Dy8SnS13.61O0.39 from single-crystal data

Daszkiewicz, M.; Gulay, L.D.; Shemet, V.Y.; Pietraszko, A.

doi:10.1107/S1600536807063416

Dy₈SnS_13.61O_0.39 from single-crystal data

M. Daszkiewicz, L. D. Gulay, V. Y. Shemet and A. Pietraszko

Crystals of the title dysprosium tin sulfide oxide, Dy₈SnS₁₃S_1-xO_x [x = 0.39 (4)], were obtained unintentionally from the Dy-Sn-S system. A statistical mixture of sulfur and oxygen was assumed for one position in the structure. S and O atoms surround each of the eight symmetrically non-equivalent dysprosium atoms. The Sn atoms are located in tetrahedral surroundings of sulfur atoms. Trigonal prisms and tetrahedra are connected to each other by their edges. All atoms are situated in mirror planes.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807063416/pk2066sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807063416/pk2066Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (Sn-S) = 0.004 Å
Disorder in main residue
R factor = 0.026
wR factor = 0.038
Data-to-parameter ratio = 16.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    S     Ueq(max)/Ueq(min) ...       4.25 Ratio

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.25 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
PLAT220_ALERT_2_C Large Non-Solvent   Dy     Ueq(max)/Ueq(min) ...       2.81 Ratio
PLAT301_ALERT_3_C Main Residue  Disorder .........................       3.00 Perc.
PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su ..       0.20

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           26.72
           From the CIF: _reflns_number_total               2287
           Count of symmetry unique reflns         1198
           Completeness (_total/calc)            190.90%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1089
           Fraction of Friedel pairs measured     0.909
           Are heavy atom types Z>Si present        yes
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          1

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

An attempt to synthesize Dy₂SnS₅, a compound with the La₂SnS₅ type structure was unsuccessful, resulting in a multiphase product. However, the formation of the new compound, Dy₈SnS₁₃S_{1 -}_xO_x (x = 0.39 (4)) was achieved. The structure of this compound was investigated by means of single-crystal X-ray diffraction. In the initial stage of refinement, the composition Dy₈SnS₁₄ was assumed. However, unusually short Dy2—S14 (2.399 (5) Å) and Dy3—S14 (2.508 (7) Å) distances and a large value for the displacement parameter of S14 were observed. To complete the refinement, a statistical mixture (S and O) was assumed at the site of S14. Refinement of this model reduced the unusual displacement parameter to a physically reasonable value. The final composition was Dy₈SnS₁₃S_{1 -}_xO_x (x = 0.39 (4)). The values of the Dy2—S14 (2.399 (5) Å) and Dy3—S14 (2.508 (7) Å) distances are intermediate between the Dy—O (2.220–2.264 Å) and Dy–S (2.704–2.742 Å) distances in Dy₂OS₂ (Schleid, 1991). A similar substitution of S by O in one position has also been observed in the structure of the La₁₀S₁₄S_1
-_xO_x (x ≈ 1/2) compound (Besançon et al., 1973).

The unit cell and coordination polyhedra of the Dy and Sn atoms in the structure of the Dy₈SnS_{14 -}_xO_x (x = 0.39 (4)) compound are shown in Fig. 1. Sulfur and oxygen atoms surround each of eight symmetrically non-equivalent dysprosium atoms. However, only one mono-capped trigonal prism is evident (Dy1) along with seven bi-capped trigonal prisms around the remaining Dy atoms. The Sn atoms are located in tetrahedral surroundings of sulfur atoms. Trigonal prisms and tetrahedra are connected to each other by edges.

Related literature top

For previous structures with a statistical mixture of sulfur and oxygen, see: Besançon et al. (1973); cShleid (1991).

Experimental top

Single crystals of the title compound were grown by fusion of the elemental constituents (Alfa Aesar; purity > 99.9%_wt) in evacuated silica ampoules. The ampoule was heated in a tube furnace with a heating rate of 30 K/h to 1420 K and kept at this temperature for 4 h. It was then cooled down slowly (10 K/h) to 870 K and annealed at this temperature for further 240 h and finally quenched in cold water. The product was a brown-coloured compact alloy containing red crystals with a prismatic habit and maximal lengths of 0.2 mm. An EDAX PV9800 microanalyser was used for the confirmation of the composition of the Dy, Sn and S in the crystal. The content of oxygen (<2%) was out of the limit of the microanalyser.

Structure description top

For previous structures with a statistical mixture of sulfur and oxygen, see: Besançon et al. (1973); cShleid (1991).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2007) and PLATON (Spek, 2003).

Figures top

Fig. 1. The structure of Dy₈SnS_13.61O_0.39 viewed down the a axis. Displacement ellipsoids are shown at the 50% probability level.

Dysprosium tin sulfide oxide top

Crystal data top

Dy₈SnS_13.61O_0.39	F(000) = 3196
M_r = 1861.27	D_x = 6.506 Mg m⁻³
Orthorhombic, Cmc2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 1910 reflections
a = 3.7822 (8) Å	θ = 2.6–26.7°
b = 23.620 (5) Å	µ = 33.80 mm⁻¹
c = 21.271 (4) Å	T = 293 K
V = 1900.3 (7) Å³	Needle, red
Z = 4	0.14 × 0.01 × 0.01 mm

Data collection top

KUMA KM-4 with CCD area-detector diffractometer	2287 independent reflections
Radiation source: fine-focus sealed tube	1910 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.049
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm^-1	θ_max = 26.7°, θ_min = 2.6°
ω–scan	h = −4→4
Absorption correction: numerical (CrysAlis; Oxford Diffraction, 2007)	k = −29→29
T_min = 0.104, T_max = 0.716	l = −26→26
11655 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.026	w = 1/[σ²(F_o²) + (0.0128P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.038	(Δ/σ)_max = 0.001
S = 0.89	Δρ_max = 3.05 e Å⁻³
2287 reflections	Δρ_min = −1.56 e Å⁻³
141 parameters	Absolute structure: Flack (1983), 1089 Friedel pairs
1 restraint	Absolute structure parameter: 0.0 (2)

Crystal data top

Dy₈SnS_13.61O_0.39	V = 1900.3 (7) Å³
M_r = 1861.27	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 3.7822 (8) Å	µ = 33.80 mm⁻¹
b = 23.620 (5) Å	T = 293 K
c = 21.271 (4) Å	0.14 × 0.01 × 0.01 mm

Data collection top

KUMA KM-4 with CCD area-detector diffractometer	2287 independent reflections
Absorption correction: numerical (CrysAlis; Oxford Diffraction, 2007)	1910 reflections with I > 2σ(I)
T_min = 0.104, T_max = 0.716	R_int = 0.049
11655 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	1 restraint
wR(F²) = 0.038	Δρ_max = 3.05 e Å⁻³
S = 0.89	Δρ_min = −1.56 e Å⁻³
2287 reflections	Absolute structure: Flack (1983), 1089 Friedel pairs
141 parameters	Absolute structure parameter: 0.0 (2)

Special details top

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 > 2σ(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.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Dy1	0.0000	0.69122 (4)	0.08524 (3)	0.0086 (2)
Dy2	0.0000	0.44849 (4)	0.24158 (5)	0.0242 (3)
Dy3	0.0000	0.10373 (4)	0.23391 (4)	0.0132 (2)
Dy4	0.0000	0.04543 (4)	0.40541 (5)	0.0125 (2)
Dy5	0.0000	0.85422 (4)	0.07459 (5)	0.0106 (2)
Dy6	0.0000	0.27636 (4)	0.24724 (4)	0.0100 (2)
Dy7	0.0000	0.37415 (4)	0.41648 (5)	0.0109 (2)
Dy8	0.5000	0.52208 (3)	0.07589 (4)	0.01244 (19)
Sn1	0.0000	0.70904 (6)	0.40908 (8)	0.0076 (2)
S1	0.0000	0.85740 (18)	0.2105 (2)	0.0088 (11)
S2	0.5000	0.43628 (19)	0.3487 (2)	0.0100 (10)
S3	0.5000	0.7734 (2)	0.1121 (2)	0.0089 (10)
S4	0.0000	0.48205 (18)	0.4751 (2)	0.0086 (9)
S5	0.0000	0.55462 (18)	0.3115 (2)	0.0100 (10)
S6	0.5000	0.63430 (18)	0.0139 (2)	0.0084 (10)
S7	0.0000	0.4362 (2)	0.1072 (2)	0.0121 (11)
S8	0.0000	0.58602 (18)	0.13619 (19)	0.0105 (9)
S9	0.5000	0.7460 (2)	0.4772 (2)	0.0141 (10)
S10	0.0000	0.1733 (2)	0.3409 (2)	0.0169 (10)
S11	0.0000	0.69522 (18)	0.21604 (19)	0.0079 (9)
S12	0.0000	0.6207 (2)	0.4722 (2)	0.0112 (10)
S13	0.0000	0.80025 (18)	0.3496 (2)	0.0096 (9)
O14	0.0000	0.0010 (3)	0.2040 (4)	0.034 (3)	0.39 (4)
S14	0.0000	0.0010 (3)	0.2040 (4)	0.034 (3)	0.61 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.0068 (4)	0.0089 (5)	0.0101 (5)	0.000	0.000	−0.0003 (4)
Dy2	0.0243 (5)	0.0308 (6)	0.0174 (7)	0.000	0.000	−0.0128 (5)
Dy3	0.0077 (4)	0.0231 (5)	0.0089 (5)	0.000	0.000	0.0020 (4)
Dy4	0.0095 (5)	0.0173 (5)	0.0106 (5)	0.000	0.000	0.0007 (4)
Dy5	0.0062 (4)	0.0107 (4)	0.0149 (5)	0.000	0.000	0.0034 (4)
Dy6	0.0069 (4)	0.0122 (4)	0.0110 (5)	0.000	0.000	0.0010 (4)
Dy7	0.0083 (4)	0.0162 (5)	0.0083 (5)	0.000	0.000	−0.0014 (4)
Dy8	0.0062 (4)	0.0104 (4)	0.0207 (5)	0.000	0.000	−0.0021 (4)
Sn1	0.0069 (4)	0.0080 (5)	0.0079 (5)	0.000	0.000	0.0016 (4)
S1	0.012 (3)	0.010 (2)	0.005 (3)	0.000	0.000	−0.0009 (18)
S2	0.007 (2)	0.013 (2)	0.010 (2)	0.000	0.000	−0.004 (2)
S3	0.006 (2)	0.010 (2)	0.010 (3)	0.000	0.000	−0.002 (2)
S4	0.008 (2)	0.008 (2)	0.010 (2)	0.000	0.000	0.0019 (18)
S5	0.009 (2)	0.014 (2)	0.006 (2)	0.000	0.000	0.0020 (17)
S6	0.008 (2)	0.009 (2)	0.008 (2)	0.000	0.000	0.0006 (16)
S7	0.008 (2)	0.014 (2)	0.014 (3)	0.000	0.000	−0.006 (2)
S8	0.011 (2)	0.012 (2)	0.009 (2)	0.000	0.000	−0.0014 (16)
S9	0.009 (2)	0.021 (3)	0.013 (2)	0.000	0.000	−0.0090 (18)
S10	0.009 (2)	0.029 (3)	0.012 (2)	0.000	0.000	−0.011 (2)
S11	0.010 (2)	0.007 (2)	0.007 (2)	0.000	0.000	0.0045 (17)
S12	0.013 (2)	0.012 (2)	0.009 (2)	0.000	0.000	0.001 (2)
S13	0.013 (2)	0.008 (2)	0.008 (2)	0.000	0.000	0.0007 (18)
O14	0.023 (4)	0.022 (5)	0.056 (6)	0.000	0.000	−0.004 (4)
S14	0.023 (4)	0.022 (5)	0.056 (6)	0.000	0.000	−0.004 (4)

Geometric parameters (Å, º) top

Dy1—S8	2.711 (4)	Dy7—S13^vii	2.940 (3)
Dy1—S9ⁱ	2.735 (5)	Dy7—S13^viii	2.940 (3)
Dy1—S3	2.769 (3)	Dy7—Dy7ⁱⁱ	3.7822 (8)
Dy1—S3ⁱⁱ	2.769 (3)	Dy7—Dy7ⁱⁱⁱ	3.7822 (8)
Dy1—S6ⁱⁱ	2.772 (3)	Dy7—Dy1^xii	3.9078 (15)
Dy1—S6	2.772 (3)	Dy8—S8ⁱⁱⁱ	2.739 (3)
Dy1—S11	2.784 (4)	Dy8—S8	2.739 (3)
Dy1—Dy1ⁱⁱ	3.7822 (8)	Dy8—S14^v	2.770 (8)
Dy1—Dy1ⁱⁱⁱ	3.7822 (8)	Dy8—O14^v	2.770 (8)
Dy1—Dy5	3.8567 (14)	Dy8—S7	2.852 (4)
Dy1—Dy7^iv	3.9078 (15)	Dy8—S7ⁱⁱⁱ	2.852 (4)
Dy2—S14^v	2.399 (5)	Dy8—S4^iv	2.861 (3)
Dy2—O14^v	2.399 (5)	Dy8—S4^xiii	2.861 (3)
Dy2—S14^vi	2.399 (5)	Dy8—S6	2.960 (4)
Dy2—O14^vi	2.399 (5)	Dy8—Dy8ⁱⁱ	3.7822 (8)
Dy2—S7	2.873 (5)	Dy8—Dy8ⁱⁱⁱ	3.7822 (8)
Dy2—S5	2.914 (5)	Dy8—Dy3^v	3.8753 (14)
Dy2—S1^vii	2.940 (3)	Sn1—S12	2.481 (5)
Dy2—S1^viii	2.940 (3)	Sn1—S13	2.498 (5)
Dy2—S2	2.976 (4)	Sn1—S10^vi	2.529 (3)
Dy2—S2ⁱⁱ	2.976 (4)	Sn1—S10^v	2.529 (3)
Dy2—Dy2ⁱⁱ	3.7822 (8)	Sn1—S9	2.537 (3)
Dy2—Dy2ⁱⁱⁱ	3.7822 (8)	Sn1—S9ⁱⁱ	2.537 (3)
Dy3—O14	2.508 (7)	S1—Dy6^vi	2.802 (3)
Dy3—S5^viii	2.765 (3)	S1—Dy6^v	2.802 (3)
Dy3—S5^vii	2.765 (3)	S1—Dy2^v	2.940 (3)
Dy3—S10	2.807 (5)	S1—Dy2^vi	2.940 (3)
Dy3—S8^vii	2.841 (3)	S2—Dy7ⁱⁱⁱ	2.794 (4)
Dy3—S8^viii	2.841 (3)	S2—Dy4^v	2.846 (5)
Dy3—S11^viii	2.897 (3)	S2—Dy2ⁱⁱⁱ	2.976 (4)
Dy3—S11^vii	2.897 (3)	S3—Dy1ⁱⁱⁱ	2.769 (3)
Dy3—Dy3ⁱⁱ	3.7822 (8)	S3—Dy5ⁱⁱⁱ	2.803 (4)
Dy3—Dy3ⁱⁱⁱ	3.7822 (8)	S3—Dy6^v	2.876 (5)
Dy3—Dy8^vii	3.8753 (14)	S4—Dy4^v	2.831 (3)
Dy4—S5^vii	2.760 (3)	S4—Dy4^vi	2.831 (3)
Dy4—S5^viii	2.760 (3)	S4—Dy8^xi	2.861 (3)
Dy4—S4^viii	2.831 (3)	S4—Dy8^xii	2.861 (3)
Dy4—S4^vii	2.831 (3)	S5—Dy4^v	2.760 (3)
Dy4—S2^vii	2.846 (5)	S5—Dy4^vi	2.760 (3)
Dy4—S12^viii	2.960 (4)	S5—Dy3^vi	2.765 (3)
Dy4—S12^vii	2.960 (4)	S5—Dy3^v	2.765 (3)
Dy4—Dy4ⁱⁱⁱ	3.7822 (8)	S6—Dy1ⁱⁱⁱ	2.772 (3)
Dy4—Dy4ⁱⁱ	3.7822 (8)	S6—Dy7^iv	2.813 (3)
Dy4—Dy8^ix	3.9612 (17)	S6—Dy7^xiii	2.813 (3)
Dy5—S7^v	2.794 (4)	S7—Dy5^vii	2.794 (4)
Dy5—S7^vi	2.794 (4)	S7—Dy5^viii	2.794 (4)
Dy5—S3	2.803 (4)	S7—Dy8ⁱⁱ	2.852 (4)
Dy5—S3ⁱⁱ	2.803 (4)	S8—Dy8ⁱⁱ	2.739 (3)
Dy5—S1	2.892 (5)	S8—Dy3^v	2.841 (3)
Dy5—S12^x	2.944 (4)	S8—Dy3^vi	2.841 (3)
Dy5—S12ⁱ	2.944 (4)	S9—Sn1ⁱⁱⁱ	2.537 (3)
Dy5—S9ⁱ	3.145 (5)	S9—Dy1^xiv	2.735 (5)
Dy5—Dy5ⁱⁱ	3.7822 (8)	S9—Dy5^xiv	3.145 (5)
Dy5—Dy5ⁱⁱⁱ	3.7822 (8)	S10—Sn1^viii	2.529 (3)
Dy5—Dy8^vi	3.9649 (15)	S10—Sn1^vii	2.529 (3)
Dy6—S11^vii	2.773 (3)	S11—Dy6^v	2.773 (3)
Dy6—S11^viii	2.773 (3)	S11—Dy6^vi	2.773 (3)
Dy6—S1^viii	2.802 (3)	S11—Dy3^vi	2.897 (3)
Dy6—S1^vii	2.802 (3)	S11—Dy3^v	2.897 (3)
Dy6—S3^vii	2.876 (5)	S12—Dy5^xiv	2.944 (4)
Dy6—S13^viii	2.939 (3)	S12—Dy5^xv	2.944 (4)
Dy6—S13^vii	2.939 (3)	S12—Dy4^vi	2.960 (4)
Dy6—S10	3.145 (5)	S12—Dy4^v	2.960 (4)
Dy6—Dy6ⁱⁱⁱ	3.7822 (8)	S13—Dy6^vi	2.939 (3)
Dy6—Dy6ⁱⁱ	3.7822 (8)	S13—Dy6^v	2.939 (3)
Dy7—S2	2.794 (4)	S13—Dy7^v	2.940 (3)
Dy7—S2ⁱⁱ	2.794 (4)	S13—Dy7^vi	2.940 (3)
Dy7—S6^xi	2.813 (3)	O14—Dy2^vii	2.399 (5)
Dy7—S6^xii	2.813 (3)	O14—Dy2^viii	2.399 (5)
Dy7—S4	2.837 (5)	O14—Dy8^vii	2.770 (8)

S8—Dy1—S9ⁱ	146.41 (14)	S11^vii—Dy6—S1^viii	149.95 (14)
S8—Dy1—S3	124.06 (10)	S11^viii—Dy6—S1^viii	86.85 (10)
S9ⁱ—Dy1—S3	78.05 (13)	S11^vii—Dy6—S1^vii	86.85 (9)
S8—Dy1—S3ⁱⁱ	124.06 (10)	S11^viii—Dy6—S1^vii	149.95 (14)
S9ⁱ—Dy1—S3ⁱⁱ	78.05 (13)	S1^viii—Dy6—S1^vii	84.89 (12)
S3—Dy1—S3ⁱⁱ	86.14 (13)	S11^vii—Dy6—S3^vii	75.16 (11)
S8—Dy1—S6ⁱⁱ	76.95 (11)	S11^viii—Dy6—S3^vii	75.16 (11)
S9ⁱ—Dy1—S6ⁱⁱ	78.66 (12)	S1^viii—Dy6—S3^vii	74.79 (12)
S3—Dy1—S6ⁱⁱ	156.70 (14)	S1^vii—Dy6—S3^vii	74.79 (12)
S3ⁱⁱ—Dy1—S6ⁱⁱ	89.24 (10)	S11^vii—Dy6—S13^viii	138.49 (12)
S8—Dy1—S6	76.95 (11)	S11^viii—Dy6—S13^viii	82.60 (10)
S9ⁱ—Dy1—S6	78.66 (12)	S1^viii—Dy6—S13^viii	68.99 (11)
S3—Dy1—S6	89.24 (10)	S1^vii—Dy6—S13^viii	120.66 (12)
S3ⁱⁱ—Dy1—S6	156.70 (14)	S3^vii—Dy6—S13^viii	138.20 (6)
S6ⁱⁱ—Dy1—S6	86.02 (13)	S11^vii—Dy6—S13^vii	82.60 (10)
S8—Dy1—S11	68.38 (12)	S11^viii—Dy6—S13^vii	138.49 (12)
S9ⁱ—Dy1—S11	145.21 (13)	S1^viii—Dy6—S13^vii	120.66 (12)
S3—Dy1—S11	76.72 (12)	S1^vii—Dy6—S13^vii	68.99 (11)
S3ⁱⁱ—Dy1—S11	76.72 (12)	S3^vii—Dy6—S13^vii	138.20 (6)
S6ⁱⁱ—Dy1—S11	124.29 (10)	S13^viii—Dy6—S13^vii	80.09 (11)
S6—Dy1—S11	124.29 (10)	S11^vii—Dy6—S10	67.46 (10)
S8—Dy1—Dy1ⁱⁱ	90.0	S11^viii—Dy6—S10	67.46 (10)
S9ⁱ—Dy1—Dy1ⁱⁱ	90.0	S1^viii—Dy6—S10	134.86 (8)
S3—Dy1—Dy1ⁱⁱ	133.07 (7)	S1^vii—Dy6—S10	134.86 (8)
S3ⁱⁱ—Dy1—Dy1ⁱⁱ	46.93 (7)	S3^vii—Dy6—S10	127.89 (13)
S6ⁱⁱ—Dy1—Dy1ⁱⁱ	46.99 (6)	S13^viii—Dy6—S10	71.30 (10)
S6—Dy1—Dy1ⁱⁱ	133.01 (6)	S13^vii—Dy6—S10	71.30 (10)
S11—Dy1—Dy1ⁱⁱ	90.0	S11^vii—Dy6—Dy6ⁱⁱⁱ	133.00 (6)
S8—Dy1—Dy1ⁱⁱⁱ	90.0	S11^viii—Dy6—Dy6ⁱⁱⁱ	47.00 (6)
S9ⁱ—Dy1—Dy1ⁱⁱⁱ	90.0	S1^viii—Dy6—Dy6ⁱⁱⁱ	47.55 (6)
S3—Dy1—Dy1ⁱⁱⁱ	46.93 (7)	S1^vii—Dy6—Dy6ⁱⁱⁱ	132.45 (6)
S3ⁱⁱ—Dy1—Dy1ⁱⁱⁱ	133.07 (7)	S3^vii—Dy6—Dy6ⁱⁱⁱ	90.0
S6ⁱⁱ—Dy1—Dy1ⁱⁱⁱ	133.01 (6)	S13^viii—Dy6—Dy6ⁱⁱⁱ	49.95 (5)
S6—Dy1—Dy1ⁱⁱⁱ	46.99 (6)	S13^vii—Dy6—Dy6ⁱⁱⁱ	130.05 (5)
S11—Dy1—Dy1ⁱⁱⁱ	90.0	S10—Dy6—Dy6ⁱⁱⁱ	90.0
Dy1ⁱⁱ—Dy1—Dy1ⁱⁱⁱ	180.00 (5)	S11^vii—Dy6—Dy6ⁱⁱ	47.00 (6)
S8—Dy1—Dy5	159.81 (9)	S11^viii—Dy6—Dy6ⁱⁱ	133.00 (6)
S9ⁱ—Dy1—Dy5	53.78 (10)	S1^viii—Dy6—Dy6ⁱⁱ	132.45 (6)
S3—Dy1—Dy5	46.56 (8)	S1^vii—Dy6—Dy6ⁱⁱ	47.55 (6)
S3ⁱⁱ—Dy1—Dy5	46.56 (8)	S3^vii—Dy6—Dy6ⁱⁱ	90.0
S6ⁱⁱ—Dy1—Dy5	116.87 (9)	S13^viii—Dy6—Dy6ⁱⁱ	130.05 (5)
S6—Dy1—Dy5	116.87 (9)	S13^vii—Dy6—Dy6ⁱⁱ	49.95 (5)
S11—Dy1—Dy5	91.43 (9)	S10—Dy6—Dy6ⁱⁱ	90.0
Dy1ⁱⁱ—Dy1—Dy5	90.0	Dy6ⁱⁱⁱ—Dy6—Dy6ⁱⁱ	180.00 (5)
Dy1ⁱⁱⁱ—Dy1—Dy5	90.0	S2—Dy7—S2ⁱⁱ	85.20 (14)
S8—Dy1—Dy7^iv	90.29 (9)	S2—Dy7—S6^xi	87.83 (11)
S9ⁱ—Dy1—Dy7^iv	56.12 (10)	S2ⁱⁱ—Dy7—S6^xi	150.73 (13)
S3—Dy1—Dy7^iv	117.79 (10)	S2—Dy7—S6^xii	150.73 (13)
S3ⁱⁱ—Dy1—Dy7^iv	117.79 (10)	S2ⁱⁱ—Dy7—S6^xii	87.83 (11)
S6ⁱⁱ—Dy1—Dy7^iv	46.02 (7)	S6^xi—Dy7—S6^xii	84.49 (13)
S6—Dy1—Dy7^iv	46.02 (7)	S2—Dy7—S4	75.80 (11)
S11—Dy1—Dy7^iv	158.67 (9)	S2ⁱⁱ—Dy7—S4	75.80 (11)
Dy1ⁱⁱ—Dy1—Dy7^iv	90.0	S6^xi—Dy7—S4	74.93 (11)
Dy1ⁱⁱⁱ—Dy1—Dy7^iv	90.0	S6^xii—Dy7—S4	74.93 (11)
Dy5—Dy1—Dy7^iv	109.91 (3)	S2—Dy7—S13^vii	119.86 (13)
S14^v—Dy2—O14^v	0.0 (5)	S2ⁱⁱ—Dy7—S13^vii	68.11 (12)
S14^v—Dy2—S14^vi	104.1 (3)	S6^xi—Dy7—S13^vii	138.30 (12)
O14^v—Dy2—S14^vi	104.1 (3)	S6^xii—Dy7—S13^vii	83.21 (10)
S14^v—Dy2—O14^vi	104.1 (3)	S4—Dy7—S13^vii	138.23 (6)
O14^v—Dy2—O14^vi	104.1 (3)	S2—Dy7—S13^viii	68.11 (12)
S14^vi—Dy2—O14^vi	0.0 (4)	S2ⁱⁱ—Dy7—S13^viii	119.86 (13)
S14^v—Dy2—S7	73.79 (19)	S6^xi—Dy7—S13^viii	83.21 (10)
O14^v—Dy2—S7	73.79 (19)	S6^xii—Dy7—S13^viii	138.30 (12)
S14^vi—Dy2—S7	73.79 (19)	S4—Dy7—S13^viii	138.23 (6)
O14^vi—Dy2—S7	73.79 (19)	S13^vii—Dy7—S13^viii	80.06 (11)
S14^v—Dy2—S5	74.03 (17)	S2—Dy7—Dy7ⁱⁱ	132.60 (7)
O14^v—Dy2—S5	74.03 (17)	S2ⁱⁱ—Dy7—Dy7ⁱⁱ	47.40 (7)
S14^vi—Dy2—S5	74.03 (17)	S6^xi—Dy7—Dy7ⁱⁱ	132.25 (6)
O14^vi—Dy2—S5	74.03 (17)	S6^xii—Dy7—Dy7ⁱⁱ	47.75 (6)
S7—Dy2—S5	126.46 (14)	S4—Dy7—Dy7ⁱⁱ	90.0
S14^v—Dy2—S1^vii	144.2 (2)	S13^vii—Dy7—Dy7ⁱⁱ	49.97 (6)
O14^v—Dy2—S1^vii	144.2 (2)	S13^viii—Dy7—Dy7ⁱⁱ	130.03 (6)
S14^vi—Dy2—S1^vii	78.26 (16)	S2—Dy7—Dy7ⁱⁱⁱ	47.40 (7)
O14^vi—Dy2—S1^vii	78.26 (16)	S2ⁱⁱ—Dy7—Dy7ⁱⁱⁱ	132.60 (7)
S7—Dy2—S1^vii	72.68 (12)	S6^xi—Dy7—Dy7ⁱⁱⁱ	47.75 (6)
S5—Dy2—S1^vii	138.10 (7)	S6^xii—Dy7—Dy7ⁱⁱⁱ	132.25 (6)
S14^v—Dy2—S1^viii	78.26 (16)	S4—Dy7—Dy7ⁱⁱⁱ	90.0
O14^v—Dy2—S1^viii	78.26 (16)	S13^vii—Dy7—Dy7ⁱⁱⁱ	130.03 (6)
S14^vi—Dy2—S1^viii	144.2 (2)	S13^viii—Dy7—Dy7ⁱⁱⁱ	49.97 (6)
O14^vi—Dy2—S1^viii	144.2 (2)	Dy7ⁱⁱ—Dy7—Dy7ⁱⁱⁱ	180.00 (8)
S7—Dy2—S1^viii	72.68 (12)	S2—Dy7—Dy1^xii	132.94 (8)
S5—Dy2—S1^viii	138.10 (7)	S2ⁱⁱ—Dy7—Dy1^xii	132.94 (8)
S1^vii—Dy2—S1^viii	80.07 (11)	S6^xi—Dy7—Dy1^xii	45.18 (7)
S14^v—Dy2—S2	78.71 (18)	S6^xii—Dy7—Dy1^xii	45.18 (7)
O14^v—Dy2—S2	78.71 (18)	S4—Dy7—Dy1^xii	87.21 (9)
S14^vi—Dy2—S2	143.7 (2)	S13^vii—Dy7—Dy1^xii	102.10 (8)
O14^vi—Dy2—S2	143.7 (2)	S13^viii—Dy7—Dy1^xii	102.10 (8)
S7—Dy2—S2	138.79 (7)	Dy7ⁱⁱ—Dy7—Dy1^xii	90.0
S5—Dy2—S2	72.10 (11)	Dy7ⁱⁱⁱ—Dy7—Dy1^xii	90.0
S1^vii—Dy2—S2	120.68 (12)	S8ⁱⁱⁱ—Dy8—S8	87.33 (13)
S1^viii—Dy2—S2	72.10 (11)	S8ⁱⁱⁱ—Dy8—S14^v	68.79 (14)
S14^v—Dy2—S2ⁱⁱ	143.7 (2)	S8—Dy8—S14^v	68.79 (14)
O14^v—Dy2—S2ⁱⁱ	143.7 (2)	S8ⁱⁱⁱ—Dy8—O14^v	68.79 (14)
S14^vi—Dy2—S2ⁱⁱ	78.71 (18)	S8—Dy8—O14^v	68.79 (14)
O14^vi—Dy2—S2ⁱⁱ	78.71 (18)	S14^v—Dy8—O14^v	0.0 (3)
S7—Dy2—S2ⁱⁱ	138.79 (7)	S8ⁱⁱⁱ—Dy8—S7	137.78 (12)
S5—Dy2—S2ⁱⁱ	72.10 (11)	S8—Dy8—S7	79.92 (11)
S1^vii—Dy2—S2ⁱⁱ	72.10 (11)	S14^v—Dy8—S7	69.06 (15)
S1^viii—Dy2—S2ⁱⁱ	120.68 (12)	O14^v—Dy8—S7	69.06 (15)
S2—Dy2—S2ⁱⁱ	78.91 (12)	S8ⁱⁱⁱ—Dy8—S7ⁱⁱⁱ	79.92 (11)
S14^v—Dy2—Dy2ⁱⁱ	142.03 (14)	S8—Dy8—S7ⁱⁱⁱ	137.78 (12)
O14^v—Dy2—Dy2ⁱⁱ	142.03 (14)	S14^v—Dy8—S7ⁱⁱⁱ	69.06 (15)
S14^vi—Dy2—Dy2ⁱⁱ	37.97 (14)	O14^v—Dy8—S7ⁱⁱⁱ	69.06 (15)
O14^vi—Dy2—Dy2ⁱⁱ	37.97 (14)	S7—Dy8—S7ⁱⁱⁱ	83.07 (13)
S7—Dy2—Dy2ⁱⁱ	90.0	S8ⁱⁱⁱ—Dy8—S4^iv	145.71 (13)
S5—Dy2—Dy2ⁱⁱ	90.0	S8—Dy8—S4^iv	85.03 (10)
S1^vii—Dy2—Dy2ⁱⁱ	49.97 (6)	S14^v—Dy8—S4^iv	136.99 (8)
S1^viii—Dy2—Dy2ⁱⁱ	130.03 (6)	O14^v—Dy8—S4^iv	136.99 (8)
S2—Dy2—Dy2ⁱⁱ	129.46 (6)	S7—Dy8—S4^iv	73.29 (12)
S2ⁱⁱ—Dy2—Dy2ⁱⁱ	50.54 (6)	S7ⁱⁱⁱ—Dy8—S4^iv	126.09 (13)
S14^v—Dy2—Dy2ⁱⁱⁱ	37.97 (14)	S8ⁱⁱⁱ—Dy8—S4^xiii	85.03 (10)
O14^v—Dy2—Dy2ⁱⁱⁱ	37.97 (14)	S8—Dy8—S4^xiii	145.71 (13)
S14^vi—Dy2—Dy2ⁱⁱⁱ	142.03 (14)	S14^v—Dy8—S4^xiii	136.99 (8)
O14^vi—Dy2—Dy2ⁱⁱⁱ	142.03 (14)	O14^v—Dy8—S4^xiii	136.99 (8)
S7—Dy2—Dy2ⁱⁱⁱ	90.0	S7—Dy8—S4^xiii	126.09 (13)
S5—Dy2—Dy2ⁱⁱⁱ	90.0	S7ⁱⁱⁱ—Dy8—S4^xiii	73.29 (12)
S1^vii—Dy2—Dy2ⁱⁱⁱ	130.03 (6)	S4^iv—Dy8—S4^xiii	82.77 (12)
S1^viii—Dy2—Dy2ⁱⁱⁱ	49.97 (6)	S8ⁱⁱⁱ—Dy8—S6	73.43 (10)
S2—Dy2—Dy2ⁱⁱⁱ	50.54 (6)	S8—Dy8—S6	73.43 (10)
S2ⁱⁱ—Dy2—Dy2ⁱⁱⁱ	129.46 (6)	S14^v—Dy8—S6	126.78 (17)
Dy2ⁱⁱ—Dy2—Dy2ⁱⁱⁱ	180.00 (6)	O14^v—Dy8—S6	126.78 (17)
O14—Dy3—S5^viii	75.25 (16)	S7—Dy8—S6	137.80 (7)
O14—Dy3—S5^vii	75.25 (16)	S7ⁱⁱⁱ—Dy8—S6	137.80 (7)
S5^viii—Dy3—S5^vii	86.32 (13)	S4^iv—Dy8—S6	72.35 (11)
O14—Dy3—S10	140.5 (2)	S4^xiii—Dy8—S6	72.35 (11)
S5^viii—Dy3—S10	76.23 (12)	S8ⁱⁱⁱ—Dy8—Dy8ⁱⁱ	133.66 (6)
S5^vii—Dy3—S10	76.23 (12)	S8—Dy8—Dy8ⁱⁱ	46.34 (6)
O14—Dy3—S8^vii	70.86 (16)	S14^v—Dy8—Dy8ⁱⁱ	90.0
S5^viii—Dy3—S8^vii	146.11 (13)	O14^v—Dy8—Dy8ⁱⁱ	90.0
S5^vii—Dy3—S8^vii	85.38 (10)	S7—Dy8—Dy8ⁱⁱ	48.47 (7)
S10—Dy3—S8^vii	132.79 (8)	S7ⁱⁱⁱ—Dy8—Dy8ⁱⁱ	131.53 (7)
O14—Dy3—S8^viii	70.86 (16)	S4^iv—Dy8—Dy8ⁱⁱ	48.62 (6)
S5^viii—Dy3—S8^viii	85.38 (10)	S4^xiii—Dy8—Dy8ⁱⁱ	131.38 (6)
S5^vii—Dy3—S8^viii	146.11 (13)	S6—Dy8—Dy8ⁱⁱ	90.0
S10—Dy3—S8^viii	132.79 (8)	S8ⁱⁱⁱ—Dy8—Dy8ⁱⁱⁱ	46.34 (6)
S8^vii—Dy3—S8^viii	83.46 (11)	S8—Dy8—Dy8ⁱⁱⁱ	133.66 (6)
O14—Dy3—S11^viii	133.50 (11)	S14^v—Dy8—Dy8ⁱⁱⁱ	90.0
S5^viii—Dy3—S11^viii	86.83 (9)	O14^v—Dy8—Dy8ⁱⁱⁱ	90.0
S5^vii—Dy3—S11^viii	146.92 (13)	S7—Dy8—Dy8ⁱⁱⁱ	131.53 (7)
S10—Dy3—S11^viii	70.70 (11)	S7ⁱⁱⁱ—Dy8—Dy8ⁱⁱⁱ	48.47 (7)
S8^vii—Dy3—S11^viii	116.65 (11)	S4^iv—Dy8—Dy8ⁱⁱⁱ	131.38 (6)
S8^viii—Dy3—S11^viii	65.12 (11)	S4^xiii—Dy8—Dy8ⁱⁱⁱ	48.62 (6)
O14—Dy3—S11^vii	133.50 (11)	S6—Dy8—Dy8ⁱⁱⁱ	90.0
S5^viii—Dy3—S11^vii	146.92 (13)	Dy8ⁱⁱ—Dy8—Dy8ⁱⁱⁱ	180.0
S5^vii—Dy3—S11^vii	86.83 (9)	S8ⁱⁱⁱ—Dy8—Dy3^v	47.11 (7)
S10—Dy3—S11^vii	70.70 (11)	S8—Dy8—Dy3^v	47.11 (7)
S8^vii—Dy3—S11^vii	65.12 (11)	S14^v—Dy8—Dy3^v	40.19 (15)
S8^viii—Dy3—S11^vii	116.65 (11)	O14^v—Dy8—Dy3^v	40.19 (15)
S11^viii—Dy3—S11^vii	81.52 (11)	S7—Dy8—Dy3^v	98.71 (10)
O14—Dy3—Dy3ⁱⁱ	90.0	S7ⁱⁱⁱ—Dy8—Dy3^v	98.71 (10)
S5^viii—Dy3—Dy3ⁱⁱ	133.16 (6)	S4^iv—Dy8—Dy3^v	131.84 (7)
S5^vii—Dy3—Dy3ⁱⁱ	46.84 (6)	S4^xiii—Dy8—Dy3^v	131.84 (7)
S10—Dy3—Dy3ⁱⁱ	90.0	S6—Dy8—Dy3^v	86.59 (9)
S8^vii—Dy3—Dy3ⁱⁱ	48.27 (6)	Dy8ⁱⁱ—Dy8—Dy3^v	90.0
S8^viii—Dy3—Dy3ⁱⁱ	131.73 (6)	Dy8ⁱⁱⁱ—Dy8—Dy3^v	90.0
S11^viii—Dy3—Dy3ⁱⁱ	130.76 (5)	S12—Sn1—S13	177.64 (19)
S11^vii—Dy3—Dy3ⁱⁱ	49.24 (5)	S12—Sn1—S10^vi	91.72 (15)
O14—Dy3—Dy3ⁱⁱⁱ	90.0	S13—Sn1—S10^vi	89.85 (14)
S5^viii—Dy3—Dy3ⁱⁱⁱ	46.84 (6)	S12—Sn1—S10^v	91.72 (15)
S5^vii—Dy3—Dy3ⁱⁱⁱ	133.16 (6)	S13—Sn1—S10^v	89.85 (14)
S10—Dy3—Dy3ⁱⁱⁱ	90.0	S10^vi—Sn1—S10^v	96.82 (16)
S8^vii—Dy3—Dy3ⁱⁱⁱ	131.73 (6)	S12—Sn1—S9	88.85 (14)
S8^viii—Dy3—Dy3ⁱⁱⁱ	48.27 (6)	S13—Sn1—S9	89.58 (14)
S11^viii—Dy3—Dy3ⁱⁱⁱ	49.24 (5)	S10^vi—Sn1—S9	179.39 (19)
S11^vii—Dy3—Dy3ⁱⁱⁱ	130.76 (5)	S10^v—Sn1—S9	83.40 (8)
Dy3ⁱⁱ—Dy3—Dy3ⁱⁱⁱ	180.00 (3)	S12—Sn1—S9ⁱⁱ	88.85 (14)
O14—Dy3—Dy8^vii	45.47 (18)	S13—Sn1—S9ⁱⁱ	89.58 (13)
S5^viii—Dy3—Dy8^vii	107.98 (9)	S10^vi—Sn1—S9ⁱⁱ	83.40 (8)
S5^vii—Dy3—Dy8^vii	107.98 (9)	S10^v—Sn1—S9ⁱⁱ	179.39 (19)
S10—Dy3—Dy8^vii	174.01 (11)	S9—Sn1—S9ⁱⁱ	96.38 (16)
S8^vii—Dy3—Dy8^vii	44.94 (7)	Dy6^vi—S1—Dy6^v	84.89 (12)
S8^viii—Dy3—Dy8^vii	44.94 (7)	Dy6^vi—S1—Dy5	105.14 (12)
S11^viii—Dy3—Dy8^vii	104.92 (9)	Dy6^v—S1—Dy5	105.14 (12)
S11^vii—Dy3—Dy8^vii	104.92 (8)	Dy6^vi—S1—Dy2^v	150.61 (19)
Dy3ⁱⁱ—Dy3—Dy8^vii	90.0	Dy6^v—S1—Dy2^v	90.17 (6)
Dy3ⁱⁱⁱ—Dy3—Dy8^vii	90.0	Dy5—S1—Dy2^v	104.12 (12)
S5^vii—Dy4—S5^viii	86.51 (13)	Dy6^vi—S1—Dy2^vi	90.17 (6)
S5^vii—Dy4—S4^viii	151.45 (13)	Dy6^v—S1—Dy2^vi	150.61 (19)
S5^viii—Dy4—S4^viii	87.87 (10)	Dy5—S1—Dy2^vi	104.12 (12)
S5^vii—Dy4—S4^vii	87.87 (10)	Dy2^v—S1—Dy2^vi	80.07 (11)
S5^viii—Dy4—S4^vii	151.45 (13)	Dy7—S2—Dy7ⁱⁱⁱ	85.20 (14)
S4^viii—Dy4—S4^vii	83.83 (12)	Dy7—S2—Dy4^v	104.92 (13)
S5^vii—Dy4—S2^vii	76.38 (11)	Dy7ⁱⁱⁱ—S2—Dy4^v	104.92 (13)
S5^viii—Dy4—S2^vii	76.38 (11)	Dy7—S2—Dy2	90.90 (5)
S4^viii—Dy4—S2^vii	75.09 (11)	Dy7ⁱⁱⁱ—S2—Dy2	151.17 (18)
S4^vii—Dy4—S2^vii	75.09 (11)	Dy4^v—S2—Dy2	103.69 (13)
S5^vii—Dy4—S12^viii	137.58 (12)	Dy7—S2—Dy2ⁱⁱⁱ	151.17 (18)
S5^viii—Dy4—S12^viii	82.10 (11)	Dy7ⁱⁱⁱ—S2—Dy2ⁱⁱⁱ	90.90 (5)
S4^viii—Dy4—S12^viii	68.88 (12)	Dy4^v—S2—Dy2ⁱⁱⁱ	103.69 (13)
S4^vii—Dy4—S12^viii	119.56 (13)	Dy2—S2—Dy2ⁱⁱⁱ	78.91 (12)
S2^vii—Dy4—S12^viii	138.40 (7)	Dy1—S3—Dy1ⁱⁱⁱ	86.14 (13)
S5^vii—Dy4—S12^vii	82.10 (11)	Dy1—S3—Dy5ⁱⁱⁱ	151.58 (19)
S5^viii—Dy4—S12^vii	137.58 (12)	Dy1ⁱⁱⁱ—S3—Dy5ⁱⁱⁱ	87.60 (5)
S4^viii—Dy4—S12^vii	119.56 (13)	Dy1—S3—Dy5	87.60 (5)
S4^vii—Dy4—S12^vii	68.88 (12)	Dy1ⁱⁱⁱ—S3—Dy5	151.58 (19)
S2^vii—Dy4—S12^vii	138.40 (7)	Dy5ⁱⁱⁱ—S3—Dy5	84.86 (13)
S12^viii—Dy4—S12^vii	79.43 (12)	Dy1—S3—Dy6^v	102.89 (13)
S5^vii—Dy4—Dy4ⁱⁱⁱ	133.25 (7)	Dy1ⁱⁱⁱ—S3—Dy6^v	102.89 (13)
S5^viii—Dy4—Dy4ⁱⁱⁱ	46.75 (7)	Dy5ⁱⁱⁱ—S3—Dy6^v	105.53 (13)
S4^viii—Dy4—Dy4ⁱⁱⁱ	48.09 (6)	Dy5—S3—Dy6^v	105.53 (13)
S4^vii—Dy4—Dy4ⁱⁱⁱ	131.91 (6)	Dy4^v—S4—Dy4^vi	83.83 (12)
S2^vii—Dy4—Dy4ⁱⁱⁱ	90.0	Dy4^v—S4—Dy7	104.18 (12)
S12^viii—Dy4—Dy4ⁱⁱⁱ	50.28 (6)	Dy4^vi—S4—Dy7	104.18 (12)
S12^vii—Dy4—Dy4ⁱⁱⁱ	129.72 (6)	Dy4^v—S4—Dy8^xi	88.21 (5)
S5^vii—Dy4—Dy4ⁱⁱ	46.75 (7)	Dy4^vi—S4—Dy8^xi	148.43 (17)
S5^viii—Dy4—Dy4ⁱⁱ	133.25 (7)	Dy7—S4—Dy8^xi	107.38 (12)
S4^viii—Dy4—Dy4ⁱⁱ	131.91 (6)	Dy4^v—S4—Dy8^xii	148.43 (17)
S4^vii—Dy4—Dy4ⁱⁱ	48.09 (6)	Dy4^vi—S4—Dy8^xii	88.21 (5)
S2^vii—Dy4—Dy4ⁱⁱ	90.0	Dy7—S4—Dy8^xii	107.38 (12)
S12^viii—Dy4—Dy4ⁱⁱ	129.72 (6)	Dy8^xi—S4—Dy8^xii	82.77 (12)
S12^vii—Dy4—Dy4ⁱⁱ	50.28 (6)	Dy4^v—S5—Dy4^vi	86.51 (13)
Dy4ⁱⁱⁱ—Dy4—Dy4ⁱⁱ	180.00 (5)	Dy4^v—S5—Dy3^vi	159.03 (18)
S5^vii—Dy4—Dy3	45.15 (7)	Dy4^vi—S5—Dy3^vi	89.79 (4)
S5^viii—Dy4—Dy3	45.15 (7)	Dy4^v—S5—Dy3^v	89.79 (4)
S4^viii—Dy4—Dy3	132.57 (7)	Dy4^vi—S5—Dy3^v	159.03 (18)
S4^vii—Dy4—Dy3	132.57 (7)	Dy3^vi—S5—Dy3^v	86.32 (13)
S2^vii—Dy4—Dy3	85.62 (10)	Dy4^v—S5—Dy2	107.56 (12)
S12^viii—Dy4—Dy3	103.71 (10)	Dy4^vi—S5—Dy2	107.56 (12)
S12^vii—Dy4—Dy3	103.71 (10)	Dy3^vi—S5—Dy2	93.24 (12)
Dy4ⁱⁱⁱ—Dy4—Dy3	90.0	Dy3^v—S5—Dy2	93.24 (12)
Dy4ⁱⁱ—Dy4—Dy3	90.0	Dy1ⁱⁱⁱ—S6—Dy1	86.02 (13)
S5^vii—Dy4—Dy8^ix	133.99 (7)	Dy1ⁱⁱⁱ—S6—Dy7^iv	153.67 (17)
S5^viii—Dy4—Dy8^ix	133.99 (7)	Dy1—S6—Dy7^iv	88.80 (5)
S4^viii—Dy4—Dy8^ix	46.20 (7)	Dy1ⁱⁱⁱ—S6—Dy7^xiii	88.80 (5)
S4^vii—Dy4—Dy8^ix	46.20 (7)	Dy1—S6—Dy7^xiii	153.67 (17)
S2^vii—Dy4—Dy8^ix	91.32 (10)	Dy7^iv—S6—Dy7^xiii	84.49 (13)
S12^viii—Dy4—Dy8^ix	78.60 (10)	Dy1ⁱⁱⁱ—S6—Dy8	100.99 (12)
S12^vii—Dy4—Dy8^ix	78.60 (10)	Dy1—S6—Dy8	100.99 (12)
Dy4ⁱⁱⁱ—Dy4—Dy8^ix	90.0	Dy7^iv—S6—Dy8	105.34 (11)
Dy4ⁱⁱ—Dy4—Dy8^ix	90.0	Dy7^xiii—S6—Dy8	105.34 (11)
Dy3—Dy4—Dy8^ix	176.94 (3)	Dy5^vii—S7—Dy5^viii	85.19 (13)
S7^v—Dy5—S7^vi	85.19 (13)	Dy5^vii—S7—Dy8ⁱⁱ	89.21 (5)
S7^v—Dy5—S3	86.84 (11)	Dy5^viii—S7—Dy8ⁱⁱ	152.1 (2)
S7^vi—Dy5—S3	149.10 (16)	Dy5^vii—S7—Dy8	152.1 (2)
S7^v—Dy5—S3ⁱⁱ	149.10 (16)	Dy5^viii—S7—Dy8	89.21 (5)
S7^vi—Dy5—S3ⁱⁱ	86.84 (11)	Dy8ⁱⁱ—S7—Dy8	83.07 (13)
S3—Dy5—S3ⁱⁱ	84.86 (13)	Dy5^vii—S7—Dy2	108.48 (14)
S7^v—Dy5—S1	74.57 (12)	Dy5^viii—S7—Dy2	108.48 (14)
S7^vi—Dy5—S1	74.57 (12)	Dy8ⁱⁱ—S7—Dy2	99.23 (13)
S3—Dy5—S1	74.54 (12)	Dy8—S7—Dy2	99.23 (13)
S3ⁱⁱ—Dy5—S1	74.54 (12)	Dy1—S8—Dy8ⁱⁱ	108.55 (12)
S7^v—Dy5—S12^x	118.62 (13)	Dy1—S8—Dy8	108.55 (12)
S7^vi—Dy5—S12^x	67.02 (12)	Dy8ⁱⁱ—S8—Dy8	87.33 (13)
S3—Dy5—S12^x	141.31 (14)	Dy1—S8—Dy3^v	99.06 (12)
S3ⁱⁱ—Dy5—S12^x	85.06 (11)	Dy8ⁱⁱ—S8—Dy3^v	152.05 (17)
S1—Dy5—S12^x	137.24 (8)	Dy8—S8—Dy3^v	87.95 (5)
S7^v—Dy5—S12ⁱ	67.02 (12)	Dy1—S8—Dy3^vi	99.06 (12)
S7^vi—Dy5—S12ⁱ	118.62 (13)	Dy8ⁱⁱ—S8—Dy3^vi	87.95 (5)
S3—Dy5—S12ⁱ	85.06 (11)	Dy8—S8—Dy3^vi	152.05 (17)
S3ⁱⁱ—Dy5—S12ⁱ	141.31 (14)	Dy3^v—S8—Dy3^vi	83.46 (11)
S1—Dy5—S12ⁱ	137.24 (8)	Sn1—S9—Sn1ⁱⁱⁱ	96.38 (16)
S12^x—Dy5—S12ⁱ	79.93 (13)	Sn1—S9—Dy1^xiv	131.79 (8)
S7^v—Dy5—S9ⁱ	133.23 (9)	Sn1ⁱⁱⁱ—S9—Dy1^xiv	131.79 (8)
S7^vi—Dy5—S9ⁱ	133.23 (9)	Sn1—S9—Dy5^xiv	96.74 (13)
S3—Dy5—S9ⁱ	71.02 (11)	Sn1ⁱⁱⁱ—S9—Dy5^xiv	96.74 (13)
S3ⁱⁱ—Dy5—S9ⁱ	71.02 (11)	Dy1^xiv—S9—Dy5^xiv	81.66 (13)
S1—Dy5—S9ⁱ	132.68 (13)	Sn1^viii—S10—Sn1^vii	96.82 (16)
S12^x—Dy5—S9ⁱ	70.38 (11)	Sn1^viii—S10—Dy3	131.34 (8)
S12ⁱ—Dy5—S9ⁱ	70.38 (11)	Sn1^vii—S10—Dy3	131.34 (8)
S7^v—Dy5—Dy5ⁱⁱ	132.60 (7)	Sn1^viii—S10—Dy6	96.03 (14)
S7^vi—Dy5—Dy5ⁱⁱ	47.40 (7)	Sn1^vii—S10—Dy6	96.03 (14)
S3—Dy5—Dy5ⁱⁱ	132.43 (7)	Dy3—S10—Dy6	86.55 (13)
S3ⁱⁱ—Dy5—Dy5ⁱⁱ	47.57 (7)	Dy6^v—S11—Dy6^vi	85.99 (12)
S1—Dy5—Dy5ⁱⁱ	90.0	Dy6^v—S11—Dy1	105.23 (11)
S12^x—Dy5—Dy5ⁱⁱ	50.03 (6)	Dy6^vi—S11—Dy1	105.23 (11)
S12ⁱ—Dy5—Dy5ⁱⁱ	129.97 (6)	Dy6^v—S11—Dy3^vi	158.35 (16)
S9ⁱ—Dy5—Dy5ⁱⁱ	90.0	Dy6^vi—S11—Dy3^vi	92.23 (4)
S7^v—Dy5—Dy5ⁱⁱⁱ	47.40 (7)	Dy1—S11—Dy3^vi	96.07 (11)
S7^vi—Dy5—Dy5ⁱⁱⁱ	132.60 (7)	Dy6^v—S11—Dy3^v	92.23 (4)
S3—Dy5—Dy5ⁱⁱⁱ	47.57 (7)	Dy6^vi—S11—Dy3^v	158.35 (16)
S3ⁱⁱ—Dy5—Dy5ⁱⁱⁱ	132.43 (7)	Dy1—S11—Dy3^v	96.07 (11)
S1—Dy5—Dy5ⁱⁱⁱ	90.0	Dy3^vi—S11—Dy3^v	81.52 (11)
S12^x—Dy5—Dy5ⁱⁱⁱ	129.97 (6)	Sn1—S12—Dy5^xiv	103.38 (14)
S12ⁱ—Dy5—Dy5ⁱⁱⁱ	50.03 (6)	Sn1—S12—Dy5^xv	103.38 (14)
S9ⁱ—Dy5—Dy5ⁱⁱⁱ	90.0	Dy5^xiv—S12—Dy5^xv	79.93 (13)
Dy5ⁱⁱ—Dy5—Dy5ⁱⁱⁱ	180.0	Sn1—S12—Dy4^vi	104.21 (14)
S7^v—Dy5—Dy1	132.63 (8)	Dy5^xiv—S12—Dy4^vi	152.42 (18)
S7^vi—Dy5—Dy1	132.63 (8)	Dy5^xv—S12—Dy4^vi	93.75 (5)
S3—Dy5—Dy1	45.84 (7)	Sn1—S12—Dy4^v	104.21 (14)
S3ⁱⁱ—Dy5—Dy1	45.84 (7)	Dy5^xiv—S12—Dy4^v	93.75 (5)
S1—Dy5—Dy1	88.12 (9)	Dy5^xv—S12—Dy4^v	152.42 (18)
S12^x—Dy5—Dy1	104.13 (10)	Dy4^vi—S12—Dy4^v	79.43 (12)
S12ⁱ—Dy5—Dy1	104.13 (10)	Sn1—S13—Dy6^vi	102.09 (12)
S9ⁱ—Dy5—Dy1	44.56 (9)	Sn1—S13—Dy6^v	102.09 (12)
Dy5ⁱⁱ—Dy5—Dy1	90.0	Dy6^vi—S13—Dy6^v	80.09 (11)
Dy5ⁱⁱⁱ—Dy5—Dy1	90.0	Sn1—S13—Dy7^v	105.50 (12)
S7^v—Dy5—Dy8^vi	45.99 (8)	Dy6^vi—S13—Dy7^v	152.39 (16)
S7^vi—Dy5—Dy8^vi	45.99 (8)	Dy6^v—S13—Dy7^v	93.35 (5)
S3—Dy5—Dy8^vi	132.78 (8)	Sn1—S13—Dy7^vi	105.50 (12)
S3ⁱⁱ—Dy5—Dy8^vi	132.78 (8)	Dy6^vi—S13—Dy7^vi	93.35 (5)
S1—Dy5—Dy8^vi	88.11 (9)	Dy6^v—S13—Dy7^vi	152.39 (16)
S12^x—Dy5—Dy8^vi	78.71 (9)	Dy7^v—S13—Dy7^vi	80.06 (11)
S12ⁱ—Dy5—Dy8^vi	78.71 (9)	Dy2^vii—O14—Dy2^viii	104.1 (3)
S9ⁱ—Dy5—Dy8^vi	139.21 (9)	Dy2^vii—O14—Dy3	114.6 (2)
Dy5ⁱⁱ—Dy5—Dy8^vi	90.0	Dy2^viii—O14—Dy3	114.6 (2)
Dy5ⁱⁱⁱ—Dy5—Dy8^vi	90.0	Dy2^vii—O14—Dy8^vii	114.9 (2)
Dy1—Dy5—Dy8^vi	176.23 (4)	Dy2^viii—O14—Dy8^vii	114.9 (2)
S11^vii—Dy6—S11^viii	85.99 (12)	Dy3—O14—Dy8^vii	94.3 (2)

Symmetry codes: (i) −x+1/2, −y+3/2, z−1/2; (ii) x−1, y, z; (iii) x+1, y, z; (iv) −x, −y+1, z−1/2; (v) x+1/2, y+1/2, z; (vi) x−1/2, y+1/2, z; (vii) x−1/2, y−1/2, z; (viii) x+1/2, y−1/2, z; (ix) −x+1/2, −y+1/2, z+1/2; (x) −x−1/2, −y+3/2, z−1/2; (xi) −x+1, −y+1, z+1/2; (xii) −x, −y+1, z+1/2; (xiii) −x+1, −y+1, z−1/2; (xiv) −x+1/2, −y+3/2, z+1/2; (xv) −x−1/2, −y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula	Dy₈SnS_13.61O_0.39
M_r	1861.27
Crystal system, space group	Orthorhombic, Cmc2₁
Temperature (K)	293
a, b, c (Å)	3.7822 (8), 23.620 (5), 21.271 (4)
V (Å³)	1900.3 (7)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	33.80
Crystal size (mm)	0.14 × 0.01 × 0.01

Data collection
Diffractometer	KUMA KM-4 with CCD area-detector
Absorption correction	Numerical (CrysAlis; Oxford Diffraction, 2007)
T_min, T_max	0.104, 0.716
No. of measured, independent and observed [I > 2σ(I)] reflections	11655, 2287, 1910
R_int	0.049
(sin θ/λ)_max (Å⁻¹)	0.633

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.038, 0.89
No. of reflections	2287
No. of parameters	141
No. of restraints	1
Δρ_max, Δρ_min (e Å⁻³)	3.05, −1.56
Absolute structure	Flack (1983), 1089 Friedel pairs
Absolute structure parameter	0.0 (2)

Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2005), publCIF (Westrip, 2007) and PLATON (Spek, 2003).

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