Bis(tetra-n-butylammonium) (a redetermination at 150 K) and bis(tetraphenylarsonium) bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II) (at 300 K)

The title compounds are salts of the general form (Q⁺)₂[Zn(dmit)₂]^2-, where dmit corresponds to the ligand (C₃S₅)^- present in both and Q⁺ to the counter-cations (ⁿBu₄N)⁺ [or C₁₆H₃₆N⁺] and (Ph₄As)⁺ [or C₂₄H₂₀As⁺], respectively. In the first case, Zn is in the 4e special positions of space group C2/c and hence the [Zn(dmit)₂]^2- dianion possesses twofold axial crystallographic symmetry. Including these, there are now 11 known examples of [Zn(dmit)₂]^2- or its analogues, with O replacing the exocyclic thione S, and [Zn(dmio)₂]^2- dianions in nine structures with various Q. Comparison of these reveals a remarkable variation in details of the conformation which the dianion may adopt in terms of Zn coordination, equivalence of the Zn-S bond lengths, displacement of Zn from the plane of the ligand and overall dianion shape.

S1. Comment

Chohan et al. (1997) and Harrison et al. (2000) and references therein have already pointed out the importance of onium salts of the [Zn(dmit)₂]^2- dianion, where dmit is the 1,3-dithiole-2-thione-4,5-dithiolato ligand, as stable and convenient precursors for the formation of complexes with other transition and main group metal elements and the synthesis of heterocyclic compounds. Müller et al. (1998) concur with this view and show that it is equally applicable to the analogous [Zn(dmio)₂]^2- dianion, where dmio is the 1,3-dithiole-2-one-4,5-dithiolato ligand i.e. with O now replacing the thione S of dmit. Müller et al. however use the acronym 'dmid' rather than 'dmio' used here.

The [Zn(dmit)₂]^2- dianions of the title compounds, Q = ⁿBu₄N at 150 K, IV(150), Fig. 1 and Table 1, and Q = Ph₄As, IX, Fig. 2 and Table 2, are as anticipated for this type of species although the twofold axial crystallographic symmetry of the dianion in IV(150) is a notable but not unusual feature. As a result whereas the asymmetric unit of IX consists of a complete dianion and two distinct Ph₄As counter cations that of IV(150) contains Zn, one complete dmit ligand and only a single cation. Aside from a degree of disorder affecting two of the ⁿBu groups in IV(150) the counter-cations are unremarkable and are not discussed further.

The results for IV(150) and IX can be compared, Table 3, with a series of previously known related structures as Chohan et al. (1997) and Harrison et al. (2000) have already done but now focused upon the shape of the dianions rather than details of their internal geometry and the sometime presence of S.·S inter-anion contacts. Certain conventions are noted here which have been adopted in the creation of Table 3. First in the calculation of out of plane Zn and exocyclic thione S for dmit and O for dmio distances, Zn_op and one_op respectively, the reference ligand plane has been defined by the C═C bond and the four S attached to it e.g. S1, S2, C1, C2, S3 and S4 in Figs. 1 and 2 or their equivalent. Second in order that the angle IP may be used as a measure of the flattening of the tetrahedral coordination of Zn it is defined as the angle between the plane defined by Zn1, S1 and S2 and that defined by Zn1, S6 and S7 as in Fig. 2. This usage avoids complications which would be induced by Zn out of plane distances if the ligand planes as defined first above were used for this purpose. The angle L, calculated as X—Zn—X' where X and X' are exocyclic thione S or, for dmio, O e.g. S5—Zn1—S10 in Fig. 2 is used as a measure of the non-linear or V-shaped nature of the dianions. The entries in the table are in order of decreasing L which is also wholly compatible with the dianions ordered in categories according to their crystallographic symmetry which decreases down the list.

The values given in Table 3 give rise to some general observations. First the ligand bite angles show little variation and fall in the comparatively narrow range 93.44 (10) to 95.22 (4)° and have, therefore, virtually no effect on the variation in the shape of the dianions. In all but two cases, both ligands of I by symmetry and fortuitously the second ligand of IX, the bidentate ligands coordinate in an asymmetric manner contributing therefore to the variation in L. L is clearly affected primarily by variation of Zn_op and to a lesser extent by one_op in which the variation is less and essentially random in nature. The primary significance of one_op is its relationship to Zn_op. If these have the same or different signs the chelate formed by the ligand is overall boat or Z shaped respectively with displacement of Zn and thione S or, for dmio, O from the chelate mean plane in both cases.

In terms of crystallographic symmetry the dianions of the compounds presented in Table 3 occur in three groups. Group 1 has I as the only representative. This is the most constrained situation and here the dianion is subject to the operation of a crystallographic twofold axis running along its length and passing through Zn and C and S of the thione groups. As a consequence the ligands coordinate in a symmetric manner, Zn and thione S are rigorously confined to the ligand planes and the dianion is strictly linear from one thione S to the other. Here, however, is found by far the lowest value of IP, 69.29 (12)°, corresponding to the most flattened form of tetrahedral coordination of Zn in the series.

In group 2, with compounds II to V providing 5 cases, the dianions are again subject to the operation of a crystallographic twofold axis but now perpendicular to the length of the ligand. Now, as for group 3 excepting the second ligand of IX, the ligands coordinate in an asymmetric manner and contribute to the non-linearity of the dianions with L now in the range 171.05 (8) to 177.86 (3)°. Within the group the values of L indicate the existence of two subgroups as II and III together with smallest Zn_op and L = 177.86 (3) and 177.04 (4) respectively and III to V with greater Zn_op and smaller L. IP now in the range 81.18 (6) to 83.58 (9)° indicates a much less flattened coordination of Zn than before.

The dianions of group 3, VI to IX and again 5 cases, are totally free from constraint by symmetry. These display the least linearity with L in the range 158.51 (2) to 169.49 (1)° and still less flattened Zn coordination with IP in the range 82.47 (4) to 89.25 (18)° which last is close to the ideal of 90°. Noticeable here is the special situation of IX with the smallest value of L where Zn is similarly greatly displaced from the planes of both ligands whereas in VI to VIII the Zn displacement is much greater for one ligand than the other.

It is clear that the linearity of the dianions, L, correlates not only with their classification in terms of crystallographic symmetry but also, because of the manner in which it is calculated, with the values of Zn_op. The flattening of the tetrahedral Zn coordination, IP, on the other hand, relates to the crystallographic dianion symmetry solely in terms of ranges of values and correlates with no other entries in the table. L and IP are in any case crude measures of completely different aspects of the shape of the dianions and no relationship between them is therefore expected. Any relationship between the nature of the counter cations and the shape of the dianions is at best superficial and supported by nothing more than I, methanol solvate with Q = Et₄N, at one extreme, IX with bulky Q = Ph₄As at the other and species as IV with Q = ⁿBu₄N in between. However VI, Q = Ph₄P DMSO solvate, and particularly VIII, Q = Et₄N, are anomolous in terms of the predicated series. This implies that the size of the counter cations probably determines the shape of the dianions only in combination with several other factors such as counter cation shape, the presence of solvent molecules and the presence of short inter-anion S.·S contacts, less than the sum of the van der Waals radii, which do not in fact occur in either IV or IX.

S2. Experimental

The salt, IV or IX, was prepared following a general procedure (Valade et al. 1985) from Na₂dmit, ZnSO₄ and ⁿBu₄NBr or Ph₄AsCl. Red crystals of IV were obtained from Me₂CO/2-propanol, m.p. 436–438 K. IR (KBr): 1411 (C═C), 1055 (C═S), 889 (C—S) cm^-1. Uv-vis (MeCN): 499 and 308 nm. Red crystals of IX were obtained from DMSO, m.p. 478–481 K. IR (KBr): 1437 (C═C), 1056 (C═S), 888 (C—S) cm^-1. Uv-vis (MeCN): 497 and 311 nm.

S3. Refinement

In the course of the refinement of IV(150) severe disorder of the terminal methylene, C10 and C14, and methyl groups, C11 and C15, of two of the ⁿBu groups of the ⁿBu₄N counter cation became apparent necessitating the splitting of each of these atoms over two sites of equal occupancy distinguished by suffix A or B. In addition constraints as 1.52 (1) and 2.48 (1) Å for direct C—C bonds and C—C—C angle defining C.·C contacts respectively were applied to the refinement of the disordered species, 16 constraints in all. Even then the need for further splitting of C14B and C15A was indicated but was not implemented. In the final stages of refinement H atoms were introduced in calculated positions and refined with a riding model with C—H 0.99 and 0.98 Å and U_iso 1.2 and 1.5U_eq of the C to which H are attached for the methylene and methyl H atoms respectively of IV(150) and with C—H 0.93 and U_iso 1.2U_eq for the phenyl H atoms of IX. Rotation parameters were refined for the methyl groups as rigid bodies of ordered C8 and C19 of IX but not for the remainder.

Computing details

Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998) for IV150; SMART (Bruker, 1999) for (IX). Cell refinement: DENZO and COLLECT for IV150; SAINT (Bruker, 1999) for (IX). Data reduction: DENZO and COLLECT for IV150; SAINT (Bruker, 1999) for (IX). For both compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures

Figure 1. The dianion of IV(150) showing atom labels. Atoms are shown as 50% probability ellipsoids. Figure 2. The dianion of IX. The representation is the same as in Fig. 1. #The captions below and the drawings to which they refer, Supp. 1–4, are not #intended for publication. They are merely provided for the convenience of #editors and referees. The representation is the same as for Figs. 1 and 2 #except for H atoms which are shown as small open circles in Supps. 1 and 2 #and have been omitted for clarity in Supps. 3 and 4. #Supp. 1. The cation of IV(150) displaying the disordered element comprising #C10A, C11A, C14A and C15A. #Supp. 2. The cation of IV(150) now showing C10B, C11B, C14B and C15B. #Supp. 3. Cation 1 of IX. #Supp. 4. Cation 2 of IX.

(IV150) Bis(tetra-n-butylammonium) bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II) at 150 K

Crystal data

(C6S10Zn^2^−)·2(C16H36N^+)	Dx = 1.245 Mg m^−3
Mr = 942.95	Melting point = 436–438 K
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 19.2564 (3) Å	Cell parameters from 22851 reflections
b = 8.9478 (2) Å	θ = 3.2–28.6°
c = 29.2379 (5) Å	µ = 0.93 mm^−1
β = 92.9544 (7)°	T = 150 K
V = 5031.06 (16) Å^3	Block, red
Z = 4	0.25 × 0.22 × 0.10 mm
F(000) = 2016

Data collection

Enraf Nonius KappaCCD area detector diffractometer	5525 independent reflections
Radiation source: Enraf Nonius FR591 rotating anode	2563 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.061
Detector resolution: 9.091 pixels mm^-1	θmax = 28.6°, θmin = 3.2°
ϕ and ω scans to fill the Ewald sphere	h = −25→23
Absorption correction: multi-scan (SORTAV; Blessing, 1995, 1997)	k = −9→11
Tmin = 0.770, Tmax = 0.859	l = −37→39
22851 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.132	H-atom parameters constrained
S = 0.98	w = 1/[σ^2(Fo^2) + (0.0614P)^2] where P = (Fo^2 + 2Fc^2)/3
5525 reflections	(Δ/σ)max < 0.001
269 parameters	Δρmax = 0.23 e Å^−3
16 restraints	Δρmin = −0.20 e Å^−3

Special details

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

Because of the manner in which the disordered atoms have been treated (see above) the following angles involving atoms of different PART's have been discarded. C10A C9 C10B 33.5 (6).. ?; C10B C9 H9A 89.0.. ?; C10B C9 H9B 140.9.. ?; C10A C9 H9C 78.5.. ?; H9A C9 H9C 130.4.. ?; H9B C9 H9C 32.2.. ?; C10A C9 H9D 121.1.. ?; H9A C9 H9D 25.0.. ?; H9B C9 H9D 82.5.. ?; C14A C13 C14B 29.6 (4).. ?; C14B C13 H13A 136.9.. ?; C14B C13 H13B 91.4.. ?; C14A C13 H13C 120.0.. ?; H13A C13 H13C 85.1.. ?; H13B C13 H13C 22.4.. ?; C14A C13 H13D 81.8.. ?; H13A C13 H13D 28.7.. ?; H13B C13 H13D 128.4.. ?; C10B C9 C10A C11A 14.1 (15).. . . ?; C10A C9 C10B C11B -26.4 (10).. . . ?; C14B C13 C14A C15A -1.5 (12).. . . ?; C14A C13 C14B C15B 52.8 (13).. . . ?.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Anisotropic refinement of all non-H. Serious disorder of C10, C11, C14 and C15 for the most part dealt with in terms of atom pairs in different PART's but further possible splitting of already split atoms not applied.

H in calculated positions and refined with a riding model. Methyl group rigid body rotation for split methyl groups C11 and C15 not refined.

Within SHELXL97 the disordered species which are 4 in number, because of the manner in which the PART instructions have been used, are coded internally as:

C9/H9A_a/H9B_a-C10_a/H10A_a/H10B_a-C11_a/H11A_a/H11B_a/H11C_a

C9/H9C_b/H9D_b-C10_b/H10C_b/H10D_b-C11_b/H11D_b/H11E_b/H11F_b

C13/H13A_a/H13B_a-C14_a/H14A_a/H14B_a-C15_a/H15A_a/H15B_a/H15C_a

and

C13/H13C_b/H13D_b-C14_b/H14C_b/H14D_b-C15_b/H15D_b/H15E_b/H15F_b

but the suffices 'a' and 'b' which correspond to the PART nos. 1 and 2 set up in the input data do not appear in the cif finally produced. This does not matter for the H atoms which are rendered distinct by the choice of suffices as A, B ··· etc in any case but results in pairwise replication of atom labels for the split C atoms. Manual intervention has therefore been applied in all cases in the loops below where the replicate labels appeared originally to install, for example, C10A where C10_a would have appeared and so on for the remaining split C atoms.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Zn1	0.5000	0.07195 (6)	0.2500	0.0810 (2)
S1	0.49898 (4)	−0.05345 (10)	0.18009 (3)	0.0868 (3)
S2	0.39523 (5)	0.19862 (11)	0.23401 (3)	0.0944 (3)
C1	0.42446 (16)	0.0334 (4)	0.15742 (10)	0.0752 (8)
C2	0.38302 (17)	0.1293 (4)	0.17908 (11)	0.0775 (9)
S3	0.39837 (5)	−0.00687 (11)	0.10064 (3)	0.0920 (3)
S4	0.30907 (5)	0.18760 (12)	0.14666 (3)	0.0992 (3)
C3	0.32301 (18)	0.0963 (4)	0.09618 (12)	0.0919 (10)
S5	0.27099 (6)	0.10584 (15)	0.04999 (4)	0.1263 (4)
N1	0.20341 (16)	0.6561 (3)	0.12021 (10)	0.0932 (8)
C4	0.1601 (2)	0.7962 (4)	0.11474 (13)	0.1090 (12)
H4A	0.1913	0.8834	0.1196	0.131*
H4B	0.1409	0.8008	0.0827	0.131*
C5	0.1012 (2)	0.8118 (5)	0.14589 (15)	0.1211 (14)
H5A	0.1193	0.8092	0.1782	0.145*
H5B	0.0684	0.7273	0.1409	0.145*
C6	0.0631 (3)	0.9597 (6)	0.13621 (18)	0.1482 (18)
H6A	0.0965	1.0430	0.1410	0.178*
H6B	0.0461	0.9615	0.1037	0.178*
C7	0.0028 (3)	0.9845 (6)	0.1657 (2)	0.168 (2)
H7A	−0.0316	0.9049	0.1602	0.252*
H7B	−0.0187	1.0814	0.1583	0.252*
H7C	0.0191	0.9833	0.1980	0.252*
C8	0.2357 (2)	0.6398 (5)	0.16769 (13)	0.1128 (13)
H8A	0.1977	0.6276	0.1889	0.135*
H8B	0.2631	0.5461	0.1688	0.135*
C9	0.2813 (3)	0.7618 (7)	0.18532 (16)	0.160 (2)
H9A	0.3248	0.7573	0.1688	0.192*	0.50
H9B	0.2583	0.8576	0.1769	0.192*	0.50
H9C	0.2541	0.8489	0.1952	0.192*	0.50
H9D	0.3142	0.7943	0.1623	0.192*	0.50
C10A	0.3007 (5)	0.7674 (15)	0.2346 (3)	0.149 (6)	0.50
H10A	0.2588	0.7477	0.2519	0.179*	0.50
H10B	0.3172	0.8694	0.2425	0.179*	0.50
C11A	0.3551 (9)	0.6591 (16)	0.2489 (5)	0.191 (6)	0.50
H11A	0.3574	0.6500	0.2823	0.286*	0.50
H11B	0.4001	0.6938	0.2388	0.286*	0.50
H11C	0.3441	0.5616	0.2351	0.286*	0.50
C10B	0.3214 (9)	0.6789 (13)	0.2287 (4)	0.190 (8)	0.50
H10C	0.2899	0.6062	0.2425	0.228*	0.50
H10D	0.3624	0.6241	0.2184	0.228*	0.50
C11B	0.3429 (8)	0.7890 (14)	0.2617 (3)	0.176 (5)	0.50
H11D	0.3610	0.7396	0.2897	0.263*	0.50
H11E	0.3031	0.8518	0.2686	0.263*	0.50
H11F	0.3794	0.8513	0.2493	0.263*	0.50
C12	0.2588 (2)	0.6719 (5)	0.08502 (13)	0.1107 (13)
H12A	0.2350	0.6848	0.0544	0.133*
H12B	0.2854	0.7645	0.0919	0.133*
C13	0.3090 (2)	0.5462 (6)	0.08235 (14)	0.1254 (15)
H13A	0.3188	0.5087	0.1139	0.150*	0.50
H13B	0.2852	0.4646	0.0648	0.150*	0.50
H13C	0.2845	0.4499	0.0771	0.150*	0.50
H13D	0.3392	0.5390	0.1107	0.150*	0.50
C14A	0.3766 (4)	0.5730 (15)	0.0618 (3)	0.133 (5)	0.50
H14A	0.4012	0.6552	0.0786	0.160*	0.50
H14B	0.4056	0.4820	0.0654	0.160*	0.50
C15A	0.3695 (8)	0.611 (2)	0.0141 (3)	0.212 (8)	0.50
H15A	0.4098	0.6700	0.0057	0.319*	0.50
H15B	0.3269	0.6698	0.0083	0.319*	0.50
H15C	0.3667	0.5194	−0.0043	0.319*	0.50
C14B	0.3532 (4)	0.5907 (12)	0.0390 (3)	0.110 (4)	0.50
H14C	0.3225	0.5983	0.0109	0.132*	0.50
H14D	0.3770	0.6877	0.0443	0.132*	0.50
C15B	0.4053 (5)	0.4677 (11)	0.0346 (4)	0.150 (4)	0.50
H15D	0.4366	0.4928	0.0103	0.224*	0.50
H15E	0.3809	0.3742	0.0269	0.224*	0.50
H15F	0.4323	0.4557	0.0637	0.224*	0.50
C16	0.1602 (2)	0.5160 (4)	0.11141 (14)	0.1012 (12)
H16A	0.1918	0.4289	0.1144	0.121*
H16B	0.1270	0.5079	0.1360	0.121*
C17	0.1196 (2)	0.5027 (5)	0.06635 (16)	0.1237 (14)
H17A	0.1506	0.5182	0.0408	0.148*
H17B	0.0824	0.5791	0.0641	0.148*
C18	0.0871 (3)	0.3416 (6)	0.06367 (19)	0.1397 (17)
H18A	0.1251	0.2670	0.0646	0.168*
H18B	0.0595	0.3252	0.0908	0.168*
C19	0.0432 (4)	0.3186 (9)	0.0228 (3)	0.222 (3)
H19A	0.0095	0.4003	0.0195	0.332*
H19B	0.0185	0.2233	0.0252	0.332*
H19C	0.0719	0.3164	−0.0039	0.332*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0799 (4)	0.0872 (4)	0.0775 (4)	0.000	0.0190 (3)	0.000
S1	0.0774 (6)	0.0939 (7)	0.0910 (6)	0.0070 (5)	0.0227 (4)	−0.0136 (5)
S2	0.1002 (7)	0.1023 (7)	0.0819 (6)	0.0231 (5)	0.0164 (5)	−0.0131 (5)
C1	0.077 (2)	0.073 (2)	0.0767 (19)	−0.0117 (17)	0.0167 (16)	−0.0009 (16)
C2	0.079 (2)	0.076 (2)	0.079 (2)	0.0013 (18)	0.0151 (17)	0.0012 (16)
S3	0.0922 (6)	0.1015 (7)	0.0837 (6)	−0.0143 (5)	0.0173 (5)	−0.0163 (5)
S4	0.0998 (7)	0.1026 (7)	0.0952 (6)	0.0175 (6)	0.0052 (5)	0.0021 (5)
C3	0.095 (2)	0.090 (3)	0.091 (2)	−0.018 (2)	0.0105 (19)	0.0041 (19)
S5	0.1238 (9)	0.1489 (11)	0.1038 (8)	−0.0100 (8)	−0.0178 (7)	0.0035 (7)
N1	0.106 (2)	0.088 (2)	0.088 (2)	−0.0018 (18)	0.0307 (16)	0.0126 (16)
C4	0.145 (3)	0.082 (3)	0.103 (3)	−0.001 (2)	0.034 (3)	0.018 (2)
C5	0.135 (3)	0.106 (3)	0.124 (3)	0.013 (3)	0.028 (3)	0.029 (3)
C6	0.160 (4)	0.117 (4)	0.171 (5)	0.031 (3)	0.039 (4)	0.034 (3)
C7	0.174 (5)	0.133 (4)	0.202 (6)	0.032 (4)	0.061 (4)	0.021 (4)
C8	0.117 (3)	0.138 (4)	0.086 (3)	0.000 (3)	0.029 (2)	0.022 (2)
C9	0.157 (5)	0.217 (6)	0.107 (4)	−0.042 (4)	0.014 (3)	−0.027 (4)
C10A	0.080 (6)	0.209 (16)	0.161 (13)	−0.016 (8)	0.028 (7)	−0.068 (11)
C11A	0.236 (18)	0.170 (13)	0.157 (13)	0.018 (12)	−0.079 (11)	0.018 (10)
C10B	0.26 (2)	0.195 (16)	0.104 (10)	0.075 (13)	−0.070 (11)	−0.040 (9)
C11B	0.185 (13)	0.134 (11)	0.209 (15)	−0.048 (10)	0.023 (11)	−0.018 (10)
C12	0.125 (3)	0.118 (3)	0.093 (2)	−0.037 (3)	0.043 (2)	0.007 (2)
C13	0.111 (3)	0.144 (4)	0.126 (3)	−0.026 (3)	0.055 (3)	−0.015 (3)
C14A	0.174 (11)	0.147 (9)	0.080 (7)	−0.014 (8)	0.023 (7)	−0.023 (8)
C15A	0.233 (16)	0.33 (2)	0.077 (8)	−0.117 (15)	0.017 (8)	−0.003 (10)
C14B	0.132 (8)	0.159 (9)	0.042 (6)	−0.065 (7)	0.033 (6)	−0.029 (7)
C15B	0.133 (8)	0.170 (10)	0.152 (10)	−0.030 (7)	0.075 (8)	−0.046 (8)
C16	0.098 (3)	0.089 (3)	0.120 (3)	−0.001 (2)	0.042 (2)	0.019 (2)
C17	0.118 (3)	0.115 (4)	0.139 (4)	−0.005 (3)	0.023 (3)	0.001 (3)
C18	0.137 (4)	0.134 (4)	0.152 (4)	−0.018 (3)	0.041 (3)	−0.027 (3)
C19	0.206 (7)	0.237 (8)	0.227 (8)	−0.074 (6)	0.057 (6)	−0.051 (6)

Geometric parameters (Å, º)

Zn1—S1	2.3308 (9)	C11A—H11B	0.9800
Zn1—S1^i	2.3308 (9)	C11A—H11C	0.9800
Zn1—S2^i	2.3401 (10)	C10B—C11B	1.424 (9)
Zn1—S2	2.3401 (10)	C10B—H10C	0.9900
S1—C1	1.733 (3)	C10B—H10D	0.9900
S2—C2	1.726 (3)	C11B—H11D	0.9800
C1—C2	1.351 (4)	C11B—H11E	0.9800
C1—S3	1.747 (3)	C11B—H11F	0.9800
C2—S4	1.749 (3)	C12—C13	1.487 (6)
S3—C3	1.719 (4)	C12—H12A	0.9900
S4—C3	1.720 (4)	C12—H12B	0.9900
C3—S5	1.642 (4)	C13—C14A	1.483 (7)
N1—C8	1.498 (5)	C13—C14B	1.613 (7)
N1—C4	1.509 (5)	C13—H13A	0.9900
N1—C16	1.520 (5)	C13—H13B	0.9900
N1—C12	1.526 (4)	C13—H13C	0.9900
C4—C5	1.498 (5)	C13—H13D	0.9900
C4—H4A	0.9900	C14A—C15A	1.435 (8)
C4—H4B	0.9900	C14A—H14A	0.9900
C5—C6	1.532 (6)	C14A—H14B	0.9900
C5—H5A	0.9900	C15A—H15A	0.9800
C5—H5B	0.9900	C15A—H15B	0.9800
C6—C7	1.499 (6)	C15A—H15C	0.9800
C6—H6A	0.9900	C14B—C15B	1.498 (9)
C6—H6B	0.9900	C14B—H14C	0.9900
C7—H7A	0.9800	C14B—H14D	0.9900
C7—H7B	0.9800	C15B—H15D	0.9800
C7—H7C	0.9800	C15B—H15E	0.9800
C8—C9	1.478 (6)	C15B—H15F	0.9800
C8—H8A	0.9900	C16—C17	1.501 (5)
C8—H8B	0.9900	C16—H16A	0.9900
C9—C10A	1.469 (8)	C16—H16B	0.9900
C9—C10B	1.629 (8)	C17—C18	1.571 (6)
C9—H9A	0.9900	C17—H17A	0.9900
C9—H9B	0.9900	C17—H17B	0.9900
C9—H9C	0.9900	C18—C19	1.442 (8)
C9—H9D	0.9900	C18—H18A	0.9900
C10A—C11A	1.473 (9)	C18—H18B	0.9900
C10A—H10A	0.9900	C19—H19A	0.9800
C10A—H10B	0.9900	C19—H19B	0.9800
C11A—H11A	0.9800	C19—H19C	0.9800
S1—Zn1—S1^i	122.45 (5)	C11B—C10B—C9	108.8 (9)
S1—Zn1—S2^i	112.12 (3)	C11B—C10B—H10C	109.9
S1^i—Zn1—S2^i	95.15 (3)	C9—C10B—H10C	109.9
S1—Zn1—S2	95.15 (3)	C11B—C10B—H10D	109.9
S1^i—Zn1—S2	112.12 (3)	C9—C10B—H10D	109.9
S2^i—Zn1—S2	122.06 (6)	H10C—C10B—H10D	108.3
C1—S1—Zn1	95.11 (11)	C10B—C11B—H11D	109.5
C2—S2—Zn1	94.97 (11)	C10B—C11B—H11E	109.5
C2—C1—S1	127.1 (2)	H11D—C11B—H11E	109.5
C2—C1—S3	115.4 (3)	C10B—C11B—H11F	109.5
S1—C1—S3	117.58 (19)	H11D—C11B—H11F	109.5
C1—C2—S2	127.5 (3)	H11E—C11B—H11F	109.5
C1—C2—S4	114.8 (2)	C13—C12—N1	116.3 (3)
S2—C2—S4	117.71 (19)	C13—C12—H12A	108.2
C3—S3—C1	99.30 (16)	N1—C12—H12A	108.2
C3—S4—C2	99.48 (17)	C13—C12—H12B	108.2
S5—C3—S3	124.5 (2)	N1—C12—H12B	108.2
S5—C3—S4	124.5 (2)	H12A—C12—H12B	107.4
S3—C3—S4	111.0 (2)	C14A—C13—C12	119.1 (6)
C8—N1—C4	112.3 (3)	C12—C13—C14B	103.1 (4)
C8—N1—C16	105.9 (3)	C14A—C13—H13A	107.6
C4—N1—C16	111.9 (3)	C12—C13—H13A	107.6
C8—N1—C12	111.3 (3)	C14A—C13—H13B	107.6
C4—N1—C12	104.6 (3)	C12—C13—H13B	107.6
C16—N1—C12	111.0 (3)	H13A—C13—H13B	107.0
C5—C4—N1	116.4 (3)	C12—C13—H13C	111.2
C5—C4—H4A	108.2	C14B—C13—H13C	111.2
N1—C4—H4A	108.2	C12—C13—H13D	111.2
C5—C4—H4B	108.2	C14B—C13—H13D	111.2
N1—C4—H4B	108.2	H13C—C13—H13D	109.1
H4A—C4—H4B	107.3	C15A—C14A—C13	112.9 (8)
C4—C5—C6	109.8 (3)	C15A—C14A—H14A	109.0
C4—C5—H5A	109.7	C13—C14A—H14A	109.0
C6—C5—H5A	109.7	C15A—C14A—H14B	109.0
C4—C5—H5B	109.7	C13—C14A—H14B	109.0
C6—C5—H5B	109.7	H14A—C14A—H14B	107.8
H5A—C5—H5B	108.2	C14A—C15A—H15A	109.5
C7—C6—C5	113.5 (4)	C14A—C15A—H15B	109.5
C7—C6—H6A	108.9	H15A—C15A—H15B	109.5
C5—C6—H6A	108.9	C14A—C15A—H15C	109.5
C7—C6—H6B	108.9	H15A—C15A—H15C	109.5
C5—C6—H6B	108.9	H15B—C15A—H15C	109.5
H6A—C6—H6B	107.7	C15B—C14B—C13	105.6 (7)
C6—C7—H7A	109.5	C15B—C14B—H14C	110.6
C6—C7—H7B	109.5	C13—C14B—H14C	110.6
H7A—C7—H7B	109.5	C15B—C14B—H14D	110.6
C6—C7—H7C	109.5	C13—C14B—H14D	110.6
H7A—C7—H7C	109.5	H14C—C14B—H14D	108.7
H7B—C7—H7C	109.5	C14B—C15B—H15D	109.5
C9—C8—N1	117.5 (4)	C14B—C15B—H15E	109.5
C9—C8—H8A	107.9	H15D—C15B—H15E	109.5
N1—C8—H8A	107.9	C14B—C15B—H15F	109.5
C9—C8—H8B	107.9	H15D—C15B—H15F	109.5
N1—C8—H8B	107.9	H15E—C15B—H15F	109.5
H8A—C8—H8B	107.2	C17—C16—N1	118.0 (3)
C10A—C9—C8	118.9 (6)	C17—C16—H16A	107.8
C8—C9—C10B	100.6 (6)	N1—C16—H16A	107.8
C10A—C9—H9A	107.6	C17—C16—H16B	107.8
C8—C9—H9A	107.6	N1—C16—H16B	107.8
C10A—C9—H9B	107.6	H16A—C16—H16B	107.1
C8—C9—H9B	107.6	C16—C17—C18	107.7 (4)
H9A—C9—H9B	107.0	C16—C17—H17A	110.2
C8—C9—H9C	111.6	C18—C17—H17A	110.2
C10B—C9—H9C	111.6	C16—C17—H17B	110.2
C8—C9—H9D	111.6	C18—C17—H17B	110.2
C10B—C9—H9D	111.6	H17A—C17—H17B	108.5
H9C—C9—H9D	109.4	C19—C18—C17	112.8 (5)
C9—C10A—C11A	113.4 (8)	C19—C18—H18A	109.0
C9—C10A—H10A	108.9	C17—C18—H18A	109.0
C11A—C10A—H10A	108.9	C19—C18—H18B	109.0
C9—C10A—H10B	108.9	C17—C18—H18B	109.0
C11A—C10A—H10B	108.9	H18A—C18—H18B	107.8
H10A—C10A—H10B	107.7	C18—C19—H19A	109.5
C10A—C11A—H11A	109.5	C18—C19—H19B	109.5
C10A—C11A—H11B	109.5	H19A—C19—H19B	109.5
H11A—C11A—H11B	109.5	C18—C19—H19C	109.5
C10A—C11A—H11C	109.5	H19A—C19—H19C	109.5
H11A—C11A—H11C	109.5	H19B—C19—H19C	109.5
H11B—C11A—H11C	109.5
S1^i—Zn1—S1—C1	124.23 (10)	C16—N1—C4—C5	60.3 (5)
S2^i—Zn1—S1—C1	−123.85 (10)	C12—N1—C4—C5	−179.5 (4)
S2—Zn1—S1—C1	3.88 (10)	N1—C4—C5—C6	179.6 (4)
S1—Zn1—S2—C2	−2.76 (11)	C4—C5—C6—C7	179.7 (5)
S1^i—Zn1—S2—C2	−130.94 (11)	C4—N1—C8—C9	−57.8 (5)
S2^i—Zn1—S2—C2	117.41 (11)	C16—N1—C8—C9	179.8 (4)
Zn1—S1—C1—C2	−5.1 (3)	C12—N1—C8—C9	59.1 (5)
Zn1—S1—C1—S3	175.64 (15)	N1—C8—C9—C10A	166.0 (6)
S1—C1—C2—S2	3.6 (5)	N1—C8—C9—C10B	−163.9 (7)
S3—C1—C2—S2	−177.13 (19)	C8—C9—C10A—C11A	77.3 (13)
S1—C1—C2—S4	−176.50 (18)	C8—C9—C10B—C11B	−153.7 (12)
S3—C1—C2—S4	2.8 (3)	C8—N1—C12—C13	59.4 (4)
Zn1—S2—C2—C1	0.5 (3)	C4—N1—C12—C13	−179.1 (4)
Zn1—S2—C2—S4	−179.38 (17)	C16—N1—C12—C13	−58.3 (5)
C2—C1—S3—C3	−2.0 (3)	N1—C12—C13—C14A	−159.2 (5)
S1—C1—S3—C3	177.39 (18)	N1—C12—C13—C14B	174.0 (5)
C1—C2—S4—C3	−2.2 (3)	C12—C13—C14A—C15A	−64.4 (15)
S2—C2—S4—C3	177.70 (19)	C12—C13—C14B—C15B	179.8 (7)
C1—S3—C3—S5	−179.3 (2)	C8—N1—C16—C17	178.3 (3)
C1—S3—C3—S4	0.4 (2)	C4—N1—C16—C17	55.7 (4)
C2—S4—C3—S5	−179.5 (2)	C12—N1—C16—C17	−60.8 (4)
C2—S4—C3—S3	0.8 (2)	N1—C16—C17—C18	173.4 (3)
C8—N1—C4—C5	−58.6 (5)	C16—C17—C18—C19	176.5 (4)

Symmetry code: (i) −x+1, y, −z+1/2.

(IX) Bis(tetraphenylarsonium) bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II)

Crystal data

(C6S10Zn^2^−)·2(C24H20As^+)	F(000) = 1240
Mr = 1224.67	Dx = 1.524 Mg m^−3
Triclinic, P1	Melting point = 478–481 K
a = 10.3451 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 15.0563 (7) Å	Cell parameters from 4866 reflections
c = 18.8083 (8) Å	θ = 2.3–24.9°
α = 73.072 (1)°	µ = 2.12 mm^−1
β = 85.867 (1)°	T = 300 K
γ = 72.259 (1)°	Block, red
V = 2668.9 (2) Å^3	0.33 × 0.21 × 0.15 mm
Z = 2

Data collection

Bruker SMART 1000 CCD area detector diffractometer	9377 independent reflections
Radiation source: fine-focus sealed tube	6069 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.028
ϕ and ω scans	θmax = 25.0°, θmin = 1.1°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −12→12
Tmin = 0.738, Tmax = 0.862	k = −17→17
16003 measured reflections	l = −22→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.067	H-atom parameters constrained
S = 0.86	w = 1/[σ^2(Fo^2) + (0.0285P)^2] where P = (Fo^2 + 2Fc^2)/3
9377 reflections	(Δ/σ)max = 0.001
604 parameters	Δρmax = 0.36 e Å^−3
0 restraints	Δρmin = −0.28 e Å^−3

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

H in calculated positions and refined with a riding model.

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

	x	y	z	Uiso*/Ueq
Zn1	0.46443 (4)	0.31624 (3)	0.24779 (2)	0.05534 (12)
S1	0.60851 (9)	0.38669 (7)	0.28674 (6)	0.0644 (3)
S2	0.26338 (9)	0.42316 (8)	0.27927 (6)	0.0723 (3)
S3	0.52705 (12)	0.58335 (8)	0.31011 (6)	0.0798 (3)
S4	0.24297 (12)	0.61810 (8)	0.29600 (6)	0.0820 (3)
S5	0.3427 (2)	0.77712 (10)	0.31257 (9)	0.1408 (6)
C1	0.4792 (4)	0.4877 (2)	0.29685 (18)	0.0556 (9)
C2	0.3445 (4)	0.5028 (3)	0.29171 (19)	0.0564 (9)
C3	0.3679 (5)	0.6661 (3)	0.3068 (2)	0.0828 (13)
S6	0.50098 (9)	0.14820 (7)	0.29673 (5)	0.0609 (3)
S7	0.47653 (10)	0.31170 (7)	0.12382 (5)	0.0605 (2)
S8	0.44669 (9)	0.01920 (6)	0.21430 (6)	0.0610 (3)
S9	0.42531 (9)	0.15664 (7)	0.07082 (5)	0.0603 (3)
S10	0.39256 (10)	−0.03646 (7)	0.08149 (7)	0.0738 (3)
C4	0.4703 (3)	0.1303 (2)	0.21255 (19)	0.0497 (8)
C5	0.4595 (3)	0.1952 (2)	0.14478 (19)	0.0494 (8)
C6	0.4204 (3)	0.0421 (2)	0.1203 (2)	0.0539 (9)
As1	0.09051 (3)	−0.26052 (2)	0.009498 (19)	0.04457 (10)
C7	−0.0398 (3)	−0.2595 (2)	0.08742 (19)	0.0480 (8)
C8	−0.0067 (4)	−0.3353 (3)	0.1510 (2)	0.0698 (11)
H8	0.0790	−0.3805	0.1568	0.084*
C9	−0.1004 (5)	−0.3445 (3)	0.2064 (2)	0.0855 (13)
H9	−0.0783	−0.3969	0.2490	0.103*
C10	−0.2257 (4)	−0.2772 (4)	0.1993 (3)	0.0754 (12)
H10	−0.2885	−0.2832	0.2370	0.090*
C11	−0.2570 (4)	−0.2021 (4)	0.1370 (3)	0.0816 (13)
H11	−0.3421	−0.1562	0.1323	0.098*
C12	−0.1656 (3)	−0.1914 (3)	0.0798 (2)	0.0730 (12)
H12	−0.1889	−0.1393	0.0372	0.088*
C13	0.2677 (3)	−0.3162 (2)	0.05412 (17)	0.0439 (8)
C14	0.3464 (3)	−0.4081 (2)	0.05359 (18)	0.0502 (8)
H14	0.3134	−0.4455	0.0322	0.060*
C15	0.4747 (3)	−0.4437 (3)	0.08515 (19)	0.0584 (9)
H15	0.5282	−0.5060	0.0859	0.070*
C16	0.5236 (3)	−0.3877 (3)	0.11534 (19)	0.0598 (10)
H16	0.6115	−0.4114	0.1350	0.072*
C17	0.4444 (4)	−0.2974 (3)	0.1168 (2)	0.0636 (10)
H17	0.4777	−0.2605	0.1386	0.076*
C18	0.3165 (3)	−0.2611 (2)	0.0864 (2)	0.0582 (10)
H18	0.2625	−0.1995	0.0875	0.070*
C19	0.0554 (3)	−0.3344 (2)	−0.04976 (18)	0.0449 (8)
C20	−0.0658 (3)	−0.3565 (2)	−0.0428 (2)	0.0594 (10)
H20	−0.1261	−0.3417	−0.0059	0.071*
C21	−0.0968 (4)	−0.4012 (3)	−0.0920 (2)	0.0740 (12)
H21	−0.1785	−0.4160	−0.0885	0.089*
C22	−0.0066 (5)	−0.4231 (3)	−0.1452 (2)	0.0767 (12)
H22	−0.0286	−0.4513	−0.1787	0.092*
C23	0.1160 (4)	−0.4044 (3)	−0.1505 (2)	0.0722 (11)
H23	0.1782	−0.4232	−0.1855	0.087*
C24	0.1472 (3)	−0.3577 (2)	−0.10374 (19)	0.0562 (9)
H24	0.2284	−0.3422	−0.1084	0.067*
C25	0.0801 (3)	−0.1356 (2)	−0.05673 (18)	0.0484 (8)
C26	0.1940 (4)	−0.1090 (3)	−0.0799 (2)	0.0817 (13)
H26	0.2782	−0.1500	−0.0599	0.098*
C27	0.1860 (4)	−0.0229 (4)	−0.1320 (3)	0.1075 (17)
H27	0.2651	−0.0063	−0.1475	0.129*
C28	0.0653 (5)	0.0387 (3)	−0.1618 (2)	0.0808 (12)
H28	0.0614	0.0981	−0.1963	0.097*
C29	−0.0497 (4)	0.0138 (3)	−0.1411 (2)	0.0801 (12)
H29	−0.1329	0.0556	−0.1620	0.096*
C30	−0.0437 (4)	−0.0735 (3)	−0.0892 (2)	0.0702 (11)
H30	−0.1227	−0.0910	−0.0758	0.084*
As2	−0.12845 (3)	0.24463 (2)	0.466014 (19)	0.04693 (10)
C31	−0.0549 (3)	0.2143 (2)	0.37682 (18)	0.0459 (8)
C32	0.0692 (3)	0.2284 (3)	0.3523 (2)	0.0612 (10)
H32	0.1141	0.2547	0.3781	0.073*
C33	0.1253 (4)	0.2034 (3)	0.2898 (2)	0.0740 (12)
H33	0.2077	0.2135	0.2726	0.089*
C34	0.0592 (4)	0.1633 (3)	0.2528 (2)	0.0798 (12)
H34	0.0977	0.1455	0.2109	0.096*
C35	−0.0627 (4)	0.1491 (3)	0.2769 (2)	0.0774 (12)
H35	−0.1059	0.1211	0.2517	0.093*
C36	−0.1221 (4)	0.1762 (2)	0.3385 (2)	0.0593 (10)
H36	−0.2066	0.1688	0.3539	0.071*
C37	0.0163 (3)	0.1883 (2)	0.53869 (18)	0.0484 (8)
C38	0.0233 (4)	0.2348 (3)	0.5906 (2)	0.0649 (10)
H38	−0.0399	0.2942	0.5898	0.078*
C39	0.1266 (5)	0.1914 (3)	0.6442 (2)	0.0859 (13)
H39	0.1343	0.2228	0.6789	0.103*
C40	0.2171 (4)	0.1027 (3)	0.6461 (2)	0.0813 (13)
H40	0.2852	0.0737	0.6826	0.098*
C41	0.2082 (4)	0.0563 (3)	0.5948 (2)	0.0744 (12)
H41	0.2690	−0.0044	0.5970	0.089*
C42	0.1094 (3)	0.0998 (3)	0.5401 (2)	0.0627 (10)
H42	0.1051	0.0696	0.5041	0.075*
C43	−0.2685 (3)	0.1839 (3)	0.50079 (19)	0.0495 (8)
C44	−0.2364 (4)	0.0975 (3)	0.5569 (2)	0.0649 (10)
H44	−0.1509	0.0725	0.5796	0.078*
C45	−0.3317 (5)	0.0485 (3)	0.5791 (3)	0.0844 (13)
H45	−0.3106	−0.0098	0.6168	0.101*
C46	−0.4558 (6)	0.0853 (4)	0.5461 (3)	0.0971 (17)
H46	−0.5192	0.0513	0.5610	0.117*
C47	−0.4898 (4)	0.1710 (4)	0.4915 (3)	0.0944 (16)
H47	−0.5765	0.1958	0.4702	0.113*
C48	−0.3948 (4)	0.2220 (3)	0.4674 (2)	0.0722 (11)
H48	−0.4167	0.2803	0.4297	0.087*
C49	−0.1865 (3)	0.3800 (2)	0.45792 (18)	0.0487 (8)
C50	−0.2910 (3)	0.4166 (3)	0.5012 (2)	0.0601 (10)
H50	−0.3422	0.3778	0.5288	0.072*
C51	−0.3188 (4)	0.5125 (3)	0.5030 (2)	0.0734 (12)
H51	−0.3887	0.5376	0.5322	0.088*
C52	−0.2443 (5)	0.5694 (3)	0.4624 (2)	0.0814 (13)
H52	−0.2634	0.6332	0.4641	0.098*
C53	−0.1418 (5)	0.5335 (3)	0.4193 (2)	0.0826 (13)
H53	−0.0917	0.5730	0.3914	0.099*
C54	−0.1119 (4)	0.4385 (3)	0.4166 (2)	0.0686 (11)
H54	−0.0418	0.4142	0.3872	0.082*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0551 (2)	0.0473 (3)	0.0651 (3)	−0.01599 (19)	−0.0011 (2)	−0.0167 (2)
S1	0.0547 (6)	0.0607 (7)	0.0760 (7)	−0.0200 (5)	−0.0117 (5)	−0.0105 (5)
S2	0.0533 (6)	0.0750 (7)	0.1034 (9)	−0.0200 (5)	0.0032 (5)	−0.0469 (7)
S3	0.1210 (9)	0.0772 (8)	0.0609 (7)	−0.0575 (7)	−0.0091 (6)	−0.0174 (6)
S4	0.1028 (9)	0.0671 (7)	0.0768 (8)	−0.0101 (6)	0.0011 (6)	−0.0372 (6)
S5	0.254 (2)	0.0762 (10)	0.1161 (12)	−0.0655 (11)	0.0303 (12)	−0.0529 (9)
C1	0.078 (3)	0.051 (2)	0.042 (2)	−0.0281 (19)	−0.0060 (18)	−0.0079 (17)
C2	0.064 (2)	0.059 (2)	0.051 (2)	−0.0159 (18)	−0.0027 (18)	−0.0236 (19)
C3	0.132 (4)	0.067 (3)	0.054 (3)	−0.029 (3)	0.007 (2)	−0.025 (2)
S6	0.0701 (6)	0.0476 (6)	0.0603 (6)	−0.0158 (5)	−0.0059 (5)	−0.0086 (5)
S7	0.0742 (6)	0.0477 (6)	0.0599 (6)	−0.0236 (5)	0.0033 (5)	−0.0106 (5)
S8	0.0628 (6)	0.0433 (6)	0.0751 (7)	−0.0160 (4)	0.0047 (5)	−0.0145 (5)
S9	0.0618 (6)	0.0563 (6)	0.0649 (6)	−0.0171 (5)	−0.0003 (5)	−0.0204 (5)
S10	0.0619 (6)	0.0631 (7)	0.1069 (9)	−0.0168 (5)	−0.0004 (6)	−0.0411 (6)
C4	0.0461 (19)	0.038 (2)	0.061 (2)	−0.0080 (15)	0.0018 (17)	−0.0130 (18)
C5	0.0428 (19)	0.043 (2)	0.060 (2)	−0.0094 (15)	0.0021 (17)	−0.0146 (18)
C6	0.0331 (17)	0.052 (2)	0.077 (3)	−0.0055 (15)	0.0002 (17)	−0.026 (2)
As1	0.03888 (18)	0.0435 (2)	0.0527 (2)	−0.01203 (15)	−0.00089 (16)	−0.01553 (17)
C7	0.045 (2)	0.056 (2)	0.049 (2)	−0.0172 (17)	0.0006 (17)	−0.0206 (19)
C8	0.071 (3)	0.068 (3)	0.058 (3)	−0.010 (2)	0.012 (2)	−0.013 (2)
C9	0.108 (4)	0.080 (3)	0.062 (3)	−0.031 (3)	0.018 (3)	−0.012 (2)
C10	0.074 (3)	0.110 (4)	0.070 (3)	−0.055 (3)	0.026 (2)	−0.044 (3)
C11	0.044 (2)	0.110 (4)	0.094 (4)	−0.016 (2)	0.005 (2)	−0.044 (3)
C12	0.050 (2)	0.087 (3)	0.065 (3)	−0.006 (2)	0.004 (2)	−0.013 (2)
C13	0.0402 (18)	0.046 (2)	0.047 (2)	−0.0158 (15)	0.0017 (15)	−0.0132 (17)
C14	0.052 (2)	0.041 (2)	0.057 (2)	−0.0117 (16)	−0.0065 (17)	−0.0137 (17)
C15	0.056 (2)	0.043 (2)	0.064 (2)	−0.0019 (17)	−0.0055 (19)	−0.0079 (19)
C16	0.046 (2)	0.064 (3)	0.060 (2)	−0.0130 (19)	−0.0154 (18)	−0.002 (2)
C17	0.064 (2)	0.064 (3)	0.070 (3)	−0.025 (2)	−0.017 (2)	−0.019 (2)
C18	0.054 (2)	0.046 (2)	0.077 (3)	−0.0083 (17)	−0.0087 (19)	−0.025 (2)
C19	0.0418 (18)	0.044 (2)	0.049 (2)	−0.0114 (15)	−0.0063 (16)	−0.0132 (16)
C20	0.047 (2)	0.058 (2)	0.079 (3)	−0.0195 (18)	0.0037 (19)	−0.024 (2)
C21	0.062 (3)	0.068 (3)	0.103 (4)	−0.027 (2)	−0.013 (2)	−0.029 (3)
C22	0.090 (3)	0.062 (3)	0.086 (3)	−0.016 (2)	−0.027 (3)	−0.033 (2)
C23	0.080 (3)	0.071 (3)	0.069 (3)	−0.012 (2)	−0.004 (2)	−0.034 (2)
C24	0.052 (2)	0.058 (2)	0.061 (2)	−0.0169 (18)	−0.0010 (19)	−0.021 (2)
C25	0.0429 (19)	0.047 (2)	0.055 (2)	−0.0121 (16)	0.0036 (17)	−0.0165 (17)
C26	0.045 (2)	0.066 (3)	0.109 (4)	−0.011 (2)	0.002 (2)	0.009 (3)
C27	0.065 (3)	0.081 (4)	0.145 (5)	−0.028 (3)	0.014 (3)	0.020 (3)
C28	0.093 (3)	0.053 (3)	0.079 (3)	−0.019 (3)	0.018 (3)	0.000 (2)
C29	0.064 (3)	0.063 (3)	0.084 (3)	0.001 (2)	0.004 (2)	0.001 (2)
C30	0.051 (2)	0.069 (3)	0.076 (3)	−0.015 (2)	0.002 (2)	−0.002 (2)
As2	0.0499 (2)	0.0444 (2)	0.0495 (2)	−0.01694 (16)	0.00489 (17)	−0.01579 (17)
C31	0.0457 (19)	0.047 (2)	0.045 (2)	−0.0136 (16)	0.0052 (16)	−0.0141 (16)
C32	0.057 (2)	0.072 (3)	0.061 (3)	−0.0202 (19)	0.005 (2)	−0.028 (2)
C33	0.055 (2)	0.089 (3)	0.073 (3)	−0.015 (2)	0.012 (2)	−0.023 (3)
C34	0.080 (3)	0.093 (3)	0.063 (3)	−0.013 (3)	0.014 (2)	−0.034 (3)
C35	0.090 (3)	0.085 (3)	0.069 (3)	−0.025 (2)	−0.002 (2)	−0.040 (3)
C36	0.059 (2)	0.062 (3)	0.063 (3)	−0.0208 (19)	0.0047 (19)	−0.025 (2)
C37	0.050 (2)	0.050 (2)	0.046 (2)	−0.0171 (17)	0.0041 (16)	−0.0142 (17)
C38	0.080 (3)	0.054 (2)	0.055 (2)	−0.007 (2)	−0.009 (2)	−0.017 (2)
C39	0.113 (4)	0.078 (3)	0.063 (3)	−0.017 (3)	−0.019 (3)	−0.021 (2)
C40	0.070 (3)	0.094 (4)	0.065 (3)	−0.020 (3)	−0.016 (2)	−0.001 (3)
C41	0.058 (3)	0.061 (3)	0.090 (3)	−0.006 (2)	−0.007 (2)	−0.012 (2)
C42	0.057 (2)	0.056 (2)	0.077 (3)	−0.0104 (19)	−0.001 (2)	−0.027 (2)
C43	0.055 (2)	0.053 (2)	0.048 (2)	−0.0232 (17)	0.0145 (17)	−0.0204 (18)
C44	0.072 (3)	0.056 (3)	0.070 (3)	−0.023 (2)	0.023 (2)	−0.024 (2)
C45	0.103 (4)	0.062 (3)	0.091 (3)	−0.040 (3)	0.044 (3)	−0.021 (3)
C46	0.100 (4)	0.111 (5)	0.117 (5)	−0.070 (4)	0.051 (4)	−0.059 (4)
C47	0.061 (3)	0.144 (5)	0.100 (4)	−0.049 (3)	0.016 (3)	−0.052 (4)
C48	0.062 (3)	0.088 (3)	0.069 (3)	−0.028 (2)	0.008 (2)	−0.021 (2)
C49	0.056 (2)	0.043 (2)	0.045 (2)	−0.0130 (17)	−0.0051 (17)	−0.0101 (17)
C50	0.066 (2)	0.052 (2)	0.058 (2)	−0.0138 (19)	0.0027 (19)	−0.015 (2)
C51	0.088 (3)	0.053 (3)	0.069 (3)	−0.001 (2)	0.000 (2)	−0.022 (2)
C52	0.119 (4)	0.048 (3)	0.079 (3)	−0.021 (3)	−0.010 (3)	−0.022 (2)
C53	0.111 (4)	0.058 (3)	0.088 (3)	−0.043 (3)	0.006 (3)	−0.017 (3)
C54	0.083 (3)	0.058 (3)	0.067 (3)	−0.026 (2)	0.017 (2)	−0.018 (2)

Geometric parameters (Å, º)

Zn1—S1	2.3360 (10)	C25—C30	1.392 (4)
Zn1—S6	2.3458 (10)	C26—C27	1.362 (5)
Zn1—S7	2.3458 (10)	C26—H26	0.9300
Zn1—S2	2.3674 (10)	C27—C28	1.351 (5)
S1—C1	1.740 (4)	C27—H27	0.9300
S2—C2	1.733 (4)	C28—C29	1.352 (5)
S3—C3	1.728 (4)	C28—H28	0.9300
S3—C1	1.745 (3)	C29—C30	1.377 (5)
S4—C3	1.711 (5)	C29—H29	0.9300
S4—C2	1.755 (3)	C30—H30	0.9300
S5—C3	1.646 (4)	As2—C49	1.904 (3)
C1—C2	1.347 (4)	As2—C31	1.911 (3)
S6—C4	1.747 (3)	As2—C37	1.917 (3)
S7—C5	1.743 (3)	As2—C43	1.919 (3)
S8—C6	1.725 (4)	C31—C36	1.373 (4)
S8—C4	1.754 (3)	C31—C32	1.389 (4)
S9—C6	1.719 (4)	C32—C33	1.375 (5)
S9—C5	1.751 (3)	C32—H32	0.9300
S10—C6	1.660 (3)	C33—C34	1.372 (5)
C4—C5	1.349 (4)	C33—H33	0.9300
As1—C25	1.906 (3)	C34—C35	1.366 (5)
As1—C19	1.908 (3)	C34—H34	0.9300
As1—C13	1.908 (3)	C35—C36	1.381 (5)
As1—C7	1.918 (3)	C35—H35	0.9300
C7—C8	1.370 (5)	C36—H36	0.9300
C7—C12	1.376 (4)	C37—C38	1.374 (4)
C8—C9	1.376 (5)	C37—C42	1.380 (4)
C8—H8	0.9300	C38—C39	1.391 (5)
C9—C10	1.367 (5)	C38—H38	0.9300
C9—H9	0.9300	C39—C40	1.370 (5)
C10—C11	1.348 (5)	C39—H39	0.9300
C10—H10	0.9300	C40—C41	1.368 (5)
C11—C12	1.386 (5)	C40—H40	0.9300
C11—H11	0.9300	C41—C42	1.372 (5)
C12—H12	0.9300	C41—H41	0.9300
C13—C14	1.378 (4)	C42—H42	0.9300
C13—C18	1.380 (4)	C43—C48	1.372 (5)
C14—C15	1.377 (4)	C43—C44	1.380 (5)
C14—H14	0.9300	C44—C45	1.376 (5)
C15—C16	1.367 (5)	C44—H44	0.9300
C15—H15	0.9300	C45—C46	1.350 (6)
C16—C17	1.364 (4)	C45—H45	0.9300
C16—H16	0.9300	C46—C47	1.359 (6)
C17—C18	1.365 (4)	C46—H46	0.9300
C17—H17	0.9300	C47—C48	1.398 (6)
C18—H18	0.9300	C47—H47	0.9300
C19—C20	1.380 (4)	C48—H48	0.9300
C19—C24	1.386 (4)	C49—C54	1.380 (5)
C20—C21	1.397 (5)	C49—C50	1.380 (4)
C20—H20	0.9300	C50—C51	1.393 (5)
C21—C22	1.360 (5)	C50—H50	0.9300
C21—H21	0.9300	C51—C52	1.359 (6)
C22—C23	1.371 (5)	C51—H51	0.9300
C22—H22	0.9300	C52—C53	1.363 (5)
C23—C24	1.383 (4)	C52—H52	0.9300
C23—H23	0.9300	C53—C54	1.382 (5)
C24—H24	0.9300	C53—H53	0.9300
C25—C26	1.360 (5)	C54—H54	0.9300
S1—Zn1—S6	118.44 (4)	C30—C25—As1	120.3 (3)
S1—Zn1—S7	117.89 (4)	C25—C26—C27	120.6 (4)
S6—Zn1—S7	94.02 (3)	C25—C26—H26	119.7
S1—Zn1—S2	94.36 (3)	C27—C26—H26	119.7
S6—Zn1—S2	118.53 (4)	C28—C27—C26	121.2 (4)
S7—Zn1—S2	115.56 (4)	C28—C27—H27	119.4
C1—S1—Zn1	94.92 (12)	C26—C27—H27	119.4
C2—S2—Zn1	94.10 (12)	C27—C28—C29	119.7 (4)
C3—S3—C1	98.84 (19)	C27—C28—H28	120.2
C3—S4—C2	99.15 (18)	C29—C28—H28	120.2
C2—C1—S1	127.1 (3)	C28—C29—C30	120.0 (4)
C2—C1—S3	115.5 (3)	C28—C29—H29	120.0
S1—C1—S3	117.2 (2)	C30—C29—H29	120.0
C1—C2—S2	127.3 (3)	C29—C30—C25	120.3 (4)
C1—C2—S4	115.0 (3)	C29—C30—H30	119.8
S2—C2—S4	117.7 (2)	C25—C30—H30	119.8
S5—C3—S4	125.2 (3)	C49—As2—C31	114.12 (14)
S5—C3—S3	123.4 (3)	C49—As2—C37	105.56 (13)
S4—C3—S3	111.4 (2)	C31—As2—C37	106.56 (13)
C4—S6—Zn1	94.86 (12)	C49—As2—C43	112.69 (14)
C5—S7—Zn1	94.65 (12)	C31—As2—C43	109.46 (13)
C6—S8—C4	98.36 (17)	C37—As2—C43	108.02 (15)
C6—S9—C5	98.44 (16)	C36—C31—C32	120.3 (3)
C5—C4—S6	126.3 (3)	C36—C31—As2	120.3 (3)
C5—C4—S8	115.3 (3)	C32—C31—As2	119.4 (2)
S6—C4—S8	118.3 (2)	C33—C32—C31	119.8 (3)
C4—C5—S7	126.9 (3)	C33—C32—H32	120.1
C4—C5—S9	115.7 (3)	C31—C32—H32	120.1
S7—C5—S9	117.4 (2)	C34—C33—C32	119.6 (4)
S10—C6—S9	123.4 (2)	C34—C33—H33	120.2
S10—C6—S8	124.4 (2)	C32—C33—H33	120.2
S9—C6—S8	112.18 (18)	C35—C34—C33	120.8 (4)
C25—As1—C19	106.02 (14)	C35—C34—H34	119.6
C25—As1—C13	108.40 (14)	C33—C34—H34	119.6
C19—As1—C13	112.06 (13)	C34—C35—C36	120.3 (4)
C25—As1—C7	114.53 (14)	C34—C35—H35	119.9
C19—As1—C7	107.73 (13)	C36—C35—H35	119.9
C13—As1—C7	108.17 (13)	C31—C36—C35	119.2 (3)
C8—C7—C12	119.8 (3)	C31—C36—H36	120.4
C8—C7—As1	116.8 (3)	C35—C36—H36	120.4
C12—C7—As1	123.2 (3)	C38—C37—C42	120.6 (3)
C7—C8—C9	120.0 (4)	C38—C37—As2	119.5 (2)
C7—C8—H8	120.0	C42—C37—As2	119.8 (2)
C9—C8—H8	120.0	C37—C38—C39	118.7 (3)
C10—C9—C8	120.6 (4)	C37—C38—H38	120.6
C10—C9—H9	119.7	C39—C38—H38	120.6
C8—C9—H9	119.7	C40—C39—C38	120.3 (4)
C11—C10—C9	119.2 (4)	C40—C39—H39	119.9
C11—C10—H10	120.4	C38—C39—H39	119.9
C9—C10—H10	120.4	C41—C40—C39	120.5 (4)
C10—C11—C12	121.7 (4)	C41—C40—H40	119.7
C10—C11—H11	119.2	C39—C40—H40	119.7
C12—C11—H11	119.2	C40—C41—C42	119.8 (4)
C7—C12—C11	118.8 (4)	C40—C41—H41	120.1
C7—C12—H12	120.6	C42—C41—H41	120.1
C11—C12—H12	120.6	C41—C42—C37	120.0 (3)
C14—C13—C18	120.4 (3)	C41—C42—H42	120.0
C14—C13—As1	121.5 (2)	C37—C42—H42	120.0
C18—C13—As1	118.1 (2)	C48—C43—C44	120.7 (3)
C15—C14—C13	119.0 (3)	C48—C43—As2	120.8 (3)
C15—C14—H14	120.5	C44—C43—As2	118.4 (3)
C13—C14—H14	120.5	C45—C44—C43	119.7 (4)
C16—C15—C14	120.2 (3)	C45—C44—H44	120.2
C16—C15—H15	119.9	C43—C44—H44	120.2
C14—C15—H15	119.9	C46—C45—C44	119.9 (5)
C17—C16—C15	120.5 (3)	C46—C45—H45	120.0
C17—C16—H16	119.8	C44—C45—H45	120.0
C15—C16—H16	119.8	C45—C46—C47	121.2 (5)
C16—C17—C18	120.2 (3)	C45—C46—H46	119.4
C16—C17—H17	119.9	C47—C46—H46	119.4
C18—C17—H17	119.9	C46—C47—C48	120.1 (5)
C17—C18—C13	119.7 (3)	C46—C47—H47	119.9
C17—C18—H18	120.2	C48—C47—H47	119.9
C13—C18—H18	120.2	C43—C48—C47	118.4 (4)
C20—C19—C24	121.0 (3)	C43—C48—H48	120.8
C20—C19—As1	119.7 (2)	C47—C48—H48	120.8
C24—C19—As1	119.1 (2)	C54—C49—C50	119.9 (3)
C19—C20—C21	119.2 (3)	C54—C49—As2	119.5 (3)
C19—C20—H20	120.4	C50—C49—As2	120.0 (3)
C21—C20—H20	120.4	C49—C50—C51	119.2 (4)
C22—C21—C20	119.5 (4)	C49—C50—H50	120.4
C22—C21—H21	120.3	C51—C50—H50	120.4
C20—C21—H21	120.3	C52—C51—C50	120.4 (4)
C21—C22—C23	121.4 (4)	C52—C51—H51	119.8
C21—C22—H22	119.3	C50—C51—H51	119.8
C23—C22—H22	119.3	C51—C52—C53	120.4 (4)
C22—C23—C24	120.1 (4)	C51—C52—H52	119.8
C22—C23—H23	120.0	C53—C52—H52	119.8
C24—C23—H23	120.0	C52—C53—C54	120.3 (4)
C23—C24—C19	118.8 (3)	C52—C53—H53	119.8
C23—C24—H24	120.6	C54—C53—H53	119.8
C19—C24—H24	120.6	C49—C54—C53	119.7 (4)
C26—C25—C30	118.1 (4)	C49—C54—H54	120.1
C26—C25—As1	121.2 (3)	C53—C54—H54	120.1
S6—Zn1—S1—C1	−137.10 (12)	C24—C19—C20—C21	−1.2 (5)
S7—Zn1—S1—C1	110.77 (12)	As1—C19—C20—C21	173.0 (3)
S2—Zn1—S1—C1	−11.23 (12)	C19—C20—C21—C22	0.7 (6)
S1—Zn1—S2—C2	12.53 (13)	C20—C21—C22—C23	1.7 (6)
S6—Zn1—S2—C2	138.34 (12)	C21—C22—C23—C24	−3.5 (6)
S7—Zn1—S2—C2	−111.27 (12)	C22—C23—C24—C19	2.9 (6)
Zn1—S1—C1—C2	7.5 (3)	C20—C19—C24—C23	−0.5 (5)
Zn1—S1—C1—S3	−168.69 (17)	As1—C19—C24—C23	−174.8 (3)
C3—S3—C1—C2	−2.6 (3)	C19—As1—C25—C26	−104.5 (3)
C3—S3—C1—S1	174.0 (2)	C13—As1—C25—C26	16.0 (3)
S1—C1—C2—S2	4.2 (5)	C7—As1—C25—C26	136.9 (3)
S3—C1—C2—S2	−179.5 (2)	C19—As1—C25—C30	68.1 (3)
S1—C1—C2—S4	−174.1 (2)	C13—As1—C25—C30	−171.4 (3)
S3—C1—C2—S4	2.2 (4)	C7—As1—C25—C30	−50.5 (3)
Zn1—S2—C2—C1	−12.7 (3)	C30—C25—C26—C27	1.5 (6)
Zn1—S2—C2—S4	165.51 (18)	As1—C25—C26—C27	174.3 (4)
C3—S4—C2—C1	−0.7 (3)	C25—C26—C27—C28	0.6 (8)
C3—S4—C2—S2	−179.1 (2)	C26—C27—C28—C29	−1.9 (8)
C2—S4—C3—S5	178.3 (3)	C27—C28—C29—C30	0.9 (7)
C2—S4—C3—S3	−1.1 (2)	C28—C29—C30—C25	1.2 (6)
C1—S3—C3—S5	−177.4 (3)	C26—C25—C30—C29	−2.4 (6)
C1—S3—C3—S4	2.0 (2)	As1—C25—C30—C29	−175.3 (3)
S1—Zn1—S6—C4	−139.31 (11)	C49—As2—C31—C36	−112.6 (3)
S7—Zn1—S6—C4	−14.46 (11)	C37—As2—C31—C36	131.3 (3)
S2—Zn1—S6—C4	107.57 (11)	C43—As2—C31—C36	14.7 (3)
S1—Zn1—S7—C5	140.13 (11)	C49—As2—C31—C32	69.3 (3)
S6—Zn1—S7—C5	14.87 (11)	C37—As2—C31—C32	−46.8 (3)
S2—Zn1—S7—C5	−109.48 (11)	C43—As2—C31—C32	−163.4 (3)
Zn1—S6—C4—C5	11.5 (3)	C36—C31—C32—C33	−0.5 (5)
Zn1—S6—C4—S8	−166.78 (16)	As2—C31—C32—C33	177.5 (3)
C6—S8—C4—C5	1.1 (3)	C31—C32—C33—C34	−1.0 (6)
C6—S8—C4—S6	179.58 (18)	C32—C33—C34—C35	0.8 (6)
S6—C4—C5—S7	1.4 (5)	C33—C34—C35—C36	0.8 (7)
S8—C4—C5—S7	179.75 (17)	C32—C31—C36—C35	2.2 (5)
S6—C4—C5—S9	−178.90 (17)	As2—C31—C36—C35	−175.9 (3)
S8—C4—C5—S9	−0.5 (3)	C34—C35—C36—C31	−2.3 (6)
Zn1—S7—C5—C4	−13.3 (3)	C49—As2—C37—C38	23.9 (3)
Zn1—S7—C5—S9	166.98 (15)	C31—As2—C37—C38	145.6 (3)
C6—S9—C5—C4	−0.3 (3)	C43—As2—C37—C38	−96.9 (3)
C6—S9—C5—S7	179.46 (18)	C49—As2—C37—C42	−158.4 (3)
C5—S9—C6—S10	−179.4 (2)	C31—As2—C37—C42	−36.7 (3)
C5—S9—C6—S8	0.98 (19)	C43—As2—C37—C42	80.8 (3)
C4—S8—C6—S10	179.2 (2)	C42—C37—C38—C39	0.5 (6)
C4—S8—C6—S9	−1.22 (19)	As2—C37—C38—C39	178.1 (3)
C25—As1—C7—C8	−155.0 (3)	C37—C38—C39—C40	−1.7 (6)
C19—As1—C7—C8	87.3 (3)	C38—C39—C40—C41	0.9 (7)
C13—As1—C7—C8	−34.0 (3)	C39—C40—C41—C42	1.1 (7)
C25—As1—C7—C12	29.8 (3)	C40—C41—C42—C37	−2.4 (6)
C19—As1—C7—C12	−87.8 (3)	C38—C37—C42—C41	1.5 (6)
C13—As1—C7—C12	150.8 (3)	As2—C37—C42—C41	−176.1 (3)
C12—C7—C8—C9	1.6 (6)	C49—As2—C43—C48	51.3 (3)
As1—C7—C8—C9	−173.7 (3)	C31—As2—C43—C48	−76.8 (3)
C7—C8—C9—C10	−1.5 (6)	C37—As2—C43—C48	167.5 (3)
C8—C9—C10—C11	0.6 (6)	C49—As2—C43—C44	−132.8 (3)
C9—C10—C11—C12	0.2 (7)	C31—As2—C43—C44	99.0 (3)
C8—C7—C12—C11	−0.7 (6)	C37—As2—C43—C44	−16.6 (3)
As1—C7—C12—C11	174.3 (3)	C48—C43—C44—C45	0.7 (5)
C10—C11—C12—C7	−0.2 (6)	As2—C43—C44—C45	−175.1 (3)
C25—As1—C13—C14	−128.0 (3)	C43—C44—C45—C46	−0.2 (6)
C19—As1—C13—C14	−11.4 (3)	C44—C45—C46—C47	−0.9 (7)
C7—As1—C13—C14	107.2 (3)	C45—C46—C47—C48	1.4 (7)
C25—As1—C13—C18	51.1 (3)	C44—C43—C48—C47	−0.2 (5)
C19—As1—C13—C18	167.7 (3)	As2—C43—C48—C47	175.5 (3)
C7—As1—C13—C18	−73.7 (3)	C46—C47—C48—C43	−0.8 (6)
C18—C13—C14—C15	−0.5 (5)	C31—As2—C49—C54	−37.9 (3)
As1—C13—C14—C15	178.5 (2)	C37—As2—C49—C54	78.7 (3)
C13—C14—C15—C16	−1.1 (5)	C43—As2—C49—C54	−163.6 (3)
C14—C15—C16—C17	2.2 (6)	C31—As2—C49—C50	151.0 (3)
C15—C16—C17—C18	−1.6 (6)	C37—As2—C49—C50	−92.3 (3)
C16—C17—C18—C13	−0.1 (6)	C43—As2—C49—C50	25.4 (3)
C14—C13—C18—C17	1.1 (5)	C54—C49—C50—C51	−0.6 (5)
As1—C13—C18—C17	−178.0 (3)	As2—C49—C50—C51	170.4 (3)
C25—As1—C19—C20	−108.5 (3)	C49—C50—C51—C52	0.3 (6)
C13—As1—C19—C20	133.4 (3)	C50—C51—C52—C53	0.2 (6)
C7—As1—C19—C20	14.5 (3)	C51—C52—C53—C54	−0.4 (7)
C25—As1—C19—C24	65.9 (3)	C50—C49—C54—C53	0.4 (6)
C13—As1—C19—C24	−52.2 (3)	As2—C49—C54—C53	−170.6 (3)
C7—As1—C19—C24	−171.1 (3)	C52—C53—C54—C49	0.1 (6)