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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805027534/hb6257sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805027534/hb6257Isup2.hkl
Contains datablock I

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

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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

Comment top

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).

Experimental top

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.

Refinement top

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

Computing details top

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 top
[Figure 1] 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 top
Crystal data top
K6[Os2(CN)8(SO2)2]·2H2OZ = 1
Mr = 987.31F(000) = 454
Triclinic, P1Dx = 2.898 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.9496 (10) ÅCell parameters from 24 reflections
b = 8.9222 (11) Åθ = 11.5–14.9°
c = 8.9747 (15) ŵ = 12.55 mm1
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) Å3
Data collection top
Enraf–Nonius CAD-4
diffractometer
1817 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.0°, θmin = 2.3°
2θ/θ scansh = 09
Absorption correction: integration
(CADDAT; Enraf–Nonius, 1989)
k = 1010
Tmin = 0.157, Tmax = 0.591l = 910
2150 measured reflections3 standard reflections every 60 min
1991 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.054 w = 1/[σ2(Fo2) + (0.0288P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
1991 reflectionsΔρmax = 1.39 e Å3
146 parametersΔρmin = 1.62 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0010 (3)
Crystal data top
K6[Os2(CN)8(SO2)2]·2H2Oγ = 81.677 (12)°
Mr = 987.31V = 565.66 (14) Å3
Triclinic, P1Z = 1
a = 7.9496 (10) ÅMo Kα radiation
b = 8.9222 (11) ŵ = 12.55 mm1
c = 8.9747 (15) ÅT = 293 K
α = 84.202 (15)°0.19 × 0.16 × 0.04 mm
β = 64.013 (12)°
Data collection top
Enraf–Nonius CAD-4
diffractometer
1817 reflections with I > 2σ(I)
Absorption correction: integration
(CADDAT; Enraf–Nonius, 1989)
Rint = 0.020
Tmin = 0.157, Tmax = 0.5913 standard reflections every 60 min
2150 measured reflections intensity decay: none
1991 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0210 restraints
wR(F2) = 0.054H-atom parameters constrained
S = 1.05Δρmax = 1.39 e Å3
1991 reflectionsΔρmin = 1.62 e Å3
146 parameters
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 > 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 (Å2) top
xyzUiso*/Ueq
Os10.50423 (3)0.15519 (3)0.44271 (3)0.01385 (11)
C10.3167 (9)0.3473 (7)0.5023 (8)0.0208 (13)
N10.1999 (8)0.4450 (7)0.5394 (8)0.0360 (15)
C20.7065 (9)0.2772 (7)0.2658 (8)0.0212 (14)
N20.8324 (8)0.3332 (7)0.1642 (7)0.0306 (13)
C30.4138 (8)0.1294 (7)0.2650 (8)0.0200 (13)
N30.3594 (7)0.1348 (7)0.1636 (7)0.0274 (13)
C40.5837 (8)0.2101 (7)0.6172 (7)0.0184 (13)
N40.6234 (8)0.2525 (7)0.7126 (7)0.0283 (13)
S10.25549 (19)0.04233 (17)0.65172 (17)0.0153 (3)
O10.1910 (6)0.0887 (5)0.8251 (5)0.0218 (9)
O20.0878 (5)0.0346 (5)0.6220 (5)0.0223 (10)
K10.2354 (2)0.35137 (19)0.9328 (2)0.0359 (4)
K20.78033 (19)0.11126 (19)0.92833 (17)0.0284 (3)
K30.99342 (19)0.24828 (17)0.42294 (18)0.0268 (3)
O1W0.1761 (10)0.5399 (9)1.1831 (8)0.077 (2)
H1W10.25080.50871.22260.093*
H1W20.06970.53361.25680.093*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Os10.01318 (14)0.01358 (14)0.01335 (14)0.00233 (9)0.00418 (9)0.00033 (9)
C10.023 (3)0.016 (3)0.025 (3)0.000 (3)0.012 (3)0.006 (3)
N10.033 (3)0.026 (3)0.046 (4)0.004 (3)0.015 (3)0.013 (3)
C20.026 (3)0.019 (3)0.022 (3)0.001 (3)0.014 (3)0.003 (3)
N20.030 (3)0.032 (3)0.025 (3)0.014 (3)0.006 (3)0.006 (3)
C30.017 (3)0.021 (3)0.019 (3)0.006 (3)0.004 (3)0.000 (3)
N30.028 (3)0.033 (4)0.022 (3)0.006 (3)0.011 (2)0.000 (3)
C40.015 (3)0.020 (3)0.016 (3)0.003 (3)0.003 (2)0.002 (3)
N40.029 (3)0.033 (4)0.026 (3)0.008 (3)0.013 (3)0.001 (3)
S10.0135 (6)0.0157 (8)0.0143 (7)0.0020 (6)0.0038 (6)0.0000 (6)
O10.024 (2)0.024 (2)0.014 (2)0.0030 (19)0.0041 (18)0.0030 (19)
O20.017 (2)0.027 (3)0.024 (2)0.0066 (18)0.0087 (18)0.003 (2)
K10.0345 (8)0.0290 (9)0.0361 (9)0.0037 (7)0.0063 (7)0.0077 (7)
K20.0232 (7)0.0398 (9)0.0194 (7)0.0026 (6)0.0070 (6)0.0007 (7)
K30.0229 (7)0.0273 (8)0.0299 (8)0.0020 (6)0.0114 (6)0.0011 (7)
O1W0.088 (5)0.097 (6)0.058 (4)0.025 (5)0.036 (4)0.007 (4)
Geometric parameters (Å, º) top
Os1—C12.048 (6)N4—K32.949 (6)
Os1—C42.050 (6)S1—O21.482 (4)
Os1—C22.052 (7)S1—O11.491 (4)
Os1—C32.059 (6)S1—Os1i2.3198 (15)
Os1—S1i2.3198 (15)O1—K12.747 (5)
Os1—S12.3210 (15)O1—K2vi2.768 (5)
Os1—Os1i2.8546 (6)O1—K2ii2.958 (4)
C1—N11.134 (9)O2—K3ii2.731 (5)
C1—K3ii3.206 (6)O2—K3i2.803 (5)
N1—K3iii2.912 (6)O2—K2ii2.830 (4)
N1—K3ii3.095 (6)K1—O1W2.775 (7)
C2—N21.156 (8)K1—N2iii2.906 (6)
C2—K33.136 (6)K1—N2vii2.976 (6)
C2—K2iv3.287 (6)K1—N3viii3.069 (6)
N2—K1iii2.906 (6)K2—O1vi2.768 (5)
N2—K1v2.976 (6)K2—O2ix2.830 (4)
N2—K33.094 (6)K2—N3i2.934 (6)
N2—K2iv3.229 (6)K2—O1ix2.958 (4)
C3—N31.162 (8)K2—N3viii3.065 (6)
C3—K3ii3.071 (6)K2—O1Wx3.191 (8)
C3—K2iv3.145 (6)K2—N2viii3.229 (6)
N3—K3ii2.932 (6)K3—O2ix2.731 (5)
N3—K2i2.934 (6)K3—O2i2.803 (5)
N3—K2iv3.065 (6)K3—N1iii2.912 (6)
N3—K1iv3.069 (6)K3—N3ix2.932 (6)
C4—N41.146 (8)K3—N1ix3.095 (6)
C4—K32.998 (6)K3—O1Wv3.277 (8)
C4—K13.181 (6)O1W—K2x3.191 (8)
N4—K22.839 (6)O1W—H1W10.8200
N4—K12.901 (6)O1W—H1W20.8200
C1—Os1—C487.1 (2)N2iii—K1—K2126.66 (12)
C1—Os1—C290.3 (3)N2vii—K1—K2132.88 (13)
C4—Os1—C289.5 (2)N3viii—K1—K242.34 (10)
C1—Os1—C386.2 (2)C4—K1—K254.59 (11)
C4—Os1—C3172.6 (2)K3vii—K1—K287.13 (4)
C2—Os1—C387.3 (2)K1xi—K1—K2158.57 (7)
C1—Os1—S1i172.38 (18)K2vi—K1—K265.71 (4)
C4—Os1—S1i93.07 (17)K2ii—K1—K2123.82 (5)
C2—Os1—S1i82.11 (18)O1vi—K2—O2ix108.79 (13)
C3—Os1—S1i93.12 (18)O1vi—K2—N4156.88 (15)
C1—Os1—S183.54 (18)O2ix—K2—N481.45 (15)
C4—Os1—S189.29 (16)O1vi—K2—N3i86.10 (15)
C2—Os1—S1173.75 (18)O2ix—K2—N3i79.53 (14)
C3—Os1—S193.10 (17)N4—K2—N3i75.22 (16)
S1i—Os1—S1104.08 (4)O1vi—K2—O1ix80.17 (13)
C1—Os1—Os1i135.56 (18)O2ix—K2—O1ix49.25 (11)
C4—Os1—Os1i91.92 (18)N4—K2—O1ix120.33 (15)
C2—Os1—Os1i134.16 (18)N3i—K2—O1ix116.93 (15)
C3—Os1—Os1i95.06 (18)O1vi—K2—N3viii82.98 (14)
S1i—Os1—Os1i52.06 (4)O2ix—K2—N3viii151.66 (14)
S1—Os1—Os1i52.02 (4)N4—K2—N3viii79.30 (16)
N1—C1—Os1173.6 (6)N3i—K2—N3viii75.58 (18)
N1—C1—K3ii74.1 (4)O1ix—K2—N3viii158.04 (14)
Os1—C1—K3ii100.4 (2)O1vi—K2—C3viii66.58 (15)
C1—N1—K3iii161.1 (6)O2ix—K2—C3viii167.87 (16)
C1—N1—K3ii85.2 (5)N4—K2—C3viii99.02 (16)
K3iii—N1—K3ii107.98 (19)N3i—K2—C3viii88.84 (16)
N2—C2—Os1173.4 (6)O1ix—K2—C3viii136.53 (14)
N2—C2—K377.3 (4)N3viii—K2—C3viii21.51 (14)
Os1—C2—K399.4 (2)O1vi—K2—O1Wx137.97 (15)
N2—C2—K2iv77.0 (4)O2ix—K2—O1Wx88.41 (16)
Os1—C2—K2iv100.7 (2)N4—K2—O1Wx60.63 (17)
K3—C2—K2iv124.6 (2)N3i—K2—O1Wx135.51 (17)
C2—N2—K1iii117.7 (5)O1ix—K2—O1Wx83.61 (16)
C2—N2—K1v155.3 (5)N3viii—K2—O1Wx99.91 (18)
K1iii—N2—K1v86.73 (16)C3viii—K2—O1Wx102.44 (18)
C2—N2—K381.3 (4)O1vi—K2—N2viii77.87 (14)
K1iii—N2—K3120.6 (2)O2ix—K2—N2viii119.01 (14)
K1v—N2—K382.96 (15)N4—K2—N2viii116.05 (17)
C2—N2—K2iv82.6 (4)N3i—K2—N2viii158.54 (15)
K1iii—N2—K2iv110.53 (18)O1ix—K2—N2viii74.54 (13)
K1v—N2—K2iv92.35 (16)N3viii—K2—N2viii88.26 (15)
K3—N2—K2iv128.2 (2)C3viii—K2—N2viii71.81 (15)
N3—C3—Os1171.3 (6)O1Wx—K2—N2viii60.45 (16)
N3—C3—K3ii72.2 (4)O1vi—K2—C2viii66.37 (15)
Os1—C3—K3ii104.5 (2)O2ix—K2—C2viii137.53 (14)
N3—C3—K2iv75.4 (4)N4—K2—C2viii120.25 (17)
Os1—C3—K2iv105.2 (2)N3i—K2—C2viii138.33 (16)
K3ii—C3—K2iv143.6 (2)O1ix—K2—C2viii89.60 (14)
C3—N3—K3ii85.7 (4)N3viii—K2—C2viii70.70 (15)
C3—N3—K2i127.0 (5)C3viii—K2—C2viii52.31 (16)
K3ii—N3—K2i95.55 (16)O1Wx—K2—C2viii75.05 (17)
C3—N3—K2iv83.1 (4)N2viii—K2—C2viii20.41 (15)
K3ii—N3—K2iv160.0 (2)O1vi—K2—S1ix94.77 (10)
K2i—N3—K2iv104.42 (18)O2ix—K2—S1ix24.28 (8)
C3—N3—K1iv143.8 (5)N4—K2—S1ix101.18 (12)
K3ii—N3—K1iv84.12 (15)N3i—K2—S1ix98.15 (12)
K2i—N3—K1iv88.57 (15)O1ix—K2—S1ix24.97 (8)
K2iv—N3—K1iv95.24 (16)N3viii—K2—S1ix173.44 (13)
N4—C4—Os1174.6 (6)C3viii—K2—S1ix159.71 (12)
N4—C4—K376.5 (4)O1Wx—K2—S1ix85.91 (14)
Os1—C4—K3103.9 (2)N2viii—K2—S1ix97.32 (11)
N4—C4—K165.6 (4)C2viii—K2—S1ix114.09 (12)
Os1—C4—K1112.1 (2)O1vi—K2—S1vi19.49 (9)
K3—C4—K1137.5 (2)O2ix—K2—S1vi124.62 (10)
C4—N4—K2134.6 (5)N4—K2—S1vi152.76 (12)
C4—N4—K193.3 (4)N3i—K2—S1vi99.99 (12)
K2—N4—K1104.24 (18)O1ix—K2—S1vi86.04 (9)
C4—N4—K381.3 (4)N3viii—K2—S1vi73.58 (11)
K2—N4—K393.16 (16)C3viii—K2—S1vi53.80 (12)
K1—N4—K3159.8 (2)O1Wx—K2—S1vi121.52 (12)
O2—S1—O1108.6 (2)N2viii—K2—S1vi61.30 (11)
O2—S1—Os1i116.86 (19)C2viii—K2—S1vi47.44 (12)
O1—S1—Os1i117.60 (18)S1ix—K2—S1vi106.05 (5)
O2—S1—Os1117.13 (18)O2ix—K3—O2i70.97 (14)
O1—S1—Os1117.96 (18)O2ix—K3—N1iii135.86 (17)
Os1i—S1—Os175.92 (4)O2i—K3—N1iii134.96 (15)
S1—O1—K1128.9 (2)O2ix—K3—N3ix84.13 (15)
S1—O1—K2vi122.3 (2)O2i—K3—N3ix80.01 (15)
K1—O1—K2vi98.97 (14)N1iii—K3—N3ix128.63 (18)
S1—O1—K2ii98.16 (19)O2ix—K3—N481.15 (15)
K1—O1—K2ii103.41 (14)O2i—K3—N483.43 (15)
K2vi—O1—K2ii99.83 (13)N1iii—K3—N470.52 (18)
S1—O2—K3ii120.9 (2)N3ix—K3—N4160.70 (17)
S1—O2—K3i119.1 (2)O2ix—K3—C491.34 (15)
K3ii—O2—K3i109.03 (14)O2i—K3—C468.11 (15)
S1—O2—K2ii104.0 (2)N1iii—K3—C474.97 (18)
K3ii—O2—K2ii98.24 (14)N3ix—K3—C4147.45 (17)
K3i—O2—K2ii100.92 (13)N4—K3—C422.20 (15)
O1—K1—O1W151.76 (19)O2ix—K3—C3ix67.63 (15)
O1—K1—N479.60 (15)O2i—K3—C3ix88.77 (15)
O1W—K1—N4117.0 (2)N1iii—K3—C3ix131.60 (18)
O1—K1—N2iii130.91 (16)N3ix—K3—C3ix22.16 (15)
O1W—K1—N2iii69.3 (2)N4—K3—C3ix148.66 (17)
N4—K1—N2iii105.77 (17)C4—K3—C3ix153.26 (18)
O1—K1—N2vii81.84 (15)O2ix—K3—N2149.73 (15)
O1W—K1—N2vii76.94 (19)O2i—K3—N278.76 (14)
N4—K1—N2vii159.32 (18)N1iii—K3—N268.24 (17)
N2iii—K1—N2vii93.27 (16)N3ix—K3—N291.10 (16)
O1—K1—N3viii83.87 (15)N4—K3—N295.33 (15)
O1W—K1—N3viii78.1 (2)C4—K3—N276.80 (16)
N4—K1—N3viii78.28 (16)C3ix—K3—N2112.88 (16)
N2iii—K1—N3viii145.21 (17)O2ix—K3—N1ix81.60 (16)
N2vii—K1—N3viii90.76 (16)O2i—K3—N1ix151.17 (15)
O1—K1—C463.50 (14)N1iii—K3—N1ix72.02 (19)
O1W—K1—C4137.28 (19)N3ix—K3—N1ix88.72 (16)
N4—K1—C421.08 (14)N4—K3—N1ix101.34 (17)
N2iii—K1—C4105.23 (17)C4—K3—N1ix122.57 (17)
N2vii—K1—C4144.97 (17)C3ix—K3—N1ix72.30 (16)
N3viii—K1—C490.46 (16)N2—K3—N1ix128.28 (17)
O1—K1—K3vii97.99 (10)O2ix—K3—C2134.43 (16)
O1W—K1—K3vii53.94 (16)O2i—K3—C267.60 (15)
N4—K1—K3vii124.32 (13)N1iii—K3—C270.79 (17)
N2iii—K1—K3vii115.69 (12)N3ix—K3—C2106.16 (16)
N2vii—K1—K3vii49.78 (12)N4—K3—C276.16 (16)
N3viii—K1—K3vii46.48 (11)C4—K3—C256.14 (17)
C4—K1—K3vii136.11 (12)C3ix—K3—C2128.22 (17)
O1—K1—K1xi111.51 (11)N2—K3—C221.37 (15)
O1W—K1—K1xi65.12 (17)N1ix—K3—C2141.23 (17)
N4—K1—K1xi152.23 (14)O2ix—K3—C1ix68.76 (15)
N2iii—K1—K1xi47.35 (11)O2i—K3—C1ix132.48 (15)
N2vii—K1—K1xi45.91 (12)N1iii—K3—C1ix92.11 (18)
N3viii—K1—K1xi126.92 (12)N3ix—K3—C1ix71.87 (16)
C4—K1—K1xi142.40 (13)N4—K3—C1ix113.63 (16)
K3vii—K1—K1xi80.57 (5)C4—K3—C1ix135.82 (17)
O1—K1—K2vi40.70 (9)C3ix—K3—C1ix53.04 (16)
O1W—K1—K2vi115.13 (17)N2—K3—C1ix137.58 (16)
N4—K1—K2vi83.06 (13)N1ix—K3—C1ix20.64 (16)
N2iii—K1—K2vi167.41 (12)C2—K3—C1ix156.81 (17)
N2vii—K1—K2vi76.92 (13)O2ix—K3—O1Wv136.77 (16)
N3viii—K1—K2vi44.39 (11)O2i—K3—O1Wv136.09 (15)
C4—K1—K2vi79.70 (12)N1iii—K3—O1Wv56.15 (19)
K3vii—K1—K2vi63.81 (4)N3ix—K3—O1Wv72.63 (18)
K1xi—K1—K2vi122.37 (6)N4—K3—O1Wv126.63 (19)
O1—K1—K2ii39.97 (9)C4—K3—O1Wv127.30 (19)
O1W—K1—K2ii122.98 (16)C3ix—K3—O1Wv78.62 (19)
N4—K1—K2ii118.36 (12)N2—K3—O1Wv68.33 (16)
N2iii—K1—K2ii106.90 (12)N1ix—K3—O1Wv62.40 (17)
N2vii—K1—K2ii46.07 (12)C2—K3—O1Wv87.67 (17)
N3viii—K1—K2ii100.66 (11)C1ix—K3—O1Wv69.53 (17)
C4—K1—K2ii99.45 (12)K1—O1W—K2x115.3 (2)
K3vii—K1—K2ii83.80 (4)K1—O1W—H1W1108.5
K1xi—K1—K2ii72.42 (5)K2x—O1W—H1W1108.5
K2vi—K1—K2ii60.60 (4)K1—O1W—H1W2108.5
O1—K1—K287.43 (10)K2x—O1W—H1W2108.5
O1W—K1—K293.46 (17)H1W1—O1W—H1W2107.5
N4—K1—K237.40 (11)
Symmetry codes: (i) x+1, y, z+1; (ii) x1, y, z; (iii) x+1, y+1, z+1; (iv) x, y, z1; (v) x+1, y, z1; (vi) x+1, y, z+2; (vii) x1, 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) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W2···N1xi0.822.122.930 (10)170
Symmetry code: (xi) x, y+1, z+2.

Experimental details

Crystal data
Chemical formulaK6[Os2(CN)8(SO2)2]·2H2O
Mr987.31
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.9496 (10), 8.9222 (11), 8.9747 (15)
α, β, γ (°)84.202 (15), 64.013 (12), 81.677 (12)
V3)565.66 (14)
Z1
Radiation typeMo Kα
µ (mm1)12.55
Crystal size (mm)0.19 × 0.16 × 0.04
Data collection
DiffractometerEnraf–Nonius CAD-4
diffractometer
Absorption correctionIntegration
(CADDAT; Enraf–Nonius, 1989)
Tmin, Tmax0.157, 0.591
No. of measured, independent and
observed [I > 2σ(I)] reflections
2150, 1991, 1817
Rint0.020
(sin θ/λ)max1)0.594
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.054, 1.05
No. of reflections1991
No. of parameters146
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.39, 1.62

Computer programs: CD4CA0 (Enraf–Nonius, 1989), CD4CA0, CADDAT (Enraf–Nonius, 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), BS (Kang & Ozawa, 2002), SHELXL97.

Selected bond lengths (Å) top
Os1—C12.048 (6)Os1—C32.059 (6)
Os1—C42.050 (6)Os1—S1i2.3198 (15)
Os1—C22.052 (7)Os1—S12.3210 (15)
Symmetry code: (i) x+1, y, z+1.
 

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