Hexapotassium di-μ-dioxosulfato-bis­[tetra­cyano­osmate(III)](Os—Os) dihydrate

The title compound, K₆[Os₂(CN)₈(SO₂)₂]·2H₂O, was prepared from the reaction of OsO₄ with elemental Se and S₂Cl₂ at 473 K and further reaction with aqueous KCN solution. It contains a centrosymmetric binuclear [Os₂S₂O₄(CN)₈]⁶⁻ cluster anion.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](N-C) = 0.009 Å
• R factor = 0.021
• wR factor = 0.054
• Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............      24.97 Deg.
PLAT220_ALERT_2_B Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.55 Ratio
PLAT420_ALERT_2_B D-H Without Acceptor       O1W    -   H1W1   ...          ?

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 ............       2.00 Ratio
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT320_ALERT_2_C Check Hybridisation of  C4     in Main Residue .          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.71 Ratio

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

   5 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
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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S1. Comment

The chemistry of cyanide and chalcocyanide compounds of transition metals has been developed extensively in recent years (Gabriel et al., 2001; Mironov & Fedorov, 2002; Naumov et al. 2000; Kalinina & Fedin, 2003). It is well known that osmium complexes can react with alkali metal cyanides, with the cyanide ligands entering the Os coordination sphere and concomitant reduction of the osmium. For example, K₂[Os⁺⁴Cl₆] or K₂[Os⁺⁶I₄] complexes react with aqueous or molten cyanides with the formation of K₄[Os⁺²(CN)₆] (Livingston, 1978). Here, we report the synthesis and structure of the title compound, (I), which is the first cluster chalcocyanide of Os. It is isostructural with K₆Re₂S₂O₄(CN)₈·2H₂O, which contains the [Re₂S₂O₄(CN)₈]⁶⁻ cluster anion (Muller et al. 1991).

Compound (I) (Fig. 1) contains the binuclear-cluster anionic unit [Os₂S₂O₄(CN)₈]⁶⁻. The major difference between the Os and Re compounds is the length of the metal–metal bond, with the Os—Os distance in (I) of 2.8546 (6) Å being longer than the corresponding Re—Re distance of 2.653 (1) Å in [Re₂S₂O₄(CN)₈]⁶⁻.

The complete cluster in (I) is generated by inversion symmetry and each Os atom is coordinated by two SO₂ ligands, with Os—µ₂-S distances of 2.319 (2) and 2.321 (1) Å (Table 1). The Os atom is further coordinatd by four terminal cyano ligands, with Os—C distances in the range 2.044 (7)–2.057 (6) Å. K⁺ cations and water molecules complete the structure of (I).

S2. Experimental

OsO₄ and a 22% solution of elemental Se in S₂Cl₂ (ratio solid:liquid = 1:10) were loaded into a reactor under argon. The reaction mixture was heated at 313–323 K with full dissolution of OsO₄ and isolation of SO₂. The temperature was then raised to 343–363 K and SO₂ was removed completely. The reactor was then sealed and placed in an oven at 473 K for 40 h. After reaction, the product was washed with S₂Cl₂, CS₂ and CCl₄, and dried in vacuo. Finally, the recovered black powder (0.05 g) and KCN (0.07 g) were boiled in water (10 ml) for 10 min and filtered. The filtrate was evaporated to a volume of 5 ml. After a few days, brown crystals of (I) were filtered and dried on filter paper. An electron-microprobe analysis indicated an Os:S ratio of 1:1.

S3. Refinement

Water H atoms were positioned geometrically, with O—H = 0.82 Å, and refined as riding, with U_iso(H) = 1.2U_eq(O).

Computing details

Data collection: CD4CA0 (Enraf–Nonius, 1989); cell refinement: CD4CA0; data reduction: CADDAT (Enraf–Nonius, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: BS (Kang & Ozawa, 2002); software used to prepare material for publication: SHELXL97.

Figures

Fig. 1. The structure of the [Os2S2O4(CN)8]^6− cluster anion in (I). Displacement ellipsoids are drawn at the 50% probability level and unlabelled atoms are generated by the symmetry operation (1 − x, −y, 1 − z).

Hexapotassium di-µ-dioxosulfato-bis[tetracyanoosmate(III)](Os—Os) dihydrate

Crystal data

K6[Os2(CN)8(SO2)2]·2H2O	Z = 1
Mr = 987.31	F(000) = 454
Triclinic, P1	Dx = 2.898 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.9496 (10) Å	Cell parameters from 24 reflections
b = 8.9222 (11) Å	θ = 11.5–14.9°
c = 8.9747 (15) Å	µ = 12.55 mm^−1
α = 84.202 (15)°	T = 293 K
β = 64.013 (12)°	Plate, brown
γ = 81.677 (12)°	0.19 × 0.16 × 0.04 mm
V = 565.66 (14) Å^3

Data collection

Enraf–Nonius CAD-4 diffractometer	1817 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.020
Graphite monochromator	θmax = 25.0°, θmin = 2.3°
2θ/θ scans	h = 0→9
Absorption correction: integration (CADDAT; Enraf–Nonius, 1989)	k = −10→10
Tmin = 0.157, Tmax = 0.591	l = −9→10
2150 measured reflections	3 standard reflections every 60 min
1991 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.021	H-atom parameters constrained
wR(F^2) = 0.054	w = 1/[σ^2(Fo^2) + (0.0288P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
1991 reflections	Δρmax = 1.39 e Å^−3
146 parameters	Δρmin = −1.62 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0010 (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.

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

	x	y	z	Uiso*/Ueq
Os1	0.50423 (3)	0.15519 (3)	0.44271 (3)	0.01385 (11)
C1	0.3167 (9)	0.3473 (7)	0.5023 (8)	0.0208 (13)
N1	0.1999 (8)	0.4450 (7)	0.5394 (8)	0.0360 (15)
C2	0.7065 (9)	0.2772 (7)	0.2658 (8)	0.0212 (14)
N2	0.8324 (8)	0.3332 (7)	0.1642 (7)	0.0306 (13)
C3	0.4138 (8)	0.1294 (7)	0.2650 (8)	0.0200 (13)
N3	0.3594 (7)	0.1348 (7)	0.1636 (7)	0.0274 (13)
C4	0.5837 (8)	0.2101 (7)	0.6172 (7)	0.0184 (13)
N4	0.6234 (8)	0.2525 (7)	0.7126 (7)	0.0283 (13)
S1	0.25549 (19)	0.04233 (17)	0.65172 (17)	0.0153 (3)
O1	0.1910 (6)	0.0887 (5)	0.8251 (5)	0.0218 (9)
O2	0.0878 (5)	0.0346 (5)	0.6220 (5)	0.0223 (10)
K1	0.2354 (2)	0.35137 (19)	0.9328 (2)	0.0359 (4)
K2	0.78033 (19)	0.11126 (19)	0.92833 (17)	0.0284 (3)
K3	0.99342 (19)	0.24828 (17)	0.42294 (18)	0.0268 (3)
O1W	0.1761 (10)	0.5399 (9)	1.1831 (8)	0.077 (2)
H1W1	0.2508	0.5087	1.2226	0.093*
H1W2	0.0697	0.5336	1.2568	0.093*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os1	0.01318 (14)	0.01358 (14)	0.01335 (14)	−0.00233 (9)	−0.00418 (9)	−0.00033 (9)
C1	0.023 (3)	0.016 (3)	0.025 (3)	0.000 (3)	−0.012 (3)	−0.006 (3)
N1	0.033 (3)	0.026 (3)	0.046 (4)	0.004 (3)	−0.015 (3)	−0.013 (3)
C2	0.026 (3)	0.019 (3)	0.022 (3)	−0.001 (3)	−0.014 (3)	−0.003 (3)
N2	0.030 (3)	0.032 (3)	0.025 (3)	−0.014 (3)	−0.006 (3)	0.006 (3)
C3	0.017 (3)	0.021 (3)	0.019 (3)	−0.006 (3)	−0.004 (3)	0.000 (3)
N3	0.028 (3)	0.033 (4)	0.022 (3)	−0.006 (3)	−0.011 (2)	0.000 (3)
C4	0.015 (3)	0.020 (3)	0.016 (3)	−0.003 (3)	−0.003 (2)	0.002 (3)
N4	0.029 (3)	0.033 (4)	0.026 (3)	−0.008 (3)	−0.013 (3)	−0.001 (3)
S1	0.0135 (6)	0.0157 (8)	0.0143 (7)	−0.0020 (6)	−0.0038 (6)	0.0000 (6)
O1	0.024 (2)	0.024 (2)	0.014 (2)	−0.0030 (19)	−0.0041 (18)	−0.0030 (19)
O2	0.017 (2)	0.027 (3)	0.024 (2)	−0.0066 (18)	−0.0087 (18)	0.003 (2)
K1	0.0345 (8)	0.0290 (9)	0.0361 (9)	−0.0037 (7)	−0.0063 (7)	−0.0077 (7)
K2	0.0232 (7)	0.0398 (9)	0.0194 (7)	−0.0026 (6)	−0.0070 (6)	−0.0007 (7)
K3	0.0229 (7)	0.0273 (8)	0.0299 (8)	−0.0020 (6)	−0.0114 (6)	−0.0011 (7)
O1W	0.088 (5)	0.097 (6)	0.058 (4)	−0.025 (5)	−0.036 (4)	−0.007 (4)

Geometric parameters (Å, º)

Os1—C1	2.048 (6)	N4—K3	2.949 (6)
Os1—C4	2.050 (6)	S1—O2	1.482 (4)
Os1—C2	2.052 (7)	S1—O1	1.491 (4)
Os1—C3	2.059 (6)	S1—Os1^i	2.3198 (15)
Os1—S1^i	2.3198 (15)	O1—K1	2.747 (5)
Os1—S1	2.3210 (15)	O1—K2^vi	2.768 (5)
Os1—Os1^i	2.8546 (6)	O1—K2^ii	2.958 (4)
C1—N1	1.134 (9)	O2—K3^ii	2.731 (5)
C1—K3^ii	3.206 (6)	O2—K3^i	2.803 (5)
N1—K3^iii	2.912 (6)	O2—K2^ii	2.830 (4)
N1—K3^ii	3.095 (6)	K1—O1W	2.775 (7)
C2—N2	1.156 (8)	K1—N2^iii	2.906 (6)
C2—K3	3.136 (6)	K1—N2^vii	2.976 (6)
C2—K2^iv	3.287 (6)	K1—N3^viii	3.069 (6)
N2—K1^iii	2.906 (6)	K2—O1^vi	2.768 (5)
N2—K1^v	2.976 (6)	K2—O2^ix	2.830 (4)
N2—K3	3.094 (6)	K2—N3^i	2.934 (6)
N2—K2^iv	3.229 (6)	K2—O1^ix	2.958 (4)
C3—N3	1.162 (8)	K2—N3^viii	3.065 (6)
C3—K3^ii	3.071 (6)	K2—O1W^x	3.191 (8)
C3—K2^iv	3.145 (6)	K2—N2^viii	3.229 (6)
N3—K3^ii	2.932 (6)	K3—O2^ix	2.731 (5)
N3—K2^i	2.934 (6)	K3—O2^i	2.803 (5)
N3—K2^iv	3.065 (6)	K3—N1^iii	2.912 (6)
N3—K1^iv	3.069 (6)	K3—N3^ix	2.932 (6)
C4—N4	1.146 (8)	K3—N1^ix	3.095 (6)
C4—K3	2.998 (6)	K3—O1W^v	3.277 (8)
C4—K1	3.181 (6)	O1W—K2^x	3.191 (8)
N4—K2	2.839 (6)	O1W—H1W1	0.8200
N4—K1	2.901 (6)	O1W—H1W2	0.8200
C1—Os1—C4	87.1 (2)	N2^iii—K1—K2	126.66 (12)
C1—Os1—C2	90.3 (3)	N2^vii—K1—K2	132.88 (13)
C4—Os1—C2	89.5 (2)	N3^viii—K1—K2	42.34 (10)
C1—Os1—C3	86.2 (2)	C4—K1—K2	54.59 (11)
C4—Os1—C3	172.6 (2)	K3^vii—K1—K2	87.13 (4)
C2—Os1—C3	87.3 (2)	K1^xi—K1—K2	158.57 (7)
C1—Os1—S1^i	172.38 (18)	K2^vi—K1—K2	65.71 (4)
C4—Os1—S1^i	93.07 (17)	K2^ii—K1—K2	123.82 (5)
C2—Os1—S1^i	82.11 (18)	O1^vi—K2—O2^ix	108.79 (13)
C3—Os1—S1^i	93.12 (18)	O1^vi—K2—N4	156.88 (15)
C1—Os1—S1	83.54 (18)	O2^ix—K2—N4	81.45 (15)
C4—Os1—S1	89.29 (16)	O1^vi—K2—N3^i	86.10 (15)
C2—Os1—S1	173.75 (18)	O2^ix—K2—N3^i	79.53 (14)
C3—Os1—S1	93.10 (17)	N4—K2—N3^i	75.22 (16)
S1^i—Os1—S1	104.08 (4)	O1^vi—K2—O1^ix	80.17 (13)
C1—Os1—Os1^i	135.56 (18)	O2^ix—K2—O1^ix	49.25 (11)
C4—Os1—Os1^i	91.92 (18)	N4—K2—O1^ix	120.33 (15)
C2—Os1—Os1^i	134.16 (18)	N3^i—K2—O1^ix	116.93 (15)
C3—Os1—Os1^i	95.06 (18)	O1^vi—K2—N3^viii	82.98 (14)
S1^i—Os1—Os1^i	52.06 (4)	O2^ix—K2—N3^viii	151.66 (14)
S1—Os1—Os1^i	52.02 (4)	N4—K2—N3^viii	79.30 (16)
N1—C1—Os1	173.6 (6)	N3^i—K2—N3^viii	75.58 (18)
N1—C1—K3^ii	74.1 (4)	O1^ix—K2—N3^viii	158.04 (14)
Os1—C1—K3^ii	100.4 (2)	O1^vi—K2—C3^viii	66.58 (15)
C1—N1—K3^iii	161.1 (6)	O2^ix—K2—C3^viii	167.87 (16)
C1—N1—K3^ii	85.2 (5)	N4—K2—C3^viii	99.02 (16)
K3^iii—N1—K3^ii	107.98 (19)	N3^i—K2—C3^viii	88.84 (16)
N2—C2—Os1	173.4 (6)	O1^ix—K2—C3^viii	136.53 (14)
N2—C2—K3	77.3 (4)	N3^viii—K2—C3^viii	21.51 (14)
Os1—C2—K3	99.4 (2)	O1^vi—K2—O1W^x	137.97 (15)
N2—C2—K2^iv	77.0 (4)	O2^ix—K2—O1W^x	88.41 (16)
Os1—C2—K2^iv	100.7 (2)	N4—K2—O1W^x	60.63 (17)
K3—C2—K2^iv	124.6 (2)	N3^i—K2—O1W^x	135.51 (17)
C2—N2—K1^iii	117.7 (5)	O1^ix—K2—O1W^x	83.61 (16)
C2—N2—K1^v	155.3 (5)	N3^viii—K2—O1W^x	99.91 (18)
K1^iii—N2—K1^v	86.73 (16)	C3^viii—K2—O1W^x	102.44 (18)
C2—N2—K3	81.3 (4)	O1^vi—K2—N2^viii	77.87 (14)
K1^iii—N2—K3	120.6 (2)	O2^ix—K2—N2^viii	119.01 (14)
K1^v—N2—K3	82.96 (15)	N4—K2—N2^viii	116.05 (17)
C2—N2—K2^iv	82.6 (4)	N3^i—K2—N2^viii	158.54 (15)
K1^iii—N2—K2^iv	110.53 (18)	O1^ix—K2—N2^viii	74.54 (13)
K1^v—N2—K2^iv	92.35 (16)	N3^viii—K2—N2^viii	88.26 (15)
K3—N2—K2^iv	128.2 (2)	C3^viii—K2—N2^viii	71.81 (15)
N3—C3—Os1	171.3 (6)	O1W^x—K2—N2^viii	60.45 (16)
N3—C3—K3^ii	72.2 (4)	O1^vi—K2—C2^viii	66.37 (15)
Os1—C3—K3^ii	104.5 (2)	O2^ix—K2—C2^viii	137.53 (14)
N3—C3—K2^iv	75.4 (4)	N4—K2—C2^viii	120.25 (17)
Os1—C3—K2^iv	105.2 (2)	N3^i—K2—C2^viii	138.33 (16)
K3^ii—C3—K2^iv	143.6 (2)	O1^ix—K2—C2^viii	89.60 (14)
C3—N3—K3^ii	85.7 (4)	N3^viii—K2—C2^viii	70.70 (15)
C3—N3—K2^i	127.0 (5)	C3^viii—K2—C2^viii	52.31 (16)
K3^ii—N3—K2^i	95.55 (16)	O1W^x—K2—C2^viii	75.05 (17)
C3—N3—K2^iv	83.1 (4)	N2^viii—K2—C2^viii	20.41 (15)
K3^ii—N3—K2^iv	160.0 (2)	O1^vi—K2—S1^ix	94.77 (10)
K2^i—N3—K2^iv	104.42 (18)	O2^ix—K2—S1^ix	24.28 (8)
C3—N3—K1^iv	143.8 (5)	N4—K2—S1^ix	101.18 (12)
K3^ii—N3—K1^iv	84.12 (15)	N3^i—K2—S1^ix	98.15 (12)
K2^i—N3—K1^iv	88.57 (15)	O1^ix—K2—S1^ix	24.97 (8)
K2^iv—N3—K1^iv	95.24 (16)	N3^viii—K2—S1^ix	173.44 (13)
N4—C4—Os1	174.6 (6)	C3^viii—K2—S1^ix	159.71 (12)
N4—C4—K3	76.5 (4)	O1W^x—K2—S1^ix	85.91 (14)
Os1—C4—K3	103.9 (2)	N2^viii—K2—S1^ix	97.32 (11)
N4—C4—K1	65.6 (4)	C2^viii—K2—S1^ix	114.09 (12)
Os1—C4—K1	112.1 (2)	O1^vi—K2—S1^vi	19.49 (9)
K3—C4—K1	137.5 (2)	O2^ix—K2—S1^vi	124.62 (10)
C4—N4—K2	134.6 (5)	N4—K2—S1^vi	152.76 (12)
C4—N4—K1	93.3 (4)	N3^i—K2—S1^vi	99.99 (12)
K2—N4—K1	104.24 (18)	O1^ix—K2—S1^vi	86.04 (9)
C4—N4—K3	81.3 (4)	N3^viii—K2—S1^vi	73.58 (11)
K2—N4—K3	93.16 (16)	C3^viii—K2—S1^vi	53.80 (12)
K1—N4—K3	159.8 (2)	O1W^x—K2—S1^vi	121.52 (12)
O2—S1—O1	108.6 (2)	N2^viii—K2—S1^vi	61.30 (11)
O2—S1—Os1^i	116.86 (19)	C2^viii—K2—S1^vi	47.44 (12)
O1—S1—Os1^i	117.60 (18)	S1^ix—K2—S1^vi	106.05 (5)
O2—S1—Os1	117.13 (18)	O2^ix—K3—O2^i	70.97 (14)
O1—S1—Os1	117.96 (18)	O2^ix—K3—N1^iii	135.86 (17)
Os1^i—S1—Os1	75.92 (4)	O2^i—K3—N1^iii	134.96 (15)
S1—O1—K1	128.9 (2)	O2^ix—K3—N3^ix	84.13 (15)
S1—O1—K2^vi	122.3 (2)	O2^i—K3—N3^ix	80.01 (15)
K1—O1—K2^vi	98.97 (14)	N1^iii—K3—N3^ix	128.63 (18)
S1—O1—K2^ii	98.16 (19)	O2^ix—K3—N4	81.15 (15)
K1—O1—K2^ii	103.41 (14)	O2^i—K3—N4	83.43 (15)
K2^vi—O1—K2^ii	99.83 (13)	N1^iii—K3—N4	70.52 (18)
S1—O2—K3^ii	120.9 (2)	N3^ix—K3—N4	160.70 (17)
S1—O2—K3^i	119.1 (2)	O2^ix—K3—C4	91.34 (15)
K3^ii—O2—K3^i	109.03 (14)	O2^i—K3—C4	68.11 (15)
S1—O2—K2^ii	104.0 (2)	N1^iii—K3—C4	74.97 (18)
K3^ii—O2—K2^ii	98.24 (14)	N3^ix—K3—C4	147.45 (17)
K3^i—O2—K2^ii	100.92 (13)	N4—K3—C4	22.20 (15)
O1—K1—O1W	151.76 (19)	O2^ix—K3—C3^ix	67.63 (15)
O1—K1—N4	79.60 (15)	O2^i—K3—C3^ix	88.77 (15)
O1W—K1—N4	117.0 (2)	N1^iii—K3—C3^ix	131.60 (18)
O1—K1—N2^iii	130.91 (16)	N3^ix—K3—C3^ix	22.16 (15)
O1W—K1—N2^iii	69.3 (2)	N4—K3—C3^ix	148.66 (17)
N4—K1—N2^iii	105.77 (17)	C4—K3—C3^ix	153.26 (18)
O1—K1—N2^vii	81.84 (15)	O2^ix—K3—N2	149.73 (15)
O1W—K1—N2^vii	76.94 (19)	O2^i—K3—N2	78.76 (14)
N4—K1—N2^vii	159.32 (18)	N1^iii—K3—N2	68.24 (17)
N2^iii—K1—N2^vii	93.27 (16)	N3^ix—K3—N2	91.10 (16)
O1—K1—N3^viii	83.87 (15)	N4—K3—N2	95.33 (15)
O1W—K1—N3^viii	78.1 (2)	C4—K3—N2	76.80 (16)
N4—K1—N3^viii	78.28 (16)	C3^ix—K3—N2	112.88 (16)
N2^iii—K1—N3^viii	145.21 (17)	O2^ix—K3—N1^ix	81.60 (16)
N2^vii—K1—N3^viii	90.76 (16)	O2^i—K3—N1^ix	151.17 (15)
O1—K1—C4	63.50 (14)	N1^iii—K3—N1^ix	72.02 (19)
O1W—K1—C4	137.28 (19)	N3^ix—K3—N1^ix	88.72 (16)
N4—K1—C4	21.08 (14)	N4—K3—N1^ix	101.34 (17)
N2^iii—K1—C4	105.23 (17)	C4—K3—N1^ix	122.57 (17)
N2^vii—K1—C4	144.97 (17)	C3^ix—K3—N1^ix	72.30 (16)
N3^viii—K1—C4	90.46 (16)	N2—K3—N1^ix	128.28 (17)
O1—K1—K3^vii	97.99 (10)	O2^ix—K3—C2	134.43 (16)
O1W—K1—K3^vii	53.94 (16)	O2^i—K3—C2	67.60 (15)
N4—K1—K3^vii	124.32 (13)	N1^iii—K3—C2	70.79 (17)
N2^iii—K1—K3^vii	115.69 (12)	N3^ix—K3—C2	106.16 (16)
N2^vii—K1—K3^vii	49.78 (12)	N4—K3—C2	76.16 (16)
N3^viii—K1—K3^vii	46.48 (11)	C4—K3—C2	56.14 (17)
C4—K1—K3^vii	136.11 (12)	C3^ix—K3—C2	128.22 (17)
O1—K1—K1^xi	111.51 (11)	N2—K3—C2	21.37 (15)
O1W—K1—K1^xi	65.12 (17)	N1^ix—K3—C2	141.23 (17)
N4—K1—K1^xi	152.23 (14)	O2^ix—K3—C1^ix	68.76 (15)
N2^iii—K1—K1^xi	47.35 (11)	O2^i—K3—C1^ix	132.48 (15)
N2^vii—K1—K1^xi	45.91 (12)	N1^iii—K3—C1^ix	92.11 (18)
N3^viii—K1—K1^xi	126.92 (12)	N3^ix—K3—C1^ix	71.87 (16)
C4—K1—K1^xi	142.40 (13)	N4—K3—C1^ix	113.63 (16)
K3^vii—K1—K1^xi	80.57 (5)	C4—K3—C1^ix	135.82 (17)
O1—K1—K2^vi	40.70 (9)	C3^ix—K3—C1^ix	53.04 (16)
O1W—K1—K2^vi	115.13 (17)	N2—K3—C1^ix	137.58 (16)
N4—K1—K2^vi	83.06 (13)	N1^ix—K3—C1^ix	20.64 (16)
N2^iii—K1—K2^vi	167.41 (12)	C2—K3—C1^ix	156.81 (17)
N2^vii—K1—K2^vi	76.92 (13)	O2^ix—K3—O1W^v	136.77 (16)
N3^viii—K1—K2^vi	44.39 (11)	O2^i—K3—O1W^v	136.09 (15)
C4—K1—K2^vi	79.70 (12)	N1^iii—K3—O1W^v	56.15 (19)
K3^vii—K1—K2^vi	63.81 (4)	N3^ix—K3—O1W^v	72.63 (18)
K1^xi—K1—K2^vi	122.37 (6)	N4—K3—O1W^v	126.63 (19)
O1—K1—K2^ii	39.97 (9)	C4—K3—O1W^v	127.30 (19)
O1W—K1—K2^ii	122.98 (16)	C3^ix—K3—O1W^v	78.62 (19)
N4—K1—K2^ii	118.36 (12)	N2—K3—O1W^v	68.33 (16)
N2^iii—K1—K2^ii	106.90 (12)	N1^ix—K3—O1W^v	62.40 (17)
N2^vii—K1—K2^ii	46.07 (12)	C2—K3—O1W^v	87.67 (17)
N3^viii—K1—K2^ii	100.66 (11)	C1^ix—K3—O1W^v	69.53 (17)
C4—K1—K2^ii	99.45 (12)	K1—O1W—K2^x	115.3 (2)
K3^vii—K1—K2^ii	83.80 (4)	K1—O1W—H1W1	108.5
K1^xi—K1—K2^ii	72.42 (5)	K2^x—O1W—H1W1	108.5
K2^vi—K1—K2^ii	60.60 (4)	K1—O1W—H1W2	108.5
O1—K1—K2	87.43 (10)	K2^x—O1W—H1W2	108.5
O1W—K1—K2	93.46 (17)	H1W1—O1W—H1W2	107.5
N4—K1—K2	37.40 (11)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W2···N1^xi	0.82	2.12	2.930 (10)	170

Symmetry code: (xi) −x, −y+1, −z+2.