in nature mainly as phosphates, containing the PO₄^3– anion. This is difficult to activate chemically in contrast to white phospho­rus P₄, which spontaneously ignites when exposed to air. This makes the element a versatile reagent in organo­phospho­rus chemistry (Iaroshenko, 2019; Donath et al., 2022; Grützmacher, 2022).

Figure 1 Known modifications of elemental phospho­rus under ambient conditions: their macroscopic manifestations combined with the structures at the atomic level.

The different modifications of phospho­rus vary markedly in their physical properties and chemical reactivity. The most stable modification at room temperature is polymeric black phospho­rus P_n. This polymorph has semiconducting properties. It displays a layered structure consisting of anellated chair-shaped six-membered rings (Fig. 1, left). At ambient pressure it crystallizes in the space group Cmca with a = 3.31, b = 10.50 and c = 4.38 Å (Hultgren et al., 1935; Brown & Rundqvist, 1965). Under increasing pressure, it undergoes several phase transitions (Jamieson, 1963; Kikegawa & Iwasaki, 1983; Kikegawa et al., 1987; Scelta et al., 2017; Marqués et al., 2008; Akahama et al., 1999; Sugimoto et al., 2012); for example, at room temperature the first phase transition at ∼5 GPa leads to the space group R3m with a = 3.38 and c = 8.81 Å. Fibrous red phospho­rus crystallizes in the space group P1 with a = 12.198, b = 12.986, c = 7.075 Å, and α = 116.99, β = 106.31, γ = 97.91° (Fig. 1, right) (Ruck et al., 2005). It consists of tubes with pentagonal cross-sections. The tubes are built from cages of eight or nine phospho­rus atoms connected by dumbbells of two phospho­rus atoms, and interconnect to form a double tube. This is similar to the structure of violet or Hittorf's phospho­rus, which crystallizes in the space group P2/c with a = 9.21, b = 9.15, c = 22.60 Å and β = 106.1° (Fig. 1, bottom) (Thurn & Krebs, 1969; Zhang et al., 2020). Zhang et al. (2020) stated that their structure differs slightly from the structure described by Thurn & Krebs (1969) and discussed the differences [e.g. different space groups (P2/n and P2/c), c axes and ß angles]; however, both structures can be transformed into each other by the matrix −100 0−10 101, hence there is no difference between them but they are identical.

Recently, another structure has been described (Cicirello et al., 2023) in the space group C2/c with eleven phospho­rus atoms in the asymmetric unit.¹ The red and violet P_n structures differ only in the orientation of the two tubes relative to each other: they are perpendicular to each other in the violet modification and parallel in the red polymorph. Although white phospho­rus is the most toxic and reactive modification, it is a major source for industrial and academic applications (Donath et al., 2022). To date, three modifications of white phospho­rus have been described in the literature (Simon et al., 1997). Though the structures for β-P₄ (Simon et al., 1987) and γ-P₄ (Okudera et al., 2005) are unequivocal, no structural data are available for α-P₄. γ-P₄ is the stable low-temperature form and crystallizes in the space group C2/m with a = 9.1709 (5), b = 8.3385 (5), c = 5.4336 (2) Å and β = 90.311 (3)° with four formula units per cell (Z = 4) (Okudera et al., 2005). It transforms into the intermediate modification β-P₄, which crystallizes in the space group P1 with a = 5.4788 (5), b = 10.7862 (11), c = 10.9616 (11) Å, α = 94.285 (8), β = 99.653 (7), γ = 100.680 (7)° and Z = 6 (Simon et al., 1987). The room-temperature form α-P₄ has been described as a plastic crystal (Simon et al., 1997). As early as 1930, a powder photograph taken at −35°C was interpreted in terms of a cubic cell with a = 7.17 Å (Natta & Passerini, 1930). However, this key structure – `a riddle, wrapped in a mystery, inside an enigma' – remained unsolved. In 1952 single-crystal data were collected in the cubic system with a = 18.51 (3) Å, assuming the space group I43m, but the structure was never solved, which was attributed to rotational disorder (Corbridge & Lowe, 1952). As the most reasonable approximation, it was assumed that the centroids of the P₄ tetrahedra are arranged similar to the atomic positions of the 58 Mn atoms in the complicated structure of α-Mn (von Schnering, 1981). The most recent verdict is that crystallographic investigations are hampered by a partial transition to red phospho­rus or that a high degree of thermal motion precludes a structure determination (Simon et al., 1997).

2. Experimental

In the course of a synthesis involving the activation of white phospho­rus, we discovered a new polymorph of phospho­rus P₄, which we introduce in this publication as δ-P₄. Diffraction data were collected from an apparently cubic crystal with a = 36 Å at 100 K. We assumed at first that the data corresponded to the proposed reaction product, not the starting material. The diffraction pattern indicated twinning. Fig. 2(a) shows every second reflection to be missing in every second line. This can be interpreted as a threefold twin, and all reflections can be indexed with three different orientations and cell constants of approximately a = 18.3, b = 18.3, c = 36.5 Å and α = β = γ = 90° [Figs. 2(b)–2(d)]. These cell constants suggest a tetragonal space group. However, the data derived by integration with these three orientation matrices, with subsequent detwinning assuming 4/m symmetry, showed only orthorhombic symmetry and hinted at additional twinning that mimicks tetragonal symmetry. This means that there are six twin domains, because each of the three domains has an additional domain, generated by reducing the crystallographic fourfold symmetry to twofold symmetry.

Figure 2 Plot of the Bragg reflections used for indexing (Bruker, 2016). (a) All reflections, (b) first, (c) second and (d) third domain. The light pale rectangles indicate the corresponding cell.

Consequently, the integration was repeated, now using six orientation matrices. The matrices of the twin laws are given in the supporting information. After detwinning, the space group could be determined unequivocally to be P2₁2₁2₁. The structure could be solved in this space group (Sheldrick, 2008) and refined as a sixfold twin without any disorder (Sheldrick, 2015b; Sevvana et al., 2019). The refinement converged to R1 [I > 2σ(I)] = 0.0363. More details can be found in the supporting information.

With these results in hand, we attempted to find suitable crystallization conditions for this new polymorph. The first trials using CS₂ as the solvent led to soft plastic crystals, as already described in the literature as α-P₄. They diffracted weakly to a resolution of ca 1.6 Å. The cell constants suggested cubic symmetry with a = 18.7 Å and the structure could not be solved. Crystallization from dry, degassed hexane gave colourless block-shaped single crystals (see Fig. 3) which were identified as the δ-polymorph we had just investigated. The crystals were again twinned, and of the same quality as before, leading to the same ordered structure with similar quality indicators (see Table S1 of the supporting information).

Figure 3 Crystals of the new polymorph.

3. Results

In the literature, the α-P₄ polymorph is described as a cubic structure with a = 18.51 (3) Å in the most probable space group I43m. The similarity to α-Mn was mentioned (von Schnering, 1981). In our δ-P₄ structure, one axis is doubled and the others are slightly shorter compared with these observations. However, the arrangement of the P₄ tetrahedra indeed resembles the structure of α-Mn, which crystallizes in space group I43m (see Fig. 4) (Oberteuffer & Ibers, 1970). The cubic symmetry forces the packing to be identical along all three axes (Fig. 4, left), whereas they are very similar in the new orthorhombic δ-P₄ modification (Fig. 4, right). This can be visualized using the centroids of the δ-P₄ tetrahedra (Fig. 4, centre).

Figure 4 Packing of α-Mn compared with δ-P4: left: α-Mn along the a axis, which is identical to the b and c axes caused by the cubic symmetry. Centre: centroids of the P4 tetrahedra along the a axis (top), b axis (middle) and c axis (bottom). Right: full tetrahedra of the new δ-P4 polymorph along the a axis (top), b axis (middle) and c axis (bottom).

The asymmetric unit consists of 29 P₄ tetrahedra. A Z′ value as high as 29 might lead one to think of modulation. However, the typical signs of modulation (strong central reflections with weaker satellites) were absent from the diffraction pattern. Additionally, we note the similarity to the non-modulated structure of α-Mn with similar environments of the Mn atoms and the P₄ tetrahedra. In α-Mn there are four independent Mn atoms with different crystallographic symmetry and environments (Types I–IV) corresponding to 58 atoms in the unit cell. Two belong to Type I [Fig. 5(a)], eight to Type II [Fig. 5(b)], 24 to Type III [Fig. 5(c)] and 24 to Type IV [Fig. 5(d)]. Similar environments can be observed for the P₄ units of the δ-P₄ structure: thus there is one tetrahedron of Type I [Fig. 5(e)], four of Type II [Fig. 5(f)], 12 of Type III [Fig. 5(g)] and 12 of Type IV [Fig. 5(h)], exactly half as many of each type as for α-Mn, coordinated in the same way as in α-Mn (see Figs. 5 and 6 and the supporting information). Therefore, our new δ-P₄ polymorph indeed resembles α-Mn, as commented by von Schnering (1981), but it is definitely different from the α-P₄ form discussed in previous publications (Simon et al., 1997, 1987; Corbridge & Lowe, 1952).

Figure 5 (a)–(d) Comparison of the α-Mn polyhedra (Momma & Izumi, 2011) and (e)–(h) the environment types of the new δ-P4 modification. (a) α-Mn Type I, (b) α-Mn Type II, (c) α-Mn Type III and (d) α-Mn Type IV, (e) δ-P4 Type I, (f) δ-P4 Type II, (g) δ-P4 Type III and (h) δ-P4 Type IV.

Figure 6 Polyhedra of the four environment types: (a) truncated tetrahedron, (b) truncated tetrahedron with the hexagonal planes capped by P4 tetrahedra, (c) all P4 tetrahedra of Type I, (d) all tetrahedra of Type II, (e) hexagonal antiprism with one edge missing of Type III and the hexagonal planes capped by P4 tetrahedra, (f) all P4 tetrahedra of Type III, (g) icosahedron, (h) icosahedron of Type IV with all P4 tetrahedra (Momma & Izumi, 2011).

The P₄ tetrahedra of Types I [Fig. 6(c)] and II [Fig. 6(d)] are surrounded by 16 further tetrahedra, and the resulting global polyhedron can be described as a distorted and truncated tetrahedron [Fig. 6(a)] with 4 tetrahedra above the sixfold planes [Fig. 6(b)]. The distortion is higher for Type II. The tetrahedra of Type IV [Fig. 6(h)] are coordinated by 12 further tetrahedra, leading to a distorted icosahedron [Fig. 6(g)], whereas the polyhedron of the Type III tetrahedra [Fig. 6(f)], with coordination number 13, can be described as a hexagonal antiprism with one corner missing and capped by two tetrahedra above and below [Fig. 6(e)].

Our new polymorph δ-P₄ and the old α-P₄ are correlated in the following way: in both the P₄-tetrahedra probably show an overall structural pattern reminiscent of α-Mn, provided that only the centroids of the tetrahedra are taken into account. Compared with α-P₄, in the new δ-P₄ polymorph all 29 tetrahedra in the asymmetric unit are ordered (rather than disordered), one cell axis is doubled, the cell is primitive and not I-centred, and the symmetry is reduced from cubic to orthorhombic. None of the tetrahedra are related by translational or rotational symmetry. In α-Mn and presumably also in α-P₄ there are only 29/24 atoms or tetrahedra, respectively, in the asymmetric unit. Therefore, severe rotational P₄-disorder is introduced, permitting only low-resolution diffraction data for α-P₄. The reduction of symmetry in δ-P₄ is accompanied by twinning. A further distinction can be found in the densities, with a value of 1.96 g cm^–3 for δ-P₄ at 100 K but only 1.83 g cm⁻³ at 100 K in α-P₄, based on the data we collected from the soft plastic crystals (see above), assuming 58 tetrahedra in a unit cell.

With the new δ-P₄ polymorph stable at ambient conditions, its energetic relationships to the other known polymorphs remained to be determined. Accordingly, the relative stabilities of the different polymorphs of phospho­rus have been computed by density-functional theory (DFT) methods, employing the generalized gradient approximation of Perdew, Burke and Ernzerhof (PBE) (Perdew et al., 1996, 1997). Since dispersion corrections are known to be important for elemental phospho­rus (Aykol et al., 2017), not only uncorrected PBE calculations but also D3 and D3/BJ dispersion corrections, as developed by Grimme and coworkers, have been performed (Grimme, 2006; Grimme et al., 2010, 2011).

Taking black phospho­rus as the reference, the relative binding energies (Table S2) show that the correct order of stability can only be achieved by including dispersion corrections, in agreement with previous work (Aykol et al., 2017). Further, the energetic ordering of γ-P₄ and δ-P₄ changes from PBE to PBE-D3, but the absolute value of the energy difference is very small. Becke–Johnson (BJ) damping increases the energy difference significantly. Consistent with previous theoretical studies (Aykol et al., 2017; Bachhuber et al., 2014) on a number of the polymorphs, the D3 and D3/BJ values show that the individual P₄ moieties are held together by van der Waals forces, resulting in metastable γ-P₄ and δ-P₄ polymorphs.

4. Conclusions

We have determined the crystal structure of a new polymorph of white phospho­rus which resembles the structure of α-Mn. This similarity has already been described for α-P₄ (von Schnering, 1981). However, many other aspects of α-P₄ do not apply to our crystals of the new δ-P₄ polymorph. While the former crystallizes from CS₂, the latter crystallizes from dry, degassed hexane. The structure refinement of cubic α-P₄ is precluded by rotational disorder, but the orthorhombic δ-P₄ polymorph was refined without disorder despite serious twinning. Additionally, the two forms differ in their densities. From DFT calculations it can be concluded that γ-P₄ and δ-P₄ are metastable and that the twinning of δ-P₄ is energetically favourable. The description of the new polymorph significantly extends our knowledge of phospho­rus.

5. Related literature

The following references are cited in the supporting information: Belsky et al. (2002); Bruker (2021a,b); Herbst-Irmer (2016); Kottke & Stalke (1993); Kresse & Furthmüller (1996); Kresse & Joubert (1999); Schulz et al. (2009); Sheldrick (2015a,c).

Supporting information

Computing details

For both structures, data collection: APEX2 v2012.2; cell refinement: SAINT V8.40A; data reduction: SAINT V8.40A; program(s) used to solve structure: SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2018); molecular graphics: XP Version 5.1; software used to prepare material for publication: XP Version 5.1.

(twin5)

Crystal data

P4	F(000) = 6960
Mr = 123.88	Dx = 1.955 Mg m^−3
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71073 Å
a = 18.302 (2) Å	Cell parameters from 2191 reflections
b = 18.302 (2) Å	θ = 3.6–23.6°
c = 36.441 (3) Å	µ = 1.56 mm^−1
V = 12206 (2) Å^3	T = 100 K
Z = 116	Needle, white

Data collection

Bruker Smart APEX II Quazar diffractometer	11974 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	Rint = 0.072
ω scans	θmax = 25.9°, θmin = 1.7°
Absorption correction: multi-scan TWINABS 2012/1: M. Sevvana, M. Ruf, I. Uson, G. M. Sheldrick, R. Herbst-Irmer, Acta Crystallogr. 2019, D75, 1040-1050.	h = −22→22
Tmin = 0.548, Tmax = 0.745	k = −22→22
52805 measured reflections	l = −44→44
12639 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0394P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.036	(Δ/σ)max < 0.001
wR(F^2) = 0.084	Δρmax = 0.48 e Å^−3
S = 1.01	Δρmin = −0.43 e Å^−3
12639 reflections	Absolute structure: No quotients, so Flack parameter determined by classical intensity fit
1050 parameters	Absolute structure parameter: −10 (10)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 6-component twin.

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

	x	y	z	Uiso*/Ueq
P2	0.68177 (18)	0.42353 (17)	0.55252 (7)	0.0403 (7)
P1	0.74685 (16)	0.36490 (17)	0.51248 (8)	0.0386 (7)
P3	0.63485 (16)	0.33071 (15)	0.52337 (8)	0.0362 (6)
P4	0.65595 (17)	0.43267 (17)	0.49444 (7)	0.0383 (7)
P5	0.54742 (15)	0.42321 (19)	0.40569 (8)	0.0409 (7)
P6	0.48195 (15)	0.36781 (18)	0.44772 (7)	0.0365 (7)
P7	0.44171 (16)	0.37502 (16)	0.39158 (7)	0.0337 (6)
P8	0.44664 (17)	0.47313 (17)	0.42561 (8)	0.0393 (7)
P9	0.53440 (15)	0.58501 (19)	0.34372 (8)	0.0429 (8)
P10	0.44931 (19)	0.51946 (15)	0.31800 (8)	0.0387 (7)
P11	0.46307 (15)	0.63425 (15)	0.30285 (7)	0.0294 (6)
P12	0.42101 (17)	0.60595 (18)	0.35669 (7)	0.0385 (7)
P13	0.49812 (16)	0.13866 (18)	0.51577 (8)	0.0416 (7)
P14	0.4353 (3)	0.23715 (17)	0.52480 (10)	0.0670 (12)
P15	0.40267 (18)	0.13581 (19)	0.54999 (9)	0.0505 (8)
P16	0.49789 (17)	0.1915 (2)	0.56946 (8)	0.0474 (8)
P17	0.46941 (15)	0.43406 (16)	0.54670 (8)	0.0358 (6)
P18	0.40472 (17)	0.52269 (18)	0.52336 (8)	0.0410 (7)
P19	0.35190 (16)	0.42164 (17)	0.54120 (8)	0.0412 (7)
P20	0.39628 (17)	0.49658 (16)	0.58154 (7)	0.0375 (7)
P21	0.58186 (17)	0.58978 (17)	0.57495 (8)	0.0431 (7)
P22	0.66719 (15)	0.60208 (17)	0.61597 (7)	0.0343 (6)
P23	0.61051 (19)	0.69799 (15)	0.59494 (9)	0.0447 (7)
P24	0.55370 (16)	0.6220 (2)	0.63064 (8)	0.0467 (8)
P25	0.55714 (17)	0.41683 (17)	0.64453 (8)	0.0392 (7)
P26	0.60626 (19)	0.31182 (17)	0.63044 (8)	0.0454 (7)
P27	0.67426 (16)	0.40223 (19)	0.64962 (8)	0.0423 (7)
P28	0.60062 (17)	0.34706 (17)	0.68746 (7)	0.0399 (7)
P29	0.37721 (16)	0.30823 (16)	0.62703 (7)	0.0358 (6)
P30	0.34752 (17)	0.19799 (15)	0.64432 (7)	0.0353 (6)
P31	0.41800 (15)	0.26538 (15)	0.67917 (7)	0.0324 (6)
P32	0.30266 (16)	0.29233 (18)	0.67317 (8)	0.0402 (7)
P33	0.67379 (18)	0.5952 (2)	0.76895 (8)	0.0466 (8)
P34	0.70161 (18)	0.60333 (17)	0.71098 (8)	0.0388 (7)
P35	0.61043 (17)	0.53554 (15)	0.72848 (8)	0.0398 (7)
P36	0.60126 (19)	0.65370 (15)	0.73176 (9)	0.0429 (7)
P37	0.47806 (16)	0.05387 (18)	0.66609 (9)	0.0444 (8)
P38	0.5789 (2)	0.1035 (2)	0.64915 (9)	0.0617 (11)
P39	0.5807 (2)	0.00991 (17)	0.68526 (9)	0.0489 (8)
P40	0.54415 (18)	0.11571 (19)	0.70522 (8)	0.0443 (8)
P41	0.17607 (16)	0.69538 (18)	0.32990 (7)	0.0396 (7)
P42	0.19039 (16)	0.67100 (16)	0.27197 (6)	0.0331 (6)
P43	0.28089 (15)	0.71504 (16)	0.30399 (8)	0.0354 (6)
P44	0.24440 (17)	0.60284 (15)	0.31298 (9)	0.0391 (7)
P45	0.23686 (18)	0.3131 (2)	0.28912 (9)	0.0482 (8)
P46	0.35295 (16)	0.33174 (17)	0.29714 (8)	0.0370 (6)
P47	0.27413 (18)	0.39696 (16)	0.32792 (10)	0.0457 (8)
P48	0.28857 (17)	0.28106 (17)	0.34044 (8)	0.0390 (7)
P49	0.73488 (16)	0.5918 (2)	0.24454 (10)	0.0531 (9)
P50	0.6338 (2)	0.54279 (18)	0.26300 (9)	0.0541 (9)
P51	0.6315 (2)	0.63807 (17)	0.22816 (9)	0.0462 (8)
P52	0.66644 (17)	0.53278 (17)	0.20590 (8)	0.0389 (7)
P53	0.48855 (18)	0.91299 (17)	0.35195 (9)	0.0436 (7)
P54	0.44309 (19)	0.80410 (18)	0.34800 (9)	0.0504 (9)
P55	0.37444 (16)	0.89481 (17)	0.36506 (8)	0.0390 (7)
P56	0.45829 (17)	0.8540 (2)	0.40118 (7)	0.0446 (8)
P57	0.56281 (18)	0.68308 (16)	0.43163 (7)	0.0391 (7)
P58	0.64675 (15)	0.67716 (16)	0.47360 (9)	0.0393 (7)
P59	0.53698 (17)	0.71126 (16)	0.48800 (8)	0.0375 (7)
P60	0.55836 (16)	0.59736 (14)	0.47307 (8)	0.0364 (6)
P61	0.54742 (17)	0.88270 (17)	0.54566 (8)	0.0391 (7)
P62	0.58727 (17)	0.98685 (16)	0.56687 (9)	0.0434 (8)
P63	0.5619 (2)	0.89806 (18)	0.60414 (8)	0.0531 (9)
P64	0.47540 (16)	0.95585 (18)	0.57609 (9)	0.0416 (7)
P65	0.35203 (16)	0.66028 (17)	0.45248 (7)	0.0365 (6)
P66	0.26392 (16)	0.61667 (15)	0.41854 (7)	0.0341 (6)
P67	0.30206 (14)	0.72835 (13)	0.41007 (6)	0.0261 (5)
P68	0.24110 (17)	0.70134 (17)	0.45933 (7)	0.0386 (7)
P69	0.87726 (17)	0.64293 (15)	0.50906 (7)	0.0350 (6)
P70	0.88837 (17)	0.52717 (15)	0.52227 (8)	0.0403 (7)
P71	0.78957 (16)	0.58647 (17)	0.53752 (7)	0.0369 (7)
P72	0.81149 (16)	0.56144 (16)	0.47995 (7)	0.0345 (6)
P73	0.20487 (15)	0.55520 (16)	0.52229 (7)	0.0339 (6)
P74	0.10164 (17)	0.51003 (16)	0.54074 (8)	0.0379 (7)
P75	0.12320 (17)	0.62625 (14)	0.54671 (8)	0.0369 (7)
P76	0.18145 (18)	0.54816 (16)	0.58104 (7)	0.0392 (7)
P77	0.42122 (17)	0.72448 (19)	0.56798 (9)	0.0468 (8)
P78	0.3070 (2)	0.7105 (2)	0.55787 (9)	0.0533 (9)
P79	0.3440 (2)	0.79491 (15)	0.59508 (8)	0.0476 (8)
P80	0.35289 (17)	0.68012 (15)	0.61066 (7)	0.0357 (6)
P81	0.71511 (16)	0.25520 (17)	0.42804 (8)	0.0390 (7)
P82	0.60456 (16)	0.21580 (19)	0.43742 (8)	0.0429 (7)
P83	0.6836 (2)	0.14935 (16)	0.40738 (9)	0.0464 (8)
P84	0.63880 (19)	0.2481 (2)	0.38226 (8)	0.0487 (8)
P85	0.40694 (17)	0.45836 (15)	0.70896 (8)	0.0391 (7)
P86	0.32527 (16)	0.50228 (16)	0.67092 (7)	0.0355 (6)
P87	0.40635 (15)	0.57478 (15)	0.69538 (7)	0.0337 (6)
P88	0.32015 (15)	0.52895 (16)	0.72931 (6)	0.0305 (6)
P89	0.15416 (16)	0.41462 (16)	0.72445 (8)	0.0374 (7)
P90	0.13555 (15)	0.46859 (17)	0.67178 (7)	0.0354 (6)
P91	0.04319 (15)	0.44001 (16)	0.70657 (8)	0.0354 (6)
P92	0.11693 (16)	0.52732 (15)	0.72297 (8)	0.0354 (6)
P93	0.72622 (18)	0.81516 (19)	0.31442 (9)	0.0468 (8)
P94	0.65432 (19)	0.7841 (2)	0.35885 (8)	0.0505 (9)
P95	0.70892 (18)	0.70059 (16)	0.32710 (8)	0.0421 (7)
P96	0.62189 (16)	0.76508 (16)	0.30209 (7)	0.0360 (6)
P97	0.46653 (17)	0.79532 (18)	0.67294 (7)	0.0417 (7)
P98	0.3977 (2)	0.87455 (18)	0.70134 (9)	0.0484 (8)
P99	0.4038 (2)	0.76422 (18)	0.72145 (9)	0.0540 (9)
P100	0.49626 (18)	0.8364 (3)	0.72689 (9)	0.0632 (11)
P101	0.80958 (15)	0.52033 (17)	0.37073 (8)	0.0375 (7)
P102	0.70339 (15)	0.55096 (14)	0.39246 (7)	0.0288 (6)
P103	0.74766 (17)	0.44324 (15)	0.40384 (8)	0.0362 (6)
P104	0.71095 (16)	0.47019 (18)	0.34871 (7)	0.0393 (7)
P105	0.19926 (15)	0.36154 (15)	0.48318 (7)	0.0314 (6)
P106	0.29692 (15)	0.31307 (16)	0.45916 (9)	0.0391 (7)
P107	0.19925 (18)	0.32839 (18)	0.42603 (7)	0.0402 (7)
P108	0.26338 (16)	0.42341 (15)	0.44330 (9)	0.0399 (7)
P109	0.56409 (18)	0.36300 (17)	0.30628 (8)	0.0425 (7)
P110	0.5394 (2)	0.25943 (17)	0.28090 (11)	0.0544 (9)
P111	0.64781 (17)	0.30547 (18)	0.27623 (9)	0.0455 (8)
P112	0.5569 (2)	0.3549 (2)	0.24732 (9)	0.0608 (10)
P113	0.47395 (17)	0.07852 (16)	0.40167 (8)	0.0405 (7)
P114	0.41388 (19)	0.16892 (19)	0.42576 (8)	0.0459 (8)
P115	0.44365 (19)	0.17071 (18)	0.36774 (8)	0.0452 (8)
P116	0.36047 (18)	0.0945 (2)	0.38716 (9)	0.0494 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
P2	0.0588 (19)	0.0410 (16)	0.0211 (13)	0.0001 (15)	0.0048 (12)	−0.0076 (12)
P1	0.0310 (15)	0.0406 (16)	0.0442 (16)	0.0081 (13)	0.0083 (12)	0.0030 (14)
P3	0.0380 (16)	0.0247 (13)	0.0458 (16)	−0.0035 (12)	0.0032 (13)	0.0001 (12)
P4	0.0442 (17)	0.0396 (16)	0.0309 (14)	0.0055 (14)	−0.0054 (12)	0.0132 (13)
P5	0.0266 (14)	0.0587 (19)	0.0375 (15)	−0.0140 (14)	0.0103 (12)	−0.0055 (15)
P6	0.0312 (15)	0.0539 (18)	0.0245 (13)	−0.0003 (13)	−0.0040 (11)	0.0113 (13)
P7	0.0396 (16)	0.0386 (15)	0.0228 (12)	−0.0103 (13)	−0.0079 (11)	−0.0040 (12)
P8	0.0440 (18)	0.0333 (15)	0.0405 (16)	−0.0037 (13)	0.0086 (13)	−0.0095 (13)
P9	0.0228 (15)	0.066 (2)	0.0395 (16)	0.0115 (14)	−0.0099 (12)	−0.0065 (15)
P10	0.057 (2)	0.0271 (14)	0.0319 (14)	−0.0025 (14)	−0.0059 (13)	−0.0017 (12)
P11	0.0351 (15)	0.0271 (13)	0.0259 (12)	0.0038 (12)	0.0006 (11)	0.0008 (11)
P12	0.0385 (17)	0.0496 (18)	0.0275 (13)	0.0195 (14)	0.0083 (12)	0.0025 (13)
P13	0.0367 (16)	0.0591 (19)	0.0289 (14)	0.0058 (15)	0.0119 (12)	−0.0068 (14)
P14	0.130 (4)	0.0263 (16)	0.0443 (19)	0.022 (2)	−0.025 (2)	0.0025 (14)
P15	0.0411 (18)	0.0528 (19)	0.0576 (19)	−0.0235 (16)	0.0219 (15)	−0.0139 (16)
P16	0.0353 (17)	0.074 (2)	0.0333 (15)	0.0012 (16)	−0.0142 (12)	−0.0167 (16)
P17	0.0292 (15)	0.0344 (15)	0.0439 (16)	0.0078 (12)	−0.0009 (12)	−0.0048 (13)
P18	0.0450 (17)	0.0474 (17)	0.0304 (14)	0.0060 (14)	0.0079 (12)	0.0188 (13)
P19	0.0327 (16)	0.0376 (16)	0.0532 (18)	−0.0078 (13)	−0.0098 (13)	−0.0063 (14)
P20	0.0519 (18)	0.0395 (16)	0.0211 (12)	−0.0006 (14)	0.0084 (12)	−0.0098 (12)
P21	0.0452 (18)	0.0409 (17)	0.0431 (16)	0.0022 (14)	−0.0131 (14)	−0.0186 (14)
P22	0.0259 (14)	0.0471 (17)	0.0298 (13)	0.0054 (13)	−0.0013 (11)	0.0040 (12)
P23	0.0564 (19)	0.0216 (13)	0.0560 (19)	−0.0080 (14)	−0.0043 (15)	0.0062 (13)
P24	0.0306 (16)	0.076 (2)	0.0337 (15)	0.0103 (16)	0.0103 (12)	0.0168 (16)
P25	0.0408 (17)	0.0344 (15)	0.0422 (16)	0.0051 (13)	−0.0024 (13)	0.0074 (13)
P26	0.058 (2)	0.0386 (17)	0.0397 (16)	−0.0012 (15)	0.0068 (14)	−0.0145 (14)
P27	0.0305 (15)	0.065 (2)	0.0312 (14)	−0.0139 (15)	0.0003 (12)	0.0032 (14)
P28	0.0457 (18)	0.0501 (18)	0.0238 (13)	−0.0035 (15)	0.0020 (12)	0.0091 (13)
P29	0.0469 (17)	0.0365 (15)	0.0241 (12)	−0.0074 (13)	0.0016 (12)	0.0091 (12)
P30	0.0475 (17)	0.0273 (14)	0.0311 (13)	−0.0096 (13)	−0.0064 (12)	−0.0052 (11)
P31	0.0324 (15)	0.0348 (15)	0.0300 (13)	−0.0065 (12)	−0.0089 (11)	0.0022 (11)
P32	0.0360 (16)	0.0531 (18)	0.0315 (14)	0.0012 (14)	0.0072 (12)	−0.0124 (13)
P33	0.0501 (19)	0.066 (2)	0.0240 (14)	−0.0059 (17)	−0.0057 (13)	−0.0090 (14)
P34	0.0489 (18)	0.0379 (15)	0.0297 (14)	0.0009 (14)	0.0080 (12)	0.0005 (12)
P35	0.0438 (17)	0.0274 (14)	0.0483 (17)	−0.0057 (13)	−0.0078 (13)	−0.0043 (13)
P36	0.055 (2)	0.0268 (14)	0.0470 (17)	0.0043 (14)	0.0100 (15)	0.0018 (13)
P37	0.0293 (16)	0.0495 (19)	0.0545 (19)	0.0013 (14)	−0.0114 (13)	−0.0203 (16)
P38	0.079 (3)	0.071 (2)	0.0347 (16)	−0.035 (2)	0.0125 (17)	0.0061 (16)
P39	0.061 (2)	0.0355 (17)	0.0505 (18)	0.0139 (15)	−0.0220 (16)	−0.0052 (14)
P40	0.0424 (18)	0.0533 (19)	0.0372 (15)	0.0104 (15)	−0.0074 (13)	−0.0234 (15)
P41	0.0414 (17)	0.0562 (19)	0.0211 (12)	0.0081 (15)	0.0063 (12)	−0.0021 (13)
P42	0.0361 (15)	0.0456 (16)	0.0177 (11)	−0.0017 (13)	−0.0057 (10)	−0.0034 (11)
P43	0.0308 (15)	0.0343 (15)	0.0412 (16)	−0.0071 (12)	−0.0034 (12)	0.0011 (13)
P44	0.0392 (17)	0.0262 (14)	0.0518 (17)	−0.0002 (13)	−0.0101 (14)	0.0045 (13)
P45	0.0389 (18)	0.062 (2)	0.0436 (17)	0.0036 (16)	−0.0163 (14)	−0.0065 (16)
P46	0.0295 (15)	0.0451 (17)	0.0363 (14)	−0.0043 (13)	0.0073 (12)	0.0002 (13)
P47	0.0479 (19)	0.0293 (15)	0.060 (2)	0.0059 (14)	0.0045 (16)	−0.0068 (15)
P48	0.0470 (18)	0.0391 (16)	0.0311 (14)	0.0041 (14)	0.0035 (12)	0.0119 (13)
P49	0.0233 (15)	0.076 (2)	0.060 (2)	−0.0016 (16)	−0.0034 (13)	−0.0346 (18)
P50	0.077 (3)	0.0470 (19)	0.0378 (16)	−0.0111 (18)	0.0236 (16)	0.0062 (15)
P51	0.063 (2)	0.0322 (15)	0.0431 (17)	0.0058 (15)	−0.0188 (15)	−0.0029 (14)
P52	0.0439 (17)	0.0427 (17)	0.0302 (14)	−0.0023 (14)	−0.0004 (12)	−0.0159 (13)
P53	0.0435 (18)	0.0358 (16)	0.0515 (18)	−0.0103 (14)	0.0174 (14)	0.0101 (14)
P54	0.056 (2)	0.0396 (17)	0.0558 (19)	−0.0126 (16)	0.0173 (16)	−0.0255 (15)
P55	0.0295 (15)	0.0403 (16)	0.0472 (17)	0.0043 (13)	−0.0027 (12)	0.0153 (14)
P56	0.0402 (17)	0.071 (2)	0.0231 (13)	0.0012 (16)	−0.0039 (12)	0.0072 (14)
P57	0.061 (2)	0.0357 (15)	0.0209 (12)	−0.0018 (14)	−0.0072 (12)	−0.0028 (12)
P58	0.0277 (15)	0.0360 (15)	0.0543 (18)	−0.0034 (12)	−0.0082 (13)	0.0044 (14)
P59	0.0481 (18)	0.0318 (15)	0.0325 (14)	0.0046 (13)	0.0142 (13)	−0.0054 (12)
P60	0.0410 (17)	0.0215 (13)	0.0466 (16)	−0.0035 (12)	−0.0012 (13)	0.0024 (12)
P61	0.0448 (17)	0.0405 (16)	0.0319 (14)	0.0005 (14)	0.0037 (12)	−0.0202 (13)
P62	0.0403 (18)	0.0331 (16)	0.0569 (19)	−0.0140 (14)	0.0123 (14)	−0.0026 (14)
P63	0.092 (3)	0.0398 (17)	0.0276 (15)	0.0175 (18)	−0.0098 (16)	0.0090 (13)
P64	0.0251 (15)	0.0543 (19)	0.0455 (17)	0.0074 (14)	0.0015 (12)	−0.0072 (15)
P65	0.0341 (15)	0.0447 (16)	0.0308 (14)	0.0054 (13)	−0.0083 (12)	0.0046 (13)
P66	0.0421 (16)	0.0244 (13)	0.0357 (15)	−0.0110 (12)	−0.0002 (12)	−0.0020 (12)
P67	0.0324 (14)	0.0232 (12)	0.0228 (12)	−0.0046 (11)	0.0043 (10)	0.0049 (10)
P68	0.0450 (17)	0.0428 (17)	0.0279 (13)	0.0068 (14)	0.0184 (12)	0.0024 (12)
P69	0.0498 (18)	0.0268 (13)	0.0285 (13)	−0.0126 (13)	0.0044 (12)	0.0004 (11)
P70	0.0503 (18)	0.0284 (14)	0.0422 (16)	0.0140 (13)	−0.0128 (14)	0.0002 (13)
P71	0.0393 (16)	0.0436 (17)	0.0279 (14)	−0.0082 (13)	0.0122 (11)	−0.0086 (13)
P72	0.0402 (16)	0.0421 (16)	0.0213 (12)	−0.0013 (13)	−0.0061 (11)	−0.0055 (11)
P73	0.0316 (15)	0.0396 (15)	0.0305 (13)	0.0039 (12)	0.0075 (11)	−0.0042 (12)
P74	0.0406 (17)	0.0331 (15)	0.0400 (15)	−0.0140 (13)	−0.0020 (12)	0.0038 (12)
P75	0.0501 (18)	0.0241 (13)	0.0366 (15)	0.0135 (13)	0.0059 (13)	−0.0019 (12)
P76	0.061 (2)	0.0349 (15)	0.0219 (13)	−0.0048 (15)	−0.0087 (12)	0.0073 (11)
P77	0.0338 (17)	0.057 (2)	0.0491 (18)	0.0128 (15)	0.0182 (14)	0.0135 (16)
P78	0.055 (2)	0.059 (2)	0.0461 (18)	−0.0214 (17)	−0.0268 (15)	0.0041 (16)
P79	0.081 (2)	0.0231 (14)	0.0387 (15)	0.0130 (15)	0.0053 (16)	−0.0052 (13)
P80	0.0526 (18)	0.0300 (14)	0.0247 (13)	0.0018 (13)	0.0055 (12)	0.0120 (11)
P81	0.0385 (17)	0.0418 (17)	0.0366 (15)	−0.0168 (14)	0.0031 (12)	−0.0043 (13)
P82	0.0302 (16)	0.064 (2)	0.0344 (15)	−0.0051 (15)	0.0056 (12)	0.0126 (15)
P83	0.064 (2)	0.0242 (14)	0.0509 (17)	−0.0055 (14)	−0.0020 (16)	−0.0018 (13)
P84	0.051 (2)	0.066 (2)	0.0292 (14)	0.0085 (17)	−0.0005 (13)	0.0188 (15)
P85	0.0464 (18)	0.0285 (14)	0.0425 (16)	0.0125 (13)	−0.0022 (13)	0.0043 (12)
P86	0.0385 (16)	0.0503 (17)	0.0178 (12)	−0.0049 (13)	−0.0038 (11)	−0.0026 (12)
P87	0.0365 (16)	0.0299 (14)	0.0346 (14)	−0.0103 (12)	0.0018 (12)	0.0072 (12)
P88	0.0294 (14)	0.0433 (16)	0.0189 (12)	−0.0014 (12)	0.0037 (10)	−0.0014 (11)
P89	0.0349 (16)	0.0363 (15)	0.0409 (15)	0.0058 (13)	−0.0064 (12)	0.0150 (13)
P90	0.0333 (15)	0.0529 (18)	0.0201 (12)	0.0019 (13)	0.0044 (11)	0.0033 (12)
P91	0.0237 (14)	0.0418 (16)	0.0406 (15)	−0.0064 (12)	−0.0014 (11)	0.0114 (13)
P92	0.0393 (16)	0.0314 (14)	0.0356 (14)	−0.0009 (12)	0.0001 (12)	−0.0106 (12)
P93	0.0460 (18)	0.0492 (18)	0.0452 (17)	−0.0205 (16)	−0.0054 (14)	0.0195 (15)
P94	0.057 (2)	0.072 (2)	0.0220 (13)	0.0095 (18)	0.0071 (13)	−0.0133 (15)
P95	0.056 (2)	0.0313 (15)	0.0390 (16)	0.0082 (14)	−0.0073 (14)	−0.0014 (13)
P96	0.0355 (16)	0.0432 (16)	0.0294 (13)	−0.0026 (13)	−0.0081 (11)	−0.0026 (12)
P97	0.0482 (18)	0.0510 (18)	0.0260 (13)	0.0042 (15)	0.0051 (12)	−0.0138 (13)
P98	0.059 (2)	0.0414 (17)	0.0452 (17)	0.0240 (16)	0.0082 (15)	0.0127 (14)
P99	0.086 (3)	0.0353 (16)	0.0407 (17)	−0.0120 (17)	0.0149 (17)	0.0023 (14)
P100	0.0305 (17)	0.116 (3)	0.0434 (18)	−0.0032 (19)	−0.0065 (14)	−0.036 (2)
P101	0.0247 (15)	0.0429 (16)	0.0448 (16)	−0.0057 (13)	0.0054 (12)	−0.0069 (13)
P102	0.0302 (14)	0.0230 (12)	0.0333 (13)	0.0082 (11)	−0.0026 (11)	−0.0042 (11)
P103	0.0488 (18)	0.0289 (14)	0.0310 (14)	0.0080 (13)	−0.0022 (12)	0.0086 (12)
P104	0.0366 (16)	0.0565 (19)	0.0247 (13)	−0.0009 (14)	−0.0069 (11)	−0.0152 (13)
P105	0.0363 (15)	0.0333 (14)	0.0247 (12)	−0.0006 (12)	0.0087 (11)	−0.0038 (11)
P106	0.0264 (15)	0.0298 (14)	0.0610 (19)	0.0094 (12)	0.0059 (13)	0.0137 (14)
P107	0.0494 (18)	0.0489 (18)	0.0223 (13)	−0.0007 (15)	−0.0034 (12)	−0.0045 (12)
P108	0.0370 (16)	0.0274 (14)	0.0554 (18)	0.0034 (13)	0.0123 (13)	0.0163 (13)
P109	0.055 (2)	0.0420 (17)	0.0308 (14)	0.0041 (15)	0.0077 (13)	−0.0169 (13)
P110	0.048 (2)	0.0282 (15)	0.087 (3)	−0.0124 (14)	0.0106 (18)	−0.0088 (16)
P111	0.0301 (15)	0.0527 (19)	0.0538 (18)	0.0035 (14)	0.0101 (14)	−0.0050 (16)
P112	0.072 (3)	0.083 (3)	0.0276 (15)	0.000 (2)	−0.0109 (15)	0.0154 (17)
P113	0.0434 (17)	0.0350 (15)	0.0433 (16)	0.0099 (13)	−0.0074 (13)	−0.0013 (13)
P114	0.0509 (19)	0.0528 (19)	0.0340 (15)	0.0013 (16)	0.0103 (14)	−0.0193 (14)
P115	0.062 (2)	0.0443 (18)	0.0290 (14)	0.0010 (16)	−0.0009 (14)	0.0115 (13)
P116	0.0370 (17)	0.068 (2)	0.0431 (17)	−0.0089 (17)	−0.0064 (14)	−0.0088 (16)

Geometric parameters (Å, º)

P2—P1	2.168 (4)	P58—P59	2.168 (4)
P2—P4	2.175 (4)	P58—P60	2.180 (4)
P2—P3	2.180 (4)	P59—P60	2.190 (4)
P1—P4	2.177 (4)	P61—P63	2.166 (4)
P1—P3	2.179 (4)	P61—P62	2.182 (4)
P3—P4	2.178 (4)	P61—P64	2.182 (4)
P5—P8	2.183 (4)	P62—P64	2.151 (4)
P5—P7	2.187 (4)	P62—P63	2.168 (4)
P5—P6	2.193 (4)	P63—P64	2.160 (5)
P6—P7	2.178 (4)	P65—P68	2.179 (4)
P6—P8	2.187 (4)	P65—P66	2.183 (4)
P7—P8	2.184 (4)	P65—P67	2.186 (4)
P9—P12	2.163 (4)	P66—P67	2.182 (4)
P9—P11	2.176 (4)	P66—P68	2.188 (4)
P9—P10	2.178 (4)	P67—P68	2.171 (3)
P10—P12	2.182 (4)	P69—P71	2.172 (4)
P10—P11	2.187 (4)	P69—P70	2.182 (4)
P11—P12	2.171 (4)	P69—P72	2.191 (4)
P13—P15	2.147 (4)	P70—P72	2.180 (4)
P13—P14	2.164 (5)	P70—P71	2.181 (4)
P13—P16	2.182 (4)	P71—P72	2.185 (4)
P14—P15	2.154 (5)	P73—P74	2.169 (4)
P14—P16	2.159 (5)	P73—P75	2.172 (4)
P15—P16	2.140 (4)	P73—P76	2.187 (4)
P17—P20	2.171 (4)	P74—P75	2.174 (4)
P17—P19	2.172 (4)	P74—P76	2.186 (4)
P17—P18	2.181 (4)	P75—P76	2.178 (4)
P18—P20	2.179 (4)	P77—P78	2.138 (5)
P18—P19	2.186 (4)	P77—P79	2.152 (4)
P19—P20	2.168 (4)	P77—P80	2.155 (4)
P21—P23	2.174 (4)	P78—P79	2.164 (5)
P21—P22	2.174 (4)	P78—P80	2.172 (4)
P21—P24	2.176 (4)	P79—P80	2.182 (4)
P22—P24	2.175 (4)	P81—P83	2.157 (4)
P22—P23	2.178 (4)	P81—P82	2.175 (4)
P23—P24	2.170 (4)	P81—P84	2.180 (4)
P25—P27	2.168 (4)	P82—P83	2.184 (5)
P25—P28	2.171 (4)	P82—P84	2.187 (4)
P25—P26	2.183 (4)	P83—P84	2.185 (4)
P26—P28	2.178 (4)	P85—P88	2.178 (4)
P26—P27	2.185 (4)	P85—P87	2.188 (4)
P27—P28	2.177 (4)	P85—P86	2.191 (4)
P29—P30	2.183 (4)	P86—P87	2.181 (4)
P29—P31	2.187 (4)	P86—P88	2.185 (3)
P29—P32	2.185 (4)	P87—P88	2.173 (4)
P30—P32	2.182 (4)	P89—P92	2.173 (4)
P30—P31	2.190 (4)	P89—P91	2.183 (4)
P31—P32	2.179 (4)	P89—P90	2.185 (4)
P33—P35	2.171 (4)	P90—P91	2.177 (4)
P33—P36	2.178 (5)	P90—P92	2.180 (4)
P33—P34	2.178 (4)	P91—P92	2.175 (4)
P34—P35	2.175 (4)	P93—P96	2.165 (4)
P34—P36	2.190 (4)	P93—P94	2.162 (4)
P35—P36	2.172 (4)	P93—P95	2.170 (4)
P37—P38	2.148 (5)	P94—P95	2.162 (4)
P37—P39	2.159 (4)	P94—P96	2.180 (4)
P37—P40	2.186 (4)	P95—P96	2.182 (4)
P38—P40	2.152 (5)	P97—P100	2.174 (4)
P38—P39	2.160 (5)	P97—P98	2.182 (4)
P39—P40	2.174 (4)	P97—P99	2.183 (4)
P41—P43	2.168 (4)	P98—P100	2.147 (5)
P41—P42	2.174 (3)	P98—P99	2.151 (4)
P41—P44	2.194 (4)	P99—P100	2.156 (5)
P42—P44	2.183 (4)	P101—P102	2.172 (4)
P42—P43	2.181 (4)	P101—P103	2.175 (4)
P43—P44	2.184 (4)	P101—P104	2.178 (4)
P45—P46	2.172 (4)	P102—P103	2.171 (4)
P45—P48	2.177 (4)	P102—P104	2.178 (4)
P45—P47	2.195 (5)	P103—P104	2.175 (4)
P46—P48	2.177 (4)	P105—P107	2.169 (4)
P46—P47	2.183 (4)	P105—P106	2.179 (4)
P47—P48	2.186 (4)	P105—P108	2.184 (4)
P49—P51	2.158 (5)	P106—P107	2.175 (4)
P49—P50	2.163 (5)	P106—P108	2.188 (4)
P49—P52	2.172 (4)	P107—P108	2.190 (4)
P50—P51	2.157 (5)	P109—P111	2.158 (4)
P50—P52	2.172 (4)	P109—P110	2.157 (4)
P51—P52	2.186 (4)	P109—P112	2.158 (4)
P53—P54	2.164 (4)	P110—P112	2.158 (5)
P53—P56	2.166 (4)	P110—P111	2.162 (5)
P53—P55	2.168 (4)	P111—P112	2.167 (5)
P54—P56	2.160 (4)	P113—P116	2.163 (4)
P54—P55	2.173 (5)	P113—P115	2.164 (4)
P55—P56	2.155 (4)	P113—P114	2.172 (4)
P57—P58	2.170 (4)	P114—P115	2.183 (4)
P57—P59	2.170 (4)	P114—P116	2.189 (4)
P57—P60	2.179 (4)	P115—P116	2.183 (5)
P1—P2—P4	60.17 (13)	P58—P59—P57	60.04 (13)
P1—P2—P3	60.18 (13)	P58—P59—P60	60.02 (13)
P4—P2—P3	60.01 (13)	P57—P59—P60	59.98 (13)
P2—P1—P4	60.09 (13)	P58—P60—P57	59.73 (14)
P2—P1—P3	60.19 (14)	P58—P60—P59	59.51 (14)
P4—P1—P3	59.99 (13)	P57—P60—P59	59.56 (12)
P4—P3—P1	59.94 (13)	P63—P61—P62	59.82 (15)
P4—P3—P2	59.89 (13)	P63—P61—P64	59.59 (14)
P1—P3—P2	59.63 (13)	P62—P61—P64	59.06 (14)
P1—P4—P3	60.07 (13)	P64—P62—P63	60.02 (16)
P1—P4—P2	59.75 (13)	P64—P62—P61	60.45 (14)
P3—P4—P2	60.11 (13)	P63—P62—P61	59.71 (14)
P8—P5—P7	59.97 (13)	P64—P63—P61	60.57 (14)
P8—P5—P6	59.97 (13)	P64—P63—P62	59.60 (14)
P7—P5—P6	59.64 (12)	P61—P63—P62	60.47 (14)
P7—P6—P8	60.05 (13)	P62—P64—P63	60.38 (16)
P7—P6—P5	60.05 (13)	P62—P64—P61	60.48 (14)
P8—P6—P5	59.78 (14)	P63—P64—P61	59.83 (14)
P6—P7—P8	60.17 (14)	P68—P65—P66	60.19 (13)
P6—P7—P5	60.31 (13)	P68—P65—P67	59.64 (12)
P8—P7—P5	59.91 (14)	P66—P65—P67	59.92 (12)
P5—P8—P7	60.12 (14)	P67—P66—P65	60.09 (12)
P5—P8—P6	60.25 (14)	P67—P66—P68	59.57 (12)
P7—P8—P6	59.78 (13)	P65—P66—P68	59.81 (13)
P12—P9—P11	60.03 (12)	P68—P67—P66	60.35 (13)
P12—P9—P10	60.36 (14)	P68—P67—P65	60.03 (13)
P11—P9—P10	60.30 (13)	P66—P67—P65	59.99 (12)
P9—P10—P12	59.48 (14)	P67—P68—P65	60.33 (12)
P9—P10—P11	59.81 (13)	P67—P68—P66	60.08 (12)
P12—P10—P11	59.58 (13)	P65—P68—P66	60.00 (13)
P12—P11—P9	59.68 (13)	P71—P69—P70	60.11 (14)
P12—P11—P10	60.11 (13)	P71—P69—P72	60.09 (12)
P9—P11—P10	59.89 (14)	P70—P69—P72	59.80 (13)
P9—P12—P11	60.29 (13)	P72—P70—P69	60.29 (13)
P9—P12—P10	60.16 (14)	P72—P70—P71	60.13 (13)
P11—P12—P10	60.32 (13)	P69—P70—P71	59.72 (13)
P15—P13—P14	59.95 (17)	P69—P71—P70	60.16 (13)
P15—P13—P16	59.23 (14)	P69—P71—P72	60.37 (13)
P14—P13—P16	59.59 (15)	P70—P71—P72	59.91 (13)
P15—P14—P16	59.48 (16)	P70—P72—P71	59.96 (13)
P15—P14—P13	59.64 (14)	P70—P72—P69	59.90 (13)
P16—P14—P13	60.64 (15)	P71—P72—P69	59.54 (12)
P16—P15—P13	61.21 (14)	P74—P73—P75	60.12 (13)
P16—P15—P14	60.39 (17)	P74—P73—P76	60.23 (13)
P13—P15—P14	60.41 (17)	P75—P73—P76	59.96 (13)
P15—P16—P14	60.12 (17)	P73—P74—P75	60.01 (13)
P15—P16—P13	59.56 (14)	P73—P74—P76	60.30 (13)
P14—P16—P13	59.78 (14)	P75—P74—P76	59.95 (13)
P20—P17—P19	59.91 (13)	P73—P75—P74	59.88 (13)
P20—P17—P18	60.08 (13)	P73—P75—P76	60.37 (13)
P19—P17—P18	60.28 (14)	P74—P75—P76	60.29 (13)
P20—P18—P17	59.73 (13)	P75—P76—P74	59.76 (13)
P20—P18—P19	59.58 (13)	P75—P76—P73	59.67 (12)
P17—P18—P19	59.66 (13)	P74—P76—P73	59.47 (13)
P20—P19—P17	60.02 (13)	P78—P77—P79	60.59 (16)
P20—P19—P18	60.05 (13)	P78—P77—P80	60.78 (15)
P17—P19—P18	60.06 (14)	P79—P77—P80	60.89 (14)
P19—P20—P17	60.07 (13)	P77—P78—P79	60.03 (16)
P19—P20—P18	60.37 (14)	P77—P78—P80	59.99 (14)
P17—P20—P18	60.19 (13)	P79—P78—P80	60.44 (14)
P23—P21—P22	60.13 (14)	P77—P79—P78	59.38 (16)
P23—P21—P24	59.84 (15)	P77—P79—P80	59.61 (14)
P22—P21—P24	60.03 (13)	P78—P79—P80	59.95 (14)
P21—P22—P24	60.03 (14)	P77—P80—P78	59.23 (15)
P21—P22—P23	59.95 (14)	P77—P80—P79	59.50 (14)
P24—P22—P23	59.78 (14)	P78—P80—P79	59.61 (14)
P24—P23—P21	60.11 (15)	P83—P81—P82	60.53 (15)
P24—P23—P22	60.05 (13)	P83—P81—P84	60.50 (15)
P21—P23—P22	59.92 (13)	P82—P81—P84	60.29 (14)
P23—P24—P22	60.17 (14)	P81—P82—P83	59.33 (14)
P23—P24—P21	60.06 (14)	P81—P82—P84	59.96 (14)
P22—P24—P21	59.95 (13)	P83—P82—P84	59.99 (14)
P27—P25—P28	60.22 (14)	P81—P83—P82	60.14 (14)
P27—P25—P26	60.30 (15)	P81—P83—P84	60.26 (15)
P28—P25—P26	60.04 (14)	P82—P83—P84	60.08 (14)
P28—P26—P25	59.69 (13)	P81—P84—P83	59.25 (14)
P28—P26—P27	59.84 (13)	P81—P84—P82	59.75 (13)
P25—P26—P27	59.51 (14)	P83—P84—P82	59.93 (15)
P25—P27—P28	59.94 (13)	P88—P85—P87	59.70 (13)
P25—P27—P26	60.19 (14)	P88—P85—P86	60.02 (12)
P28—P27—P26	59.92 (14)	P87—P85—P86	59.75 (13)
P25—P28—P27	59.83 (13)	P87—P86—P88	59.69 (12)
P25—P28—P26	60.26 (14)	P87—P86—P85	60.04 (13)
P27—P28—P26	60.24 (14)	P88—P86—P85	59.68 (12)
P30—P29—P31	60.17 (12)	P88—P87—P86	60.25 (12)
P30—P29—P32	59.95 (13)	P88—P87—P85	59.92 (13)
P31—P29—P32	59.78 (13)	P86—P87—P85	60.21 (13)
P32—P30—P29	60.08 (13)	P87—P88—P85	60.37 (13)
P32—P30—P31	59.78 (13)	P87—P88—P86	60.07 (12)
P29—P30—P31	60.02 (12)	P85—P88—P86	60.30 (13)
P32—P31—P29	60.06 (13)	P92—P89—P91	59.92 (13)
P32—P31—P30	59.92 (13)	P92—P89—P90	60.01 (13)
P29—P31—P30	59.82 (12)	P91—P89—P90	59.78 (12)
P31—P32—P30	60.30 (13)	P91—P90—P92	59.91 (13)
P31—P32—P29	60.15 (13)	P91—P90—P89	60.06 (13)
P30—P32—P29	59.97 (13)	P92—P90—P89	59.71 (13)
P35—P33—P36	59.93 (13)	P90—P91—P92	60.11 (13)
P35—P33—P34	60.02 (14)	P90—P91—P89	60.17 (13)
P36—P33—P34	60.36 (14)	P92—P91—P89	59.82 (13)
P35—P34—P33	59.82 (14)	P89—P92—P91	60.27 (13)
P35—P34—P36	59.69 (13)	P89—P92—P90	60.28 (13)
P33—P34—P36	59.83 (14)	P91—P92—P90	59.98 (13)
P33—P35—P36	60.21 (15)	P96—P93—P94	60.50 (14)
P33—P35—P34	60.16 (13)	P96—P93—P95	60.43 (14)
P36—P35—P34	60.50 (14)	P94—P93—P95	59.86 (15)
P35—P36—P33	59.85 (14)	P95—P94—P93	60.26 (15)
P35—P36—P34	59.81 (14)	P95—P94—P96	60.34 (14)
P33—P36—P34	59.81 (14)	P93—P94—P96	59.82 (14)
P38—P37—P39	60.19 (17)	P94—P95—P93	59.88 (16)
P38—P37—P40	59.53 (15)	P94—P95—P96	60.24 (14)
P39—P37—P40	60.04 (14)	P93—P95—P96	59.66 (14)
P37—P38—P40	61.11 (15)	P93—P96—P95	59.90 (14)
P37—P38—P39	60.17 (16)	P93—P96—P94	59.69 (14)
P40—P38—P39	60.56 (16)	P95—P96—P94	59.42 (14)
P37—P39—P38	59.64 (17)	P100—P97—P98	59.06 (15)
P37—P39—P40	60.58 (14)	P100—P97—P99	59.32 (16)
P38—P39—P40	59.54 (16)	P98—P97—P99	59.03 (14)
P38—P40—P39	59.90 (17)	P100—P98—P99	60.22 (18)
P38—P40—P37	59.36 (15)	P100—P98—P97	60.28 (14)
P39—P40—P37	59.38 (14)	P99—P98—P97	60.50 (15)
P43—P41—P42	60.29 (13)	P98—P99—P100	59.80 (18)
P43—P41—P44	60.09 (14)	P98—P99—P97	60.46 (14)
P42—P41—P44	59.99 (13)	P100—P99—P97	60.13 (15)
P41—P42—P44	60.47 (13)	P98—P100—P99	59.98 (16)
P41—P42—P43	59.73 (13)	P98—P100—P97	60.66 (15)
P44—P42—P43	60.07 (13)	P99—P100—P97	60.55 (15)
P41—P43—P42	59.98 (12)	P102—P101—P103	59.93 (13)
P41—P43—P44	60.53 (14)	P102—P101—P104	60.10 (13)
P42—P43—P44	60.03 (13)	P103—P101—P104	59.95 (13)
P42—P44—P43	59.90 (13)	P103—P102—P101	60.10 (13)
P42—P44—P41	59.55 (12)	P103—P102—P104	60.00 (13)
P43—P44—P41	59.37 (14)	P101—P102—P104	60.09 (13)
P46—P45—P48	60.08 (13)	P102—P103—P101	59.97 (13)
P46—P45—P47	59.97 (14)	P102—P103—P104	60.16 (13)
P48—P45—P47	59.99 (14)	P101—P103—P104	60.10 (13)
P45—P46—P48	60.07 (14)	P103—P104—P101	59.95 (13)
P45—P46—P47	60.55 (15)	P103—P104—P102	59.84 (12)
P48—P46—P47	60.18 (14)	P101—P104—P102	59.82 (13)
P46—P47—P48	59.78 (13)	P107—P105—P106	60.03 (14)
P46—P47—P45	59.48 (14)	P107—P105—P108	60.41 (14)
P48—P47—P45	59.58 (14)	P106—P105—P108	60.20 (12)
P46—P48—P45	59.85 (14)	P107—P106—P105	59.76 (13)
P46—P48—P47	60.04 (14)	P107—P106—P108	60.26 (14)
P45—P48—P47	60.43 (15)	P105—P106—P108	60.02 (12)
P51—P49—P50	59.91 (16)	P105—P107—P106	60.21 (13)
P51—P49—P52	60.66 (14)	P105—P107—P108	60.14 (13)
P50—P49—P52	60.14 (14)	P106—P107—P108	60.17 (13)
P51—P50—P49	59.92 (16)	P105—P108—P106	59.78 (13)
P51—P50—P52	60.66 (15)	P105—P108—P107	59.45 (12)
P49—P50—P52	60.13 (14)	P106—P108—P107	59.57 (14)
P50—P51—P49	60.18 (17)	P111—P109—P110	60.15 (15)
P50—P51—P52	60.01 (14)	P111—P109—P112	60.29 (16)
P49—P51—P52	60.00 (14)	P110—P109—P112	60.01 (17)
P50—P52—P49	59.72 (15)	P109—P110—P112	60.01 (15)
P50—P52—P51	59.33 (14)	P109—P110—P111	59.94 (14)
P49—P52—P51	59.34 (14)	P112—P110—P111	60.22 (16)
P54—P53—P56	59.84 (15)	P109—P111—P110	59.91 (15)
P54—P53—P55	60.20 (15)	P109—P111—P112	59.85 (15)
P56—P53—P55	59.65 (13)	P110—P111—P112	59.79 (17)
P56—P54—P53	60.12 (14)	P109—P112—P110	59.99 (16)
P56—P54—P55	59.67 (14)	P109—P112—P111	59.86 (14)
P53—P54—P55	59.98 (14)	P110—P112—P111	60.00 (16)
P56—P55—P53	60.13 (14)	P116—P113—P115	60.60 (15)
P56—P55—P54	59.87 (15)	P116—P113—P114	60.66 (15)
P53—P55—P54	59.82 (15)	P115—P113—P114	60.48 (14)
P55—P56—P54	60.46 (15)	P113—P114—P115	59.59 (14)
P55—P56—P53	60.22 (14)	P113—P114—P116	59.47 (14)
P54—P56—P53	60.04 (14)	P115—P114—P116	59.91 (15)
P58—P57—P59	59.94 (14)	P113—P115—P114	59.94 (14)
P58—P57—P60	60.15 (13)	P113—P115—P116	59.67 (15)
P59—P57—P60	60.46 (13)	P114—P115—P116	60.17 (15)
P59—P58—P57	60.02 (14)	P113—P116—P115	59.72 (15)
P59—P58—P60	60.48 (14)	P113—P116—P114	59.87 (14)
P57—P58—P60	60.12 (13)	P115—P116—P114	59.92 (14)

(twin5_2)

Crystal data

P4	Dx = 1.958 Mg m^−3
Mr = 123.88	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9646 reflections
a = 18.298 (2) Å	θ = 3.7–23.2°
b = 18.298 (2) Å	µ = 1.56 mm^−1
c = 36.408 (3) Å	T = 100 K
V = 12190 (2) Å^3	Block, white
Z = 116	0.21 × 0.18 × 0.17 mm
F(000) = 6960

Data collection

Bruker Smart APEX II Quazar diffractometer	13145 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	Rint = 0.097
ω scans	θmax = 26.1°, θmin = 1.1°
Absorption correction: multi-scan TWINABS 2012/1: M. Sevvana, M. Ruf, I. Uson, G. M. Sheldrick, R. Herbst-Irmer, Acta Crystallogr. 2019, D75, 1040-1050.	h = −22→22
Tmin = 0.669, Tmax = 0.745	k = −22→22
340118 measured reflections	l = −45→45
13397 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.025P)^2 + 11.1353P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.034	(Δ/σ)max = 0.001
wR(F^2) = 0.077	Δρmax = 0.66 e Å^−3
S = 1.13	Δρmin = −0.41 e Å^−3
13397 reflections	Absolute structure: No quotients, so Flack parameter determined by classical intensity fit
1050 parameters	Absolute structure parameter: 10 (10)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 6-component twin.

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

	x	y	z	Uiso*/Ueq
P2	0.68193 (18)	0.42339 (17)	0.55247 (8)	0.0426 (7)
P1	0.74694 (15)	0.36619 (16)	0.51204 (9)	0.0409 (7)
P3	0.63598 (16)	0.33093 (15)	0.52255 (9)	0.0416 (7)
P4	0.65632 (17)	0.43413 (17)	0.49466 (8)	0.0413 (7)
P5	0.54712 (15)	0.4213 (2)	0.40673 (9)	0.0466 (8)
P6	0.48099 (15)	0.3657 (2)	0.44801 (8)	0.0450 (8)
P7	0.44252 (16)	0.37410 (17)	0.39160 (7)	0.0359 (6)
P8	0.44630 (17)	0.47110 (18)	0.42650 (9)	0.0438 (7)
P9	0.53411 (16)	0.5833 (2)	0.34405 (9)	0.0526 (9)
P10	0.4481 (2)	0.51862 (16)	0.31846 (9)	0.0470 (8)
P11	0.46279 (15)	0.63299 (15)	0.30328 (8)	0.0339 (6)
P12	0.42123 (18)	0.60507 (19)	0.35725 (8)	0.0456 (8)
P13	0.49723 (19)	0.1406 (2)	0.51543 (9)	0.0531 (9)
P14	0.4287 (4)	0.23611 (19)	0.52553 (11)	0.099 (2)
P15	0.4046 (2)	0.1347 (2)	0.55102 (12)	0.0639 (10)
P16	0.49689 (18)	0.1942 (2)	0.56872 (9)	0.0600 (10)
P17	0.46934 (14)	0.43413 (16)	0.54594 (8)	0.0378 (6)
P18	0.40476 (17)	0.52362 (18)	0.52354 (8)	0.0433 (7)
P19	0.35207 (16)	0.42211 (16)	0.54011 (9)	0.0444 (7)
P20	0.39564 (17)	0.49553 (16)	0.58117 (7)	0.0389 (7)
P21	0.58125 (17)	0.58915 (17)	0.57521 (9)	0.0448 (7)
P22	0.66728 (14)	0.60279 (17)	0.61532 (8)	0.0349 (6)
P23	0.61027 (18)	0.69796 (15)	0.59398 (10)	0.0469 (7)
P24	0.55463 (15)	0.6234 (2)	0.63057 (9)	0.0476 (8)
P25	0.55593 (17)	0.41746 (16)	0.64460 (9)	0.0403 (6)
P26	0.6054 (2)	0.31309 (18)	0.63042 (9)	0.0503 (8)
P27	0.67299 (16)	0.40380 (19)	0.64997 (8)	0.0458 (8)
P28	0.59963 (18)	0.34847 (19)	0.68763 (8)	0.0449 (7)
P29	0.37638 (16)	0.30901 (16)	0.62797 (7)	0.0370 (6)
P30	0.34818 (16)	0.19842 (14)	0.64472 (7)	0.0348 (6)
P31	0.41777 (14)	0.26546 (15)	0.67978 (7)	0.0318 (6)
P32	0.30231 (16)	0.29179 (18)	0.67390 (8)	0.0420 (7)
P33	0.67525 (19)	0.5952 (2)	0.76892 (8)	0.0479 (8)
P34	0.70270 (17)	0.60286 (16)	0.71069 (8)	0.0390 (6)
P35	0.61116 (17)	0.53550 (15)	0.72863 (9)	0.0425 (7)
P36	0.60238 (19)	0.65337 (16)	0.73171 (9)	0.0463 (7)
P37	0.47725 (16)	0.05276 (18)	0.66664 (9)	0.0459 (8)
P38	0.5762 (3)	0.1052 (2)	0.64872 (10)	0.0670 (12)
P39	0.58171 (19)	0.01175 (18)	0.68452 (10)	0.0515 (8)
P40	0.54305 (17)	0.11518 (19)	0.70545 (9)	0.0459 (8)
P41	0.17725 (16)	0.69682 (19)	0.33045 (8)	0.0433 (7)
P42	0.19013 (15)	0.67127 (16)	0.27260 (7)	0.0351 (6)
P43	0.28127 (15)	0.71471 (16)	0.30392 (8)	0.0370 (6)
P44	0.24365 (16)	0.60333 (15)	0.31363 (9)	0.0405 (7)
P45	0.23498 (18)	0.3119 (2)	0.28982 (9)	0.0503 (8)
P46	0.35167 (16)	0.33114 (17)	0.29708 (8)	0.0394 (6)
P47	0.2729 (2)	0.39608 (17)	0.32840 (11)	0.0522 (8)
P48	0.28827 (17)	0.28082 (17)	0.34063 (8)	0.0423 (7)
P49	0.73439 (16)	0.5937 (2)	0.24397 (12)	0.0686 (13)
P50	0.6346 (2)	0.5433 (2)	0.26343 (10)	0.0633 (11)
P51	0.6303 (2)	0.63708 (17)	0.22939 (10)	0.0520 (9)
P52	0.66592 (18)	0.53336 (18)	0.20687 (9)	0.0449 (7)
P53	0.48795 (18)	0.91310 (18)	0.35140 (10)	0.0502 (8)
P54	0.4431 (2)	0.80384 (18)	0.34799 (10)	0.0564 (10)
P55	0.37356 (15)	0.89397 (18)	0.36430 (9)	0.0441 (7)
P56	0.45768 (18)	0.8555 (2)	0.40048 (8)	0.0504 (8)
P57	0.56286 (18)	0.68461 (17)	0.43159 (7)	0.0402 (7)
P58	0.64725 (15)	0.67739 (16)	0.47300 (9)	0.0400 (6)
P59	0.53756 (16)	0.71207 (15)	0.48785 (7)	0.0359 (6)
P60	0.55829 (16)	0.59843 (14)	0.47241 (9)	0.0388 (6)
P61	0.54727 (18)	0.88279 (17)	0.54563 (8)	0.0418 (7)
P62	0.58513 (18)	0.98767 (17)	0.56658 (10)	0.0491 (8)
P63	0.5638 (3)	0.8989 (2)	0.60409 (9)	0.0644 (11)
P64	0.47511 (16)	0.95344 (19)	0.57725 (10)	0.0497 (8)
P65	0.35304 (16)	0.66060 (17)	0.45289 (8)	0.0384 (6)
P66	0.26476 (16)	0.61660 (14)	0.41922 (8)	0.0360 (6)
P67	0.30294 (14)	0.72751 (13)	0.41028 (7)	0.0285 (5)
P68	0.24213 (17)	0.70123 (17)	0.45982 (8)	0.0414 (7)
P69	0.87911 (18)	0.64286 (15)	0.50918 (8)	0.0393 (7)
P70	0.88901 (18)	0.52706 (15)	0.52178 (9)	0.0449 (7)
P71	0.79080 (16)	0.58636 (17)	0.53768 (8)	0.0396 (7)
P72	0.81281 (16)	0.56309 (17)	0.47985 (7)	0.0377 (6)
P73	0.20355 (14)	0.55421 (16)	0.52206 (7)	0.0348 (6)
P74	0.10137 (16)	0.50859 (16)	0.54034 (8)	0.0403 (6)
P75	0.12261 (17)	0.62511 (14)	0.54659 (8)	0.0380 (6)
P76	0.18102 (19)	0.54712 (16)	0.58075 (7)	0.0421 (7)
P77	0.42031 (17)	0.72513 (19)	0.56740 (9)	0.0475 (8)
P78	0.3058 (2)	0.7097 (2)	0.55867 (10)	0.0571 (9)
P79	0.3428 (2)	0.79428 (14)	0.59559 (9)	0.0462 (8)
P80	0.35411 (17)	0.67986 (14)	0.61089 (7)	0.0359 (6)
P81	0.71373 (17)	0.25538 (17)	0.42757 (9)	0.0454 (8)
P82	0.60428 (16)	0.2137 (2)	0.43680 (9)	0.0480 (8)
P83	0.6854 (2)	0.14932 (16)	0.40728 (10)	0.0510 (8)
P84	0.6387 (2)	0.2460 (2)	0.38195 (9)	0.0552 (9)
P85	0.40564 (18)	0.45886 (16)	0.70959 (9)	0.0440 (7)
P86	0.32541 (15)	0.50330 (17)	0.67088 (7)	0.0371 (6)
P87	0.40751 (16)	0.57469 (16)	0.69554 (8)	0.0385 (6)
P88	0.32014 (14)	0.53060 (17)	0.72929 (7)	0.0341 (6)
P89	0.15537 (16)	0.41418 (16)	0.72413 (8)	0.0410 (7)
P90	0.13613 (15)	0.46889 (17)	0.67218 (7)	0.0376 (6)
P91	0.04405 (15)	0.43933 (18)	0.70695 (9)	0.0424 (7)
P92	0.11706 (16)	0.52622 (16)	0.72341 (8)	0.0392 (6)
P93	0.72680 (19)	0.8137 (2)	0.31418 (10)	0.0599 (10)
P94	0.6558 (2)	0.7867 (3)	0.35852 (9)	0.0619 (11)
P95	0.7079 (2)	0.70090 (18)	0.32765 (10)	0.0563 (9)
P96	0.62154 (16)	0.76614 (17)	0.30224 (8)	0.0393 (6)
P97	0.46768 (17)	0.79666 (18)	0.67273 (8)	0.0440 (7)
P98	0.39662 (19)	0.87282 (18)	0.70122 (9)	0.0510 (8)
P99	0.4077 (3)	0.76394 (17)	0.72179 (10)	0.0674 (12)
P100	0.49665 (18)	0.8396 (3)	0.72633 (10)	0.0749 (14)
P101	0.80869 (14)	0.52075 (17)	0.37024 (9)	0.0412 (7)
P102	0.70251 (14)	0.54980 (14)	0.39273 (7)	0.0309 (5)
P103	0.74864 (17)	0.44341 (16)	0.40403 (8)	0.0410 (7)
P104	0.71064 (16)	0.4678 (2)	0.34950 (8)	0.0448 (7)
P105	0.19830 (15)	0.36137 (15)	0.48276 (7)	0.0339 (6)
P106	0.29493 (16)	0.31266 (16)	0.45840 (10)	0.0439 (7)
P107	0.19682 (19)	0.32738 (19)	0.42581 (8)	0.0463 (7)
P108	0.26139 (16)	0.42255 (16)	0.44247 (10)	0.0463 (8)
P109	0.5633 (2)	0.3623 (2)	0.30646 (9)	0.0526 (8)
P110	0.5388 (2)	0.25963 (18)	0.28011 (12)	0.0614 (10)
P111	0.64707 (16)	0.30627 (19)	0.27591 (10)	0.0495 (8)
P112	0.5559 (2)	0.3563 (3)	0.24778 (10)	0.0695 (11)
P113	0.47279 (17)	0.07781 (16)	0.40130 (9)	0.0442 (7)
P114	0.41221 (19)	0.1683 (2)	0.42489 (9)	0.0533 (8)
P115	0.4428 (2)	0.1694 (2)	0.36703 (9)	0.0511 (8)
P116	0.35910 (18)	0.0933 (2)	0.38677 (10)	0.0567 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
P2	0.0570 (18)	0.0447 (16)	0.0260 (13)	0.0025 (14)	0.0062 (13)	−0.0105 (12)
P1	0.0283 (13)	0.0418 (15)	0.0526 (17)	0.0109 (12)	0.0081 (12)	0.0030 (14)
P3	0.0405 (16)	0.0242 (13)	0.0602 (19)	−0.0020 (12)	−0.0016 (14)	0.0002 (13)
P4	0.0439 (16)	0.0439 (16)	0.0361 (15)	0.0078 (14)	−0.0043 (13)	0.0167 (13)
P5	0.0228 (13)	0.069 (2)	0.0483 (17)	−0.0132 (14)	0.0092 (12)	−0.0114 (16)
P6	0.0290 (14)	0.076 (2)	0.0303 (14)	0.0062 (14)	−0.0040 (11)	0.0110 (15)
P7	0.0401 (15)	0.0447 (16)	0.0230 (12)	−0.0127 (13)	−0.0060 (11)	−0.0082 (11)
P8	0.0385 (16)	0.0421 (16)	0.0507 (17)	−0.0009 (13)	0.0082 (14)	−0.0171 (14)
P9	0.0270 (14)	0.079 (2)	0.0522 (19)	0.0144 (16)	−0.0140 (13)	−0.0069 (18)
P10	0.071 (2)	0.0269 (14)	0.0428 (17)	−0.0053 (14)	−0.0123 (16)	−0.0035 (12)
P11	0.0328 (14)	0.0339 (14)	0.0352 (14)	0.0041 (11)	0.0006 (11)	−0.0015 (11)
P12	0.0448 (17)	0.0550 (19)	0.0370 (15)	0.0198 (15)	0.0112 (13)	−0.0054 (14)
P13	0.0487 (18)	0.073 (2)	0.0376 (17)	−0.0011 (17)	0.0134 (14)	−0.0146 (16)
P14	0.214 (6)	0.0271 (16)	0.057 (2)	0.041 (3)	−0.050 (3)	−0.0018 (16)
P15	0.054 (2)	0.055 (2)	0.083 (3)	−0.0252 (17)	0.0385 (19)	−0.0176 (19)
P16	0.0337 (16)	0.100 (3)	0.0461 (18)	−0.0036 (18)	−0.0141 (14)	−0.029 (2)
P17	0.0237 (12)	0.0374 (15)	0.0523 (17)	0.0073 (11)	−0.0011 (12)	−0.0084 (13)
P18	0.0419 (15)	0.0516 (17)	0.0364 (15)	0.0070 (14)	0.0104 (12)	0.0216 (13)
P19	0.0305 (14)	0.0321 (14)	0.071 (2)	−0.0078 (12)	−0.0083 (14)	−0.0094 (14)
P20	0.0509 (17)	0.0397 (15)	0.0261 (13)	0.0005 (13)	0.0110 (12)	−0.0064 (11)
P21	0.0442 (16)	0.0421 (16)	0.0482 (17)	0.0023 (14)	−0.0158 (14)	−0.0211 (13)
P22	0.0221 (12)	0.0478 (16)	0.0348 (14)	0.0042 (12)	−0.0037 (11)	0.0012 (12)
P23	0.0490 (17)	0.0233 (13)	0.068 (2)	−0.0064 (13)	0.0022 (16)	0.0078 (14)
P24	0.0279 (14)	0.074 (2)	0.0411 (16)	0.0115 (15)	0.0110 (12)	0.0203 (16)
P25	0.0404 (15)	0.0332 (14)	0.0474 (16)	0.0047 (13)	−0.0014 (13)	0.0096 (12)
P26	0.063 (2)	0.0397 (16)	0.0476 (17)	−0.0051 (15)	0.0064 (16)	−0.0178 (14)
P27	0.0318 (14)	0.066 (2)	0.0391 (15)	−0.0199 (15)	0.0024 (12)	−0.0011 (14)
P28	0.0460 (17)	0.0576 (19)	0.0311 (14)	−0.0033 (15)	0.0048 (13)	0.0056 (13)
P29	0.0399 (15)	0.0385 (15)	0.0326 (13)	−0.0075 (12)	0.0004 (12)	0.0125 (12)
P30	0.0451 (15)	0.0236 (12)	0.0358 (14)	−0.0084 (12)	−0.0048 (12)	−0.0066 (10)
P31	0.0292 (13)	0.0323 (13)	0.0339 (13)	−0.0050 (11)	−0.0105 (11)	0.0052 (11)
P32	0.0326 (14)	0.0548 (18)	0.0386 (15)	0.0041 (13)	0.0060 (12)	−0.0161 (14)
P33	0.0537 (18)	0.066 (2)	0.0239 (13)	−0.0016 (17)	−0.0091 (13)	−0.0063 (13)
P34	0.0439 (16)	0.0373 (15)	0.0358 (14)	−0.0006 (13)	0.0090 (12)	0.0008 (12)
P35	0.0411 (16)	0.0274 (13)	0.0590 (19)	−0.0076 (12)	−0.0063 (14)	−0.0081 (13)
P36	0.0555 (19)	0.0309 (14)	0.0526 (18)	0.0084 (14)	0.0141 (15)	0.0000 (13)
P37	0.0287 (14)	0.0512 (18)	0.0578 (19)	0.0050 (13)	−0.0115 (13)	−0.0246 (16)
P38	0.087 (3)	0.073 (3)	0.0412 (18)	−0.041 (2)	0.0139 (19)	0.0029 (17)
P39	0.054 (2)	0.0418 (17)	0.0590 (19)	0.0215 (15)	−0.0238 (16)	−0.0046 (15)
P40	0.0377 (16)	0.0586 (19)	0.0415 (16)	0.0110 (14)	−0.0095 (13)	−0.0263 (15)
P41	0.0398 (15)	0.0603 (19)	0.0299 (14)	0.0109 (14)	0.0116 (12)	−0.0024 (14)
P42	0.0325 (13)	0.0487 (16)	0.0239 (12)	−0.0007 (12)	−0.0059 (11)	−0.0061 (11)
P43	0.0308 (14)	0.0354 (14)	0.0450 (16)	−0.0092 (11)	−0.0047 (12)	0.0020 (12)
P44	0.0347 (15)	0.0292 (13)	0.0576 (18)	−0.0043 (12)	−0.0126 (13)	0.0043 (13)
P45	0.0398 (16)	0.058 (2)	0.0534 (19)	0.0055 (15)	−0.0185 (15)	−0.0068 (16)
P46	0.0319 (14)	0.0437 (16)	0.0425 (15)	−0.0039 (12)	0.0087 (12)	−0.0044 (13)
P47	0.0520 (19)	0.0349 (16)	0.070 (2)	0.0085 (14)	0.0049 (17)	−0.0076 (16)
P48	0.0473 (17)	0.0414 (16)	0.0383 (15)	0.0038 (13)	0.0023 (13)	0.0139 (13)
P49	0.0219 (14)	0.100 (3)	0.083 (3)	−0.0048 (17)	0.0007 (15)	−0.057 (2)
P50	0.092 (3)	0.0488 (19)	0.0495 (19)	−0.004 (2)	0.031 (2)	0.0086 (16)
P51	0.064 (2)	0.0312 (15)	0.061 (2)	0.0098 (15)	−0.0274 (17)	−0.0067 (14)
P52	0.0455 (17)	0.0452 (17)	0.0440 (16)	0.0027 (14)	−0.0069 (13)	−0.0199 (14)
P53	0.0464 (18)	0.0373 (16)	0.067 (2)	−0.0126 (14)	0.0255 (16)	0.0094 (15)
P54	0.063 (2)	0.0341 (16)	0.073 (2)	−0.0163 (15)	0.0243 (18)	−0.0330 (16)
P55	0.0262 (14)	0.0469 (17)	0.0593 (19)	0.0066 (13)	−0.0010 (13)	0.0210 (15)
P56	0.0413 (16)	0.075 (2)	0.0353 (16)	−0.0005 (16)	−0.0061 (13)	0.0056 (15)
P57	0.0549 (18)	0.0397 (15)	0.0260 (13)	−0.0008 (14)	−0.0053 (12)	−0.0032 (12)
P58	0.0237 (12)	0.0345 (14)	0.0617 (19)	−0.0030 (11)	−0.0085 (12)	0.0001 (14)
P59	0.0402 (15)	0.0334 (14)	0.0340 (14)	0.0042 (12)	0.0148 (12)	−0.0075 (11)
P60	0.0374 (15)	0.0189 (12)	0.0600 (18)	−0.0043 (11)	−0.0062 (13)	−0.0004 (12)
P61	0.0462 (16)	0.0426 (16)	0.0366 (15)	−0.0029 (13)	0.0051 (13)	−0.0193 (13)
P62	0.0473 (18)	0.0382 (16)	0.062 (2)	−0.0221 (14)	0.0197 (16)	−0.0084 (15)
P63	0.110 (3)	0.049 (2)	0.0338 (16)	0.030 (2)	−0.0162 (19)	0.0076 (14)
P64	0.0240 (14)	0.059 (2)	0.066 (2)	0.0033 (14)	0.0039 (14)	−0.0212 (17)
P65	0.0355 (14)	0.0454 (16)	0.0342 (14)	0.0051 (13)	−0.0117 (12)	0.0045 (12)
P66	0.0428 (15)	0.0194 (12)	0.0457 (16)	−0.0109 (11)	0.0017 (13)	−0.0009 (11)
P67	0.0350 (13)	0.0243 (12)	0.0261 (12)	−0.0041 (10)	0.0037 (10)	0.0057 (10)
P68	0.0445 (16)	0.0450 (16)	0.0346 (14)	0.0091 (14)	0.0154 (12)	0.0031 (13)
P69	0.0537 (18)	0.0280 (13)	0.0362 (14)	−0.0135 (13)	0.0091 (13)	0.0000 (11)
P70	0.0528 (18)	0.0267 (13)	0.0552 (18)	0.0145 (13)	−0.0166 (15)	0.0020 (13)
P71	0.0392 (15)	0.0447 (16)	0.0348 (14)	−0.0101 (13)	0.0142 (12)	−0.0117 (13)
P72	0.0404 (15)	0.0469 (16)	0.0257 (13)	0.0014 (13)	−0.0079 (11)	−0.0083 (12)
P73	0.0278 (13)	0.0416 (15)	0.0349 (13)	0.0027 (11)	0.0094 (11)	−0.0028 (12)
P74	0.0355 (15)	0.0388 (15)	0.0465 (16)	−0.0122 (12)	−0.0016 (12)	0.0023 (13)
P75	0.0463 (16)	0.0251 (13)	0.0427 (15)	0.0165 (12)	0.0025 (13)	−0.0021 (12)
P76	0.0607 (19)	0.0367 (15)	0.0289 (14)	−0.0047 (14)	−0.0086 (13)	0.0074 (11)
P77	0.0342 (16)	0.0534 (19)	0.0548 (19)	0.0086 (14)	0.0174 (14)	0.0133 (16)
P78	0.055 (2)	0.059 (2)	0.057 (2)	−0.0144 (17)	−0.0329 (17)	−0.0001 (17)
P79	0.073 (2)	0.0203 (13)	0.0451 (16)	0.0116 (14)	0.0083 (16)	−0.0041 (12)
P80	0.0525 (17)	0.0280 (13)	0.0273 (13)	0.0071 (12)	0.0071 (12)	0.0102 (11)
P81	0.0414 (16)	0.0415 (16)	0.0532 (18)	−0.0228 (14)	0.0127 (14)	−0.0093 (14)
P82	0.0268 (14)	0.074 (2)	0.0434 (17)	−0.0053 (14)	0.0061 (12)	0.0179 (16)
P83	0.064 (2)	0.0293 (15)	0.0598 (19)	−0.0058 (15)	0.0013 (17)	0.0019 (14)
P84	0.0503 (19)	0.078 (2)	0.0371 (16)	0.0100 (18)	−0.0018 (14)	0.0240 (16)
P85	0.0504 (18)	0.0289 (14)	0.0526 (18)	0.0126 (13)	−0.0029 (15)	0.0065 (13)
P86	0.0352 (14)	0.0543 (18)	0.0218 (12)	−0.0056 (13)	−0.0010 (11)	−0.0034 (12)
P87	0.0377 (15)	0.0357 (14)	0.0419 (15)	−0.0128 (12)	0.0015 (12)	0.0121 (12)
P88	0.0261 (12)	0.0531 (17)	0.0230 (12)	−0.0020 (12)	0.0031 (10)	−0.0046 (11)
P89	0.0357 (14)	0.0397 (15)	0.0477 (16)	0.0025 (12)	−0.0057 (13)	0.0222 (13)
P90	0.0315 (14)	0.0556 (18)	0.0256 (12)	0.0003 (13)	0.0063 (11)	0.0030 (12)
P91	0.0245 (13)	0.0493 (17)	0.0533 (18)	−0.0072 (12)	−0.0011 (12)	0.0134 (14)
P92	0.0378 (15)	0.0363 (15)	0.0436 (16)	−0.0010 (12)	0.0026 (12)	−0.0106 (13)
P93	0.0459 (18)	0.070 (2)	0.064 (2)	−0.0318 (18)	−0.0074 (16)	0.0318 (19)
P94	0.055 (2)	0.099 (3)	0.0319 (15)	0.017 (2)	0.0010 (14)	−0.0237 (18)
P95	0.077 (2)	0.0350 (16)	0.056 (2)	0.0098 (17)	−0.0244 (19)	−0.0008 (15)
P96	0.0368 (14)	0.0483 (16)	0.0327 (14)	−0.0032 (13)	−0.0114 (12)	−0.0062 (12)
P97	0.0461 (17)	0.0554 (19)	0.0306 (14)	0.0091 (15)	0.0021 (13)	−0.0148 (14)
P98	0.0529 (19)	0.0474 (18)	0.0527 (19)	0.0251 (16)	0.0122 (15)	0.0133 (15)
P99	0.125 (4)	0.0289 (15)	0.0484 (19)	−0.008 (2)	0.026 (2)	0.0031 (14)
P100	0.0280 (15)	0.143 (4)	0.054 (2)	−0.003 (2)	−0.0086 (15)	−0.045 (2)
P101	0.0244 (13)	0.0416 (16)	0.0577 (18)	−0.0064 (12)	0.0124 (12)	−0.0069 (14)
P102	0.0264 (12)	0.0265 (12)	0.0398 (14)	0.0100 (10)	−0.0004 (11)	−0.0034 (11)
P103	0.0529 (18)	0.0323 (14)	0.0377 (15)	0.0077 (13)	0.0012 (13)	0.0084 (12)
P104	0.0347 (15)	0.069 (2)	0.0312 (14)	−0.0014 (14)	−0.0107 (12)	−0.0220 (14)
P105	0.0362 (14)	0.0333 (13)	0.0322 (13)	−0.0006 (11)	0.0120 (11)	−0.0044 (11)
P106	0.0288 (13)	0.0300 (14)	0.073 (2)	0.0119 (11)	0.0086 (14)	0.0179 (14)
P107	0.0551 (19)	0.0563 (19)	0.0275 (14)	0.0014 (16)	−0.0022 (13)	−0.0022 (13)
P108	0.0387 (16)	0.0288 (14)	0.072 (2)	0.0075 (12)	0.0181 (15)	0.0183 (14)
P109	0.057 (2)	0.056 (2)	0.0452 (17)	0.0040 (16)	0.0103 (15)	−0.0237 (15)
P110	0.051 (2)	0.0323 (16)	0.101 (3)	−0.0137 (15)	0.013 (2)	−0.0116 (18)
P111	0.0281 (14)	0.0558 (19)	0.065 (2)	0.0011 (14)	0.0099 (14)	−0.0013 (16)
P112	0.081 (3)	0.087 (3)	0.0410 (18)	0.003 (2)	−0.0203 (18)	0.0202 (19)
P113	0.0421 (16)	0.0331 (15)	0.0574 (19)	0.0127 (13)	−0.0093 (14)	0.0021 (13)
P114	0.0505 (19)	0.058 (2)	0.0518 (18)	0.0030 (16)	0.0153 (16)	−0.0215 (16)
P115	0.062 (2)	0.055 (2)	0.0368 (16)	0.0044 (17)	−0.0012 (15)	0.0177 (14)
P116	0.0361 (16)	0.079 (3)	0.0550 (19)	−0.0065 (17)	−0.0068 (15)	−0.0075 (18)

Geometric parameters (Å, º)

P2—P1	2.163 (4)	P58—P59	2.173 (4)
P2—P4	2.165 (4)	P58—P60	2.177 (4)
P2—P3	2.181 (4)	P59—P60	2.187 (4)
P1—P3	2.164 (4)	P61—P63	2.170 (4)
P1—P4	2.167 (4)	P61—P64	2.177 (4)
P3—P4	2.176 (4)	P61—P62	2.178 (4)
P5—P7	2.171 (4)	P62—P64	2.144 (4)
P5—P8	2.180 (4)	P62—P63	2.158 (5)
P5—P6	2.182 (4)	P63—P64	2.141 (5)
P6—P8	2.177 (5)	P65—P68	2.176 (4)
P6—P7	2.177 (4)	P65—P67	2.178 (4)
P7—P8	2.184 (4)	P65—P66	2.182 (4)
P9—P12	2.158 (4)	P66—P67	2.171 (3)
P9—P11	2.176 (4)	P66—P68	2.180 (4)
P9—P10	2.179 (5)	P67—P68	2.173 (4)
P10—P12	2.177 (4)	P69—P70	2.176 (4)
P10—P11	2.181 (4)	P69—P72	2.178 (4)
P11—P12	2.168 (4)	P69—P71	2.181 (4)
P13—P15	2.137 (4)	P70—P72	2.170 (4)
P13—P16	2.174 (4)	P70—P71	2.177 (4)
P13—P14	2.183 (6)	P71—P72	2.185 (4)
P14—P15	2.121 (6)	P73—P74	2.153 (4)
P14—P16	2.148 (5)	P73—P75	2.162 (4)
P15—P16	2.111 (5)	P73—P76	2.180 (4)
P17—P19	2.167 (4)	P74—P75	2.179 (4)
P17—P20	2.174 (4)	P74—P76	2.188 (4)
P17—P18	2.178 (4)	P75—P76	2.174 (4)
P18—P20	2.167 (4)	P77—P78	2.137 (5)
P18—P19	2.178 (4)	P77—P80	2.159 (4)
P19—P20	2.162 (4)	P77—P79	2.161 (4)
P21—P22	2.162 (4)	P78—P79	2.158 (5)
P21—P24	2.166 (4)	P78—P80	2.166 (4)
P21—P23	2.171 (4)	P79—P80	2.176 (4)
P22—P24	2.168 (4)	P81—P83	2.140 (4)
P22—P23	2.174 (4)	P81—P84	2.162 (5)
P23—P24	2.162 (4)	P81—P82	2.169 (4)
P25—P28	2.165 (4)	P82—P84	2.176 (4)
P25—P27	2.165 (4)	P82—P83	2.178 (5)
P25—P26	2.175 (4)	P83—P84	2.170 (5)
P26—P28	2.184 (4)	P85—P88	2.165 (4)
P26—P27	2.189 (4)	P85—P87	2.181 (4)
P27—P28	2.170 (4)	P85—P86	2.191 (4)
P29—P30	2.176 (4)	P86—P87	2.184 (4)
P29—P32	2.176 (4)	P86—P88	2.187 (4)
P29—P31	2.183 (4)	P87—P88	2.172 (4)
P30—P32	2.180 (4)	P89—P92	2.167 (4)
P30—P31	2.181 (4)	P89—P90	2.169 (4)
P31—P32	2.177 (4)	P89—P91	2.180 (4)
P33—P35	2.173 (4)	P90—P92	2.168 (4)
P33—P36	2.179 (5)	P90—P91	2.176 (4)
P33—P34	2.183 (4)	P91—P92	2.161 (4)
P34—P35	2.180 (4)	P93—P94	2.130 (5)
P34—P36	2.193 (4)	P93—P95	2.150 (5)
P35—P36	2.166 (4)	P93—P96	2.158 (4)
P37—P38	2.150 (5)	P94—P95	2.153 (5)
P37—P39	2.154 (4)	P94—P96	2.176 (4)
P37—P40	2.180 (4)	P95—P96	2.185 (4)
P38—P39	2.152 (5)	P97—P100	2.169 (4)
P38—P40	2.160 (5)	P97—P98	2.170 (4)
P39—P40	2.159 (4)	P97—P99	2.180 (5)
P41—P43	2.159 (4)	P98—P100	2.134 (5)
P41—P42	2.171 (4)	P98—P99	2.138 (4)
P41—P44	2.186 (4)	P99—P100	2.143 (6)
P42—P43	2.171 (4)	P101—P103	2.173 (4)
P42—P44	2.176 (4)	P101—P104	2.174 (4)
P43—P44	2.180 (4)	P101—P102	2.175 (4)
P45—P48	2.167 (4)	P102—P103	2.161 (4)
P45—P46	2.180 (4)	P102—P104	2.180 (4)
P45—P47	2.198 (5)	P103—P104	2.150 (4)
P46—P48	2.170 (4)	P105—P107	2.165 (4)
P46—P47	2.188 (4)	P105—P106	2.170 (4)
P47—P48	2.174 (4)	P105—P108	2.177 (4)
P49—P51	2.131 (5)	P106—P107	2.169 (4)
P49—P52	2.148 (4)	P106—P108	2.181 (4)
P49—P50	2.165 (5)	P107—P108	2.190 (5)
P50—P51	2.119 (5)	P109—P112	2.143 (5)
P50—P52	2.145 (5)	P109—P111	2.153 (4)
P51—P52	2.168 (4)	P109—P110	2.157 (5)
P53—P56	2.148 (5)	P110—P112	2.148 (5)
P53—P54	2.165 (4)	P110—P111	2.163 (5)
P53—P55	2.174 (4)	P111—P112	2.161 (5)
P54—P56	2.148 (5)	P113—P115	2.159 (4)
P54—P55	2.166 (5)	P113—P116	2.165 (4)
P55—P56	2.145 (4)	P113—P114	2.170 (4)
P57—P59	2.159 (4)	P114—P115	2.180 (5)
P57—P58	2.162 (4)	P114—P116	2.181 (5)
P57—P60	2.169 (4)	P115—P116	2.191 (5)
P1—P2—P4	60.09 (13)	P57—P59—P58	59.87 (13)
P1—P2—P3	59.78 (14)	P57—P59—P60	59.85 (13)
P4—P2—P3	60.09 (14)	P58—P59—P60	59.89 (12)
P2—P1—P3	60.53 (14)	P57—P60—P58	59.68 (14)
P2—P1—P4	60.01 (13)	P57—P60—P59	59.43 (12)
P3—P1—P4	60.32 (13)	P58—P60—P59	59.74 (13)
P1—P3—P4	59.90 (13)	P63—P61—P64	59.01 (16)
P1—P3—P2	59.69 (14)	P63—P61—P62	59.52 (16)
P4—P3—P2	59.60 (13)	P64—P61—P62	58.98 (14)
P2—P4—P1	59.89 (13)	P64—P62—P63	59.69 (18)
P2—P4—P3	60.31 (14)	P64—P62—P61	60.48 (14)
P1—P4—P3	59.79 (13)	P63—P62—P61	60.04 (16)
P7—P5—P8	60.26 (13)	P64—P63—P62	59.83 (16)
P7—P5—P6	60.00 (13)	P64—P63—P61	60.66 (15)
P8—P5—P6	59.87 (14)	P62—P63—P61	60.43 (15)
P8—P6—P7	60.23 (14)	P63—P64—P62	60.49 (18)
P8—P6—P5	60.02 (15)	P63—P64—P61	60.32 (15)
P7—P6—P5	59.75 (14)	P62—P64—P61	60.54 (14)
P5—P7—P6	60.24 (14)	P68—P65—P67	59.87 (12)
P5—P7—P8	60.07 (14)	P68—P65—P66	60.05 (13)
P6—P7—P8	59.89 (15)	P67—P65—P66	59.72 (12)
P6—P8—P5	60.11 (15)	P67—P66—P68	59.92 (12)
P6—P8—P7	59.89 (14)	P67—P66—P65	60.06 (12)
P5—P8—P7	59.67 (14)	P68—P66—P65	59.85 (14)
P12—P9—P11	60.04 (13)	P66—P67—P68	60.26 (13)
P12—P9—P10	60.26 (16)	P66—P67—P65	60.21 (13)
P11—P9—P10	60.12 (13)	P68—P67—P65	60.01 (13)
P12—P10—P9	59.39 (15)	P67—P68—P65	60.12 (12)
P12—P10—P11	59.67 (14)	P67—P68—P66	59.82 (12)
P9—P10—P11	59.86 (14)	P65—P68—P66	60.10 (13)
P12—P11—P9	59.57 (14)	P70—P69—P72	59.80 (13)
P12—P11—P10	60.07 (14)	P70—P69—P71	59.98 (14)
P9—P11—P10	60.02 (16)	P72—P69—P71	60.18 (13)
P9—P12—P11	60.39 (14)	P72—P70—P69	60.14 (13)
P9—P12—P10	60.35 (15)	P72—P70—P71	60.35 (13)
P11—P12—P10	60.26 (14)	P69—P70—P71	60.13 (13)
P15—P13—P16	58.63 (16)	P70—P71—P69	59.89 (14)
P15—P13—P14	58.8 (2)	P70—P71—P72	59.66 (13)
P16—P13—P14	59.08 (17)	P69—P71—P72	59.84 (13)
P15—P14—P16	59.26 (19)	P70—P72—P69	60.05 (13)
P15—P14—P13	59.52 (16)	P70—P72—P71	59.99 (14)
P16—P14—P13	60.27 (18)	P69—P72—P71	59.98 (12)
P16—P15—P14	61.0 (2)	P74—P73—P75	60.67 (13)
P16—P15—P13	61.58 (16)	P74—P73—P76	60.65 (14)
P14—P15—P13	61.7 (2)	P75—P73—P76	60.09 (13)
P15—P16—P14	59.7 (2)	P73—P74—P75	59.87 (13)
P15—P16—P13	59.79 (16)	P73—P74—P76	60.29 (13)
P14—P16—P13	60.65 (17)	P75—P74—P76	59.71 (13)
P19—P17—P20	59.74 (13)	P73—P75—P76	60.37 (13)
P19—P17—P18	60.16 (14)	P73—P75—P74	59.46 (13)
P20—P17—P18	59.72 (13)	P76—P75—P74	60.35 (13)
P20—P18—P17	60.05 (13)	P75—P76—P73	59.54 (12)
P20—P18—P19	59.69 (14)	P75—P76—P74	59.95 (14)
P17—P18—P19	59.68 (13)	P73—P76—P74	59.06 (13)
P20—P19—P17	60.28 (13)	P78—P77—P80	60.56 (15)
P20—P19—P18	59.89 (13)	P78—P77—P79	60.28 (16)
P17—P19—P18	60.15 (14)	P80—P77—P79	60.51 (13)
P19—P20—P18	60.41 (15)	P77—P78—P79	60.40 (16)
P19—P20—P17	59.98 (13)	P77—P78—P80	60.21 (14)
P18—P20—P17	60.23 (13)	P79—P78—P80	60.43 (14)
P22—P21—P24	60.11 (13)	P78—P79—P77	59.32 (16)
P22—P21—P23	60.22 (14)	P78—P79—P80	59.97 (14)
P24—P21—P23	59.79 (15)	P77—P79—P80	59.70 (13)
P21—P22—P24	60.04 (14)	P77—P80—P78	59.23 (15)
P21—P22—P23	60.10 (14)	P77—P80—P79	59.79 (14)
P24—P22—P23	59.73 (14)	P78—P80—P79	59.60 (15)
P24—P23—P21	59.99 (15)	P83—P81—P84	60.59 (16)
P24—P23—P22	60.00 (13)	P83—P81—P82	60.71 (16)
P21—P23—P22	59.68 (13)	P84—P81—P82	60.32 (15)
P23—P24—P21	60.21 (14)	P81—P82—P84	59.67 (15)
P23—P24—P22	60.27 (14)	P81—P82—P83	58.98 (14)
P21—P24—P22	59.84 (13)	P84—P82—P83	59.79 (15)
P28—P25—P27	60.13 (14)	P81—P83—P84	60.20 (16)
P28—P25—P26	60.41 (15)	P81—P83—P82	60.31 (15)
P27—P25—P26	60.57 (15)	P84—P83—P82	60.06 (15)
P25—P26—P28	59.56 (14)	P81—P84—P83	59.22 (15)
P25—P26—P27	59.49 (14)	P81—P84—P82	60.02 (14)
P28—P26—P27	59.49 (14)	P83—P84—P82	60.15 (15)
P25—P27—P28	59.93 (14)	P88—P85—P87	59.97 (13)
P25—P27—P26	59.94 (15)	P88—P85—P86	60.26 (12)
P28—P27—P26	60.13 (14)	P87—P85—P86	59.94 (13)
P25—P28—P27	59.94 (14)	P87—P86—P88	59.59 (12)
P25—P28—P26	60.03 (15)	P87—P86—P85	59.79 (13)
P27—P28—P26	60.38 (14)	P88—P86—P85	59.26 (13)
P30—P29—P32	60.13 (13)	P88—P87—P85	59.65 (14)
P30—P29—P31	60.04 (12)	P88—P87—P86	60.27 (12)
P32—P29—P31	59.94 (13)	P85—P87—P86	60.28 (14)
P29—P30—P32	59.93 (13)	P85—P88—P87	60.38 (13)
P29—P30—P31	60.16 (12)	P85—P88—P86	60.48 (13)
P32—P30—P31	59.91 (12)	P87—P88—P86	60.15 (13)
P32—P31—P30	60.02 (13)	P92—P89—P90	60.01 (13)
P32—P31—P29	59.85 (13)	P92—P89—P91	59.63 (13)
P30—P31—P29	59.80 (12)	P90—P89—P91	60.04 (13)
P29—P32—P31	60.21 (13)	P92—P90—P89	59.95 (14)
P29—P32—P30	59.93 (13)	P92—P90—P91	59.67 (14)
P31—P32—P30	60.06 (13)	P89—P90—P91	60.23 (13)
P35—P33—P36	59.69 (14)	P92—P91—P90	59.99 (13)
P35—P33—P34	60.05 (14)	P92—P91—P89	59.88 (14)
P36—P33—P34	60.37 (14)	P90—P91—P89	59.73 (13)
P35—P34—P33	59.73 (14)	P91—P92—P89	60.49 (14)
P35—P34—P36	59.37 (13)	P91—P92—P90	60.34 (14)
P33—P34—P36	59.71 (15)	P89—P92—P90	60.04 (14)
P36—P35—P33	60.29 (15)	P94—P93—P95	60.40 (18)
P36—P35—P34	60.62 (14)	P94—P93—P96	60.97 (15)
P33—P35—P34	60.22 (14)	P95—P93—P96	60.96 (15)
P35—P36—P33	60.02 (15)	P93—P94—P95	60.26 (18)
P35—P36—P34	60.01 (14)	P93—P94—P96	60.15 (15)
P33—P36—P34	59.92 (14)	P95—P94—P96	60.64 (15)
P38—P37—P39	59.99 (18)	P93—P95—P94	59.33 (18)
P38—P37—P40	59.86 (16)	P93—P95—P96	59.69 (15)
P39—P37—P40	59.77 (14)	P94—P95—P96	60.19 (15)
P37—P38—P39	60.09 (16)	P93—P96—P94	58.88 (16)
P37—P38—P40	60.74 (16)	P93—P96—P95	59.34 (16)
P39—P38—P40	60.09 (17)	P94—P96—P95	59.18 (15)
P38—P39—P37	59.92 (18)	P100—P97—P98	58.93 (16)
P38—P39—P40	60.14 (17)	P100—P97—P99	59.03 (18)
P37—P39—P40	60.70 (14)	P98—P97—P99	58.88 (15)
P39—P40—P38	59.76 (17)	P100—P98—P99	60.2 (2)
P39—P40—P37	59.53 (14)	P100—P98—P97	60.52 (15)
P38—P40—P37	59.40 (16)	P99—P98—P97	60.80 (16)
P43—P41—P42	60.19 (13)	P98—P99—P100	59.82 (19)
P43—P41—P44	60.22 (13)	P98—P99—P97	60.32 (15)
P42—P41—P44	59.94 (13)	P100—P99—P97	60.23 (17)
P41—P42—P43	59.65 (13)	P98—P100—P99	59.98 (17)
P41—P42—P44	60.38 (14)	P98—P100—P97	60.55 (15)
P43—P42—P44	60.19 (12)	P99—P100—P97	60.74 (16)
P41—P43—P42	60.16 (13)	P103—P101—P104	59.28 (14)
P41—P43—P44	60.49 (14)	P103—P101—P102	59.62 (13)
P42—P43—P44	60.02 (13)	P104—P101—P102	60.16 (13)
P42—P44—P43	59.79 (13)	P103—P102—P101	60.17 (13)
P42—P44—P41	59.68 (13)	P103—P102—P104	59.38 (14)
P43—P44—P41	59.29 (14)	P101—P102—P104	59.92 (13)
P48—P45—P46	59.88 (14)	P104—P103—P102	60.74 (14)
P48—P45—P47	59.74 (15)	P104—P103—P101	60.38 (14)
P46—P45—P47	59.97 (14)	P102—P103—P101	60.22 (13)
P48—P46—P45	59.75 (14)	P103—P104—P101	60.34 (14)
P48—P46—P47	59.85 (14)	P103—P104—P102	59.88 (13)
P45—P46—P47	60.41 (15)	P101—P104—P102	59.92 (13)
P48—P47—P46	59.65 (14)	P107—P105—P106	60.05 (14)
P48—P47—P45	59.42 (15)	P107—P105—P108	60.59 (15)
P46—P47—P45	59.62 (14)	P106—P105—P108	60.24 (12)
P45—P48—P46	60.37 (14)	P107—P106—P105	59.87 (13)
P45—P48—P47	60.84 (16)	P107—P106—P108	60.46 (15)
P46—P48—P47	60.50 (15)	P105—P106—P108	60.04 (13)
P51—P49—P52	60.88 (15)	P105—P107—P106	60.08 (14)
P51—P49—P50	59.09 (17)	P105—P107—P108	59.97 (14)
P52—P49—P50	59.65 (16)	P106—P107—P108	60.04 (14)
P51—P50—P52	61.11 (16)	P105—P108—P106	59.72 (13)
P51—P50—P49	59.64 (18)	P105—P108—P107	59.44 (13)
P52—P50—P49	59.78 (16)	P106—P108—P107	59.49 (14)
P50—P51—P49	61.3 (2)	P112—P109—P111	60.39 (17)
P50—P51—P52	60.05 (16)	P112—P109—P110	59.94 (19)
P49—P51—P52	59.96 (15)	P111—P109—P110	60.26 (16)
P50—P52—P49	60.57 (18)	P112—P110—P109	59.72 (17)
P50—P52—P51	58.84 (16)	P112—P110—P111	60.16 (17)
P49—P52—P51	59.16 (16)	P109—P110—P111	59.79 (15)
P56—P53—P54	59.76 (16)	P109—P111—P112	59.58 (17)
P56—P53—P55	59.51 (14)	P109—P111—P110	59.96 (16)
P54—P53—P55	59.90 (15)	P112—P111—P110	59.58 (18)
P56—P54—P53	59.72 (15)	P109—P112—P110	60.34 (18)
P56—P54—P55	59.62 (14)	P109—P112—P111	60.02 (16)
P53—P54—P55	60.25 (14)	P110—P112—P111	60.27 (17)
P56—P55—P54	59.78 (16)	P115—P113—P116	60.89 (16)
P56—P55—P53	59.64 (15)	P115—P113—P114	60.46 (16)
P54—P55—P53	59.85 (15)	P116—P113—P114	60.39 (16)
P55—P56—P53	60.85 (15)	P113—P114—P115	59.52 (15)
P55—P56—P54	60.60 (17)	P113—P114—P116	59.69 (15)
P53—P56—P54	60.52 (16)	P115—P114—P116	60.33 (16)
P59—P57—P58	60.39 (14)	P113—P115—P114	60.01 (15)
P59—P57—P60	60.71 (13)	P113—P115—P116	59.68 (15)
P58—P57—P60	60.34 (13)	P114—P115—P116	59.85 (16)
P57—P58—P59	59.74 (13)	P113—P116—P114	59.92 (15)
P57—P58—P60	59.97 (14)	P113—P116—P115	59.43 (15)
P59—P58—P60	60.37 (13)	P114—P116—P115	59.82 (16)

 

Footnotes

¹The cell parameters are nearly identical to the structure refined in P2/n with P₂₁ in the asymmetric unit by Zhang et al. (2020) and hence to Thurn & Krebs (1969). The data quality of Cicirello et al. (2023) is very poor. In the Checkcif report there are several A alerts, e.g. no anisotropic refinement, max residual density of 4.65 e Å⁻³, wR2 = 0.49. It is possible to refine the coordinates of the structure deposited by Zhang et al. (2020) against the data deposited by Cicirello et al. (2023). Of course, half of the data are then missing and 5 of the 21 P atoms adopt negative U_iso values. However, wR2 reaches 0.29 and the highest residual density is 2.09 e Å⁻³. Therefore, there is reasonable doubt whether this is really a new structure and whether P₁₁ is indeed the content of the asymmetric unit, rather than P₂₁ as in the original structure by Thurn & Krebs (1969).