K₄Nb_0.96Ta_1.04S₁₁

The reaction of K₂S₃, Nb, Ta and S yields single crystals of non-stoichiometric tetra­potassium niobium tantalum undeca­sulfide, K₄Nb_0.96Ta_1.04S₁₁. The compound is isotypic with K₄Nb₂S₁₁ and the ortho­rhom­bic modification of K₄Ta₂S₁₁. The structure consists of discrete K⁺ cations and complex [M₂S₁₁]^4- (M = Nb and Ta) anions, in which the Nb and Ta atoms occupy the same Wyckoff positions statistically. Both M atoms are sevenfold coordinated by S₂^2- and S^2- anions. The coordination polyhedra can be described as distorted penta­gonal bipyramids. Two such bipyramids share a common face, thus forming the [M₂S₁₁]^4- anion.

Key indicators

• Single-crystal X-ray study
• T = 180 K
• Mean [sigma](S-S) = 0.002 Å
• Disorder in main residue
• R factor = 0.021
• wR factor = 0.056
• Data-to-parameter ratio = 25.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
PLAT301_ALERT_3_C Main Residue  Disorder .........................      11.00 Perc.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          3
              K

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           27.97
           From the CIF: _reflns_number_total               4000
           Count of symmetry unique reflns         2184
           Completeness (_total/calc)            183.15%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1816
           Fraction of Friedel pairs measured     0.832
           Are heavy atom types Z>Si present        yes

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   3 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.

tetrapotassium niobium tantalum undecasulfide

Crystal data

K4Nb1.04Ta0.96S11	F(000) = 1458.6
Mr = 779.33	Dx = 2.941 Mg m^−3
Orthorhombic, Pca21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2ac	Cell parameters from 8000 reflections
a = 13.1554 (10) Å	θ = 10–24°
b = 7.4520 (4) Å	µ = 8.85 mm^−1
c = 17.9508 (10) Å	T = 180 K
V = 1759.79 (19) Å^3	Polyhedron, dark red
Z = 4	0.12 × 0.08 × 0.05 mm

Data collection

Stoe IPDS diffractometer	4000 independent reflections
Radiation source: fine-focus sealed tube	3956 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
φ scans	θmax = 28.0°, θmin = 2.7°
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998)	h = −17→17
Tmin = 0.429, Tmax = 0.638	k = −8→9
14338 measured reflections	l = −22→22

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0443P)^2 + 1.0044P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.021	(Δ/σ)max = 0.002
wR(F^2) = 0.057	Δρmax = 0.73 e Å^−3
S = 1.05	Δρmin = −0.96 e Å^−3
4000 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
157 parameters	Extinction coefficient: 0.0042 (3)
1 restraint	Absolute structure: Flack (1983), 1966 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.006 (6)

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.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ta1	0.618887 (15)	0.29320 (3)	0.439728 (15)	0.00814 (9)	0.473 (3)
Nb1	0.618887 (15)	0.29320 (3)	0.439728 (15)	0.00814 (9)	0.527 (3)
Ta2	0.562809 (16)	0.24148 (3)	0.626899 (15)	0.00852 (10)	0.485 (3)
Nb2	0.562809 (16)	0.24148 (3)	0.626899 (15)	0.00852 (10)	0.515 (3)
K1	0.28523 (8)	0.30213 (13)	0.53294 (6)	0.0185 (2)
K2	0.72790 (7)	−0.15317 (14)	0.78114 (6)	0.0221 (2)
K3	0.54168 (9)	0.29060 (15)	0.88320 (7)	0.0252 (2)
K4	0.58491 (8)	0.31479 (17)	0.18179 (7)	0.0269 (2)
S1	0.68813 (7)	0.51970 (15)	0.37557 (7)	0.0162 (2)
S2	0.45111 (9)	0.25853 (16)	0.38323 (8)	0.0201 (3)
S3	0.56151 (9)	0.09532 (17)	0.33486 (7)	0.0225 (3)
S4	0.76224 (7)	0.08562 (15)	0.45638 (6)	0.0159 (2)
S5	0.74454 (8)	0.26616 (13)	0.54352 (6)	0.0117 (2)
S6	0.52118 (8)	0.47513 (13)	0.53207 (6)	0.0124 (2)
S7	0.51827 (8)	0.02818 (13)	0.52524 (6)	0.0129 (2)
S8	0.60123 (8)	−0.07989 (14)	0.61311 (6)	0.0164 (2)
S9	0.66097 (8)	0.48899 (14)	0.68300 (6)	0.0159 (2)
S10	0.68236 (9)	0.24200 (15)	0.73471 (7)	0.0162 (2)
S11	0.41708 (9)	0.24434 (17)	0.69033 (8)	0.0205 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ta1	0.00861 (11)	0.00723 (12)	0.00857 (13)	0.00008 (7)	0.00061 (7)	0.00088 (8)
Nb1	0.00861 (11)	0.00723 (12)	0.00857 (13)	0.00008 (7)	0.00061 (7)	0.00088 (8)
Ta2	0.00810 (13)	0.00875 (13)	0.00870 (14)	0.00008 (7)	0.00042 (8)	0.00099 (8)
Nb2	0.00810 (13)	0.00875 (13)	0.00870 (14)	0.00008 (7)	0.00042 (8)	0.00099 (8)
K1	0.0216 (5)	0.0138 (4)	0.0201 (5)	−0.0031 (3)	−0.0007 (4)	−0.0009 (3)
K2	0.0216 (4)	0.0177 (5)	0.0268 (5)	0.0041 (4)	0.0088 (4)	0.0058 (4)
K3	0.0261 (5)	0.0194 (5)	0.0299 (6)	0.0076 (4)	0.0027 (5)	−0.0056 (4)
K4	0.0164 (4)	0.0314 (6)	0.0330 (6)	0.0023 (4)	0.0007 (4)	0.0143 (5)
S1	0.0186 (4)	0.0133 (5)	0.0168 (5)	−0.0043 (4)	0.0042 (4)	0.0060 (4)
S2	0.0140 (5)	0.0244 (6)	0.0218 (7)	−0.0039 (4)	−0.0067 (5)	0.0021 (4)
S3	0.0372 (6)	0.0173 (6)	0.0131 (6)	−0.0042 (5)	0.0023 (4)	−0.0043 (4)
S4	0.0154 (4)	0.0145 (5)	0.0177 (6)	0.0067 (4)	0.0045 (3)	0.0014 (3)
S5	0.0079 (4)	0.0134 (5)	0.0139 (5)	−0.0009 (3)	−0.0004 (3)	0.0029 (3)
S6	0.0157 (5)	0.0108 (4)	0.0106 (5)	0.0063 (3)	0.0013 (3)	0.0011 (3)
S7	0.0145 (5)	0.0117 (4)	0.0124 (5)	−0.0051 (3)	−0.0011 (3)	−0.0004 (3)
S8	0.0233 (5)	0.0081 (4)	0.0179 (6)	0.0013 (4)	−0.0012 (4)	0.0027 (4)
S9	0.0203 (5)	0.0119 (5)	0.0154 (5)	−0.0031 (4)	−0.0023 (4)	−0.0008 (4)
S10	0.0173 (5)	0.0188 (5)	0.0125 (6)	0.0007 (4)	−0.0050 (4)	0.0032 (4)
S11	0.0114 (5)	0.0311 (7)	0.0190 (7)	0.0023 (4)	0.0078 (5)	0.0057 (4)

Geometric parameters (Å, º)

Ta1—S1	2.2372 (10)	K3—S7^vii	3.5730 (17)
Ta1—S2	2.4427 (12)	K3—Nb1^iii	3.8873 (11)
Ta1—S4	2.4573 (10)	K3—Ta1^iii	3.8873 (11)
Ta1—S6	2.4975 (10)	K3—K2^iv	4.6308 (16)
Ta1—S5	2.4989 (11)	K3—K1^iii	4.6499 (16)
Ta1—S3	2.5075 (12)	K4—S3	3.2124 (17)
Ta1—S7	2.8299 (10)	K4—S10^xi	3.2511 (16)
Ta1—K3^i	3.8873 (11)	K4—S8^xii	3.2528 (16)
Ta1—K1^ii	4.0844 (10)	K4—S11^i	3.2890 (18)
Ta2—S11	2.2299 (12)	K4—S5^xi	3.3654 (16)
Ta2—S8	2.4601 (11)	K4—S6^i	3.4092 (15)
Ta2—S9	2.4666 (11)	K4—S9^i	3.5499 (16)
Ta2—S7	2.4900 (10)	K4—S9^xi	3.5863 (16)
Ta2—S10	2.4938 (12)	K4—Ta2^i	3.9600 (11)
Ta2—S6	2.4959 (10)	K4—Nb2^i	3.9600 (11)
Ta2—S5	2.8265 (11)	K4—K1^i	4.2671 (15)
Ta2—K4^iii	3.9600 (11)	K4—K2^xi	4.6266 (15)
Ta2—K1	4.0477 (11)	S1—K2^xiii	3.1681 (15)
K1—S4^iv	3.2139 (14)	S1—K3^i	3.3402 (15)
K1—S5^v	3.2669 (14)	S1—K1^ii	3.3726 (16)
K1—S8^iv	3.2669 (15)	S2—S3	2.0838 (18)
K1—S11	3.3432 (18)	S2—K2^xii	3.0855 (16)
K1—S6	3.3612 (15)	S2—K3^i	3.3613 (16)
K1—S1^v	3.3726 (16)	S3—K3^xii	3.2963 (18)
K1—S2	3.4770 (18)	S3—K2^xi	3.4691 (17)
K1—S9^v	3.5145 (15)	S4—S5	2.0764 (15)
K1—S7	3.6858 (15)	S4—K1^vi	3.2139 (14)
K1—Nb1^v	4.0844 (10)	S4—K3^xi	3.2731 (16)
K2—S11^vi	3.0516 (16)	S4—K2^xi	3.6164 (16)
K2—S2^vii	3.0855 (16)	S5—K1^ii	3.2669 (14)
K2—S10	3.1186 (15)	S5—K4^x	3.3654 (16)
K2—S1^viii	3.1681 (15)	S6—K3^i	3.2974 (15)
K2—S9^ix	3.3150 (16)	S6—K4^iii	3.4092 (15)
K2—S3^x	3.4691 (17)	S7—S8	2.0803 (15)
K2—S8	3.4890 (16)	S7—K3^xii	3.5730 (17)
K2—S4^x	3.6164 (16)	S8—K4^vii	3.2528 (16)
K2—K3	4.5048 (15)	S8—K1^vi	3.2669 (15)
K2—K4^x	4.6266 (15)	S9—S10	2.0805 (15)
K2—K3^vi	4.6308 (16)	S9—K2^xiv	3.3150 (16)
K2—K4^vii	4.6438 (16)	S9—K1^ii	3.5145 (15)
K3—S10	3.2651 (18)	S9—K4^iii	3.5499 (16)
K3—S4^x	3.2731 (16)	S9—K4^x	3.5863 (16)
K3—S3^vii	3.2963 (18)	S10—K4^x	3.2511 (16)
K3—S6^iii	3.2974 (15)	S11—K2^iv	3.0516 (16)
K3—S1^iii	3.3402 (15)	S11—K4^iii	3.2890 (18)
K3—S2^iii	3.3613 (16)
S1—Ta1—S2	103.53 (4)	S3—K4—S5^xi	129.78 (4)
S1—Ta1—S4	103.01 (4)	S10^xi—K4—S5^xi	64.51 (3)
S2—Ta1—S4	132.64 (4)	S8^xii—K4—S5^xi	99.46 (4)
S1—Ta1—S6	98.14 (4)	S11^i—K4—S5^xi	98.47 (4)
S2—Ta1—S6	82.41 (4)	S3—K4—S6^i	150.33 (4)
S4—Ta1—S6	130.99 (4)	S10^xi—K4—S6^i	133.83 (4)
S1—Ta1—S5	100.10 (4)	S8^xii—K4—S6^i	68.91 (3)
S2—Ta1—S5	153.99 (4)	S11^i—K4—S6^i	64.84 (4)
S4—Ta1—S5	49.53 (4)	S5^xi—K4—S6^i	74.99 (3)
S6—Ta1—S5	83.65 (4)	S3—K4—S9^i	96.73 (4)
S1—Ta1—S3	100.36 (4)	S10^xi—K4—S9^i	157.67 (5)
S2—Ta1—S3	49.77 (4)	S8^xii—K4—S9^i	62.48 (3)
S4—Ta1—S3	87.26 (4)	S11^i—K4—S9^i	65.23 (3)
S6—Ta1—S3	131.49 (4)	S5^xi—K4—S9^i	131.02 (4)
S5—Ta1—S3	135.35 (4)	S6^i—K4—S9^i	56.13 (3)
S1—Ta1—S7	174.99 (4)	S3—K4—S9^xi	105.57 (4)
S2—Ta1—S7	74.26 (4)	S10^xi—K4—S9^xi	35.00 (3)
S4—Ta1—S7	81.59 (3)	S8^xii—K4—S9^xi	154.01 (5)
S6—Ta1—S7	77.18 (3)	S11^i—K4—S9^xi	69.24 (4)
S5—Ta1—S7	81.30 (3)	S5^xi—K4—S9^xi	54.69 (3)
S3—Ta1—S7	81.72 (4)	S6^i—K4—S9^xi	102.72 (4)
S11—Ta2—S8	103.73 (4)	S9^i—K4—S9^xi	134.45 (4)
S11—Ta2—S9	103.56 (5)	Ta1—S1—K2^xiii	176.35 (5)
S8—Ta2—S9	131.41 (4)	Ta1—S1—K3^i	85.97 (4)
S11—Ta2—S7	100.25 (4)	K2^xiii—S1—K3^i	90.68 (4)
S8—Ta2—S7	49.70 (4)	Ta1—S1—K1^ii	91.15 (4)
S9—Ta2—S7	154.13 (4)	K2^xiii—S1—K1^ii	90.75 (4)
S11—Ta2—S10	98.39 (5)	K3^i—S1—K1^ii	98.16 (4)
S8—Ta2—S10	87.13 (4)	S3—S2—Ta1	66.73 (5)
S9—Ta2—S10	49.59 (4)	S3—S2—K2^xii	97.81 (6)
S7—Ta2—S10	135.90 (4)	Ta1—S2—K2^xii	164.39 (6)
S11—Ta2—S6	98.80 (4)	S3—S2—K3^i	124.31 (6)
S8—Ta2—S6	130.96 (4)	Ta1—S2—K3^i	82.46 (4)
S9—Ta2—S6	82.63 (4)	K2^xii—S2—K3^i	106.01 (4)
S7—Ta2—S6	83.90 (4)	S3—S2—K1	144.49 (7)
S10—Ta2—S6	131.81 (4)	Ta1—S2—K1	103.67 (5)
S11—Ta2—S5	175.52 (4)	K2^xii—S2—K1	90.22 (4)
S8—Ta2—S5	80.58 (3)	K3^i—S2—K1	85.67 (4)
S9—Ta2—S5	74.02 (3)	S2—S3—Ta1	63.50 (5)
S7—Ta2—S5	81.52 (3)	S2—S3—K4	97.24 (6)
S10—Ta2—S5	82.96 (4)	Ta1—S3—K4	108.29 (5)
S6—Ta2—S5	77.24 (3)	S2—S3—K3^xii	96.46 (6)
S4^iv—K1—S5^v	153.48 (5)	Ta1—S3—K3^xii	116.07 (5)
S4^iv—K1—S8^iv	70.30 (3)	K4—S3—K3^xii	135.13 (5)
S5^v—K1—S8^iv	110.62 (4)	S2—S3—K2^xi	169.73 (7)
S4^iv—K1—S11	107.12 (4)	Ta1—S3—K2^xi	106.39 (4)
S5^v—K1—S11	99.36 (4)	K4—S3—K2^xi	87.56 (4)
S8^iv—K1—S11	86.95 (4)	K3^xii—S3—K2^xi	86.35 (4)
S4^iv—K1—S6	115.45 (4)	S5—S4—Ta1	66.28 (4)
S5^v—K1—S6	76.93 (3)	S5—S4—K1^vi	105.72 (5)
S8^iv—K1—S6	151.73 (4)	Ta1—S4—K1^vi	133.64 (4)
S11—K1—S6	64.80 (3)	S5—S4—K3^xi	95.07 (5)
S4^iv—K1—S1^v	87.72 (4)	Ta1—S4—K3^xi	105.20 (4)
S5^v—K1—S1^v	66.36 (3)	K1^vi—S4—K3^xi	121.13 (4)
S8^iv—K1—S1^v	106.73 (4)	S5—S4—K2^xi	168.01 (6)
S11—K1—S1^v	162.76 (4)	Ta1—S4—K2^xi	103.39 (4)
S6—K1—S1^v	101.24 (4)	K1^vi—S4—K2^xi	85.77 (4)
S4^iv—K1—S2	69.18 (3)	K3^xi—S4—K2^xi	81.50 (3)
S5^v—K1—S2	103.88 (4)	S4—S5—Ta1	64.19 (4)
S8^iv—K1—S2	139.30 (4)	S4—S5—Ta2	116.85 (5)
S11—K1—S2	108.39 (4)	Ta1—S5—Ta2	80.83 (3)
S6—K1—S2	56.81 (3)	S4—S5—K1^ii	125.16 (6)
S1^v—K1—S2	68.11 (3)	Ta1—S5—K1^ii	89.18 (4)
S4^iv—K1—S9^v	133.01 (4)	Ta2—S5—K1^ii	103.50 (4)
S5^v—K1—S9^v	56.15 (3)	S4—S5—K4^x	123.41 (6)
S8^iv—K1—S9^v	62.76 (3)	Ta1—S5—K4^x	169.18 (4)
S11—K1—S9^v	69.55 (3)	Ta2—S5—K4^x	100.39 (4)
S6—K1—S9^v	105.26 (4)	K1^ii—S5—K4^x	80.07 (4)
S1^v—K1—S9^v	106.95 (4)	Ta2—S6—Ta1	87.77 (3)
S2—K1—S9^v	157.78 (4)	Ta2—S6—K3^i	167.72 (5)
S4^iv—K1—S7	64.17 (3)	Ta1—S6—K3^i	83.03 (4)
S5^v—K1—S7	133.15 (4)	Ta2—S6—K1	86.09 (3)
S8^iv—K1—S7	110.61 (4)	Ta1—S6—K1	105.68 (4)
S11—K1—S7	61.89 (3)	K3^i—S6—K1	88.58 (4)
S6—K1—S7	56.23 (3)	Ta2—S6—K4^iii	82.67 (3)
S1^v—K1—S7	120.11 (4)	Ta1—S6—K4^iii	169.48 (4)
S2—K1—S7	52.93 (3)	K3^i—S6—K4^iii	107.05 (4)
S9^v—K1—S7	131.37 (4)	K1—S6—K4^iii	78.13 (3)
S11^vi—K2—S2^vii	152.01 (5)	S8—S7—Ta2	64.41 (4)
S11^vi—K2—S10	102.95 (4)	S8—S7—Ta1	115.85 (5)
S2^vii—K2—S10	104.62 (4)	Ta2—S7—Ta1	80.91 (3)
S11^vi—K2—S1^viii	80.22 (4)	S8—S7—K3^xii	113.54 (5)
S2^vii—K2—S1^viii	75.67 (4)	Ta2—S7—K3^xii	177.94 (4)
S10—K2—S1^viii	159.49 (5)	Ta1—S7—K3^xii	100.38 (4)
S11^vi—K2—S9^ix	75.74 (4)	S8—S7—K1	128.49 (6)
S2^vii—K2—S9^ix	84.74 (4)	Ta2—S7—K1	79.32 (3)
S10—K2—S9^ix	124.51 (5)	Ta1—S7—K1	91.31 (3)
S1^viii—K2—S9^ix	75.99 (4)	K3^xii—S7—K1	102.21 (3)
S11^vi—K2—S3^x	67.42 (4)	S7—S8—Ta2	65.90 (4)
S2^vii—K2—S3^x	125.47 (5)	S7—S8—K4^vii	95.78 (5)
S10—K2—S3^x	73.96 (4)	Ta2—S8—K4^vii	109.33 (4)
S1^viii—K2—S3^x	89.06 (4)	S7—S8—K1^vi	104.54 (6)
S9^ix—K2—S3^x	142.11 (4)	Ta2—S8—K1^vi	133.63 (4)
S11^vi—K2—S8	87.85 (4)	K4^vii—S8—K1^vi	116.87 (4)
S2^vii—K2—S8	100.88 (4)	S7—S8—K2	165.16 (6)
S10—K2—S8	61.93 (3)	Ta2—S8—K2	99.41 (4)
S1^viii—K2—S8	138.55 (5)	K4^vii—S8—K2	87.00 (4)
S9^ix—K2—S8	62.59 (3)	K1^vi—S8—K2	87.00 (4)
S3^x—K2—S8	122.56 (4)	S10—S9—Ta2	65.88 (4)
S11^vi—K2—S4^x	123.02 (5)	S10—S9—K2^xiv	116.02 (6)
S2^vii—K2—S4^x	68.65 (4)	Ta2—S9—K2^xiv	163.25 (5)
S10—K2—S4^x	76.98 (4)	S10—S9—K1^ii	132.13 (6)
S1^viii—K2—S4^x	84.30 (4)	Ta2—S9—K1^ii	105.17 (4)
S9^ix—K2—S4^x	150.18 (4)	K2^xiv—S9—K1^ii	85.84 (4)
S3^x—K2—S4^x	57.78 (3)	S10—S9—K4^iii	119.37 (6)
S8—K2—S4^x	133.80 (4)	Ta2—S9—K4^iii	80.12 (3)
S10—K3—S6^iii	149.59 (5)	K2^xiv—S9—K4^iii	85.06 (4)
S4^x—K3—S6^iii	96.86 (4)	K1^ii—S9—K4^iii	103.69 (4)
S3^vii—K3—S6^iii	124.89 (5)	S10—S9—K4^x	63.66 (5)
S10—K3—S1^iii	121.77 (5)	Ta2—S9—K4^x	102.41 (4)
S4^x—K3—S1^iii	158.01 (5)	K2^xiv—S9—K4^x	92.68 (4)
S3^vii—K3—S1^iii	89.18 (4)	K1^ii—S9—K4^x	73.87 (3)
S6^iii—K3—S1^iii	65.30 (3)	K4^iii—S9—K4^x	176.82 (4)
S10—K3—S2^iii	95.45 (4)	S9—S10—Ta2	64.52 (4)
S4^x—K3—S2^iii	116.37 (5)	S9—S10—K2	168.70 (7)
S3^vii—K3—S2^iii	152.10 (5)	Ta2—S10—K2	109.09 (4)
S6^iii—K3—S2^iii	58.51 (4)	S9—S10—K4^x	81.34 (5)
S1^iii—K3—S2^iii	66.58 (3)	Ta2—S10—K4^x	111.56 (5)
S10—K3—S7^vii	129.34 (4)	K2—S10—K4^x	93.14 (4)
S4^x—K3—S7^vii	64.99 (3)	S9—S10—K3	100.92 (6)
S3^vii—K3—S7^vii	61.11 (3)	Ta2—S10—K3	106.03 (4)
S6^iii—K3—S7^vii	73.64 (4)	K2—S10—K3	89.74 (4)
S1^iii—K3—S7^vii	96.37 (4)	K4^x—S10—K3	138.92 (5)
S2^iii—K3—S7^vii	132.12 (5)	Ta2—S11—K2^iv	166.36 (6)
S3—K4—S10^xi	75.84 (4)	Ta2—S11—K4^iii	89.58 (4)
S3—K4—S8^xii	88.74 (4)	K2^iv—S11—K4^iii	103.93 (4)
S10^xi—K4—S8^xii	136.88 (5)	Ta2—S11—K1	90.90 (5)
S3—K4—S11^i	117.90 (5)	K2^iv—S11—K1	93.27 (4)
S10^xi—K4—S11^i	99.24 (4)	K4^iii—S11—K1	80.08 (4)
S8^xii—K4—S11^i	123.31 (4)

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