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Very stable crystals of the title compound, (CH6N3)8[PtW6O24], containing the well known A-type Anderson–Evans heteropolyoxotungstate structure, were obtained by hydro­thermal reaction. All O atoms in the polyanion form strong N—H...O hydrogen bonds with all N atoms of the guanidinium ions. The [PtW6O24]8− anion has S6 (\overline 3) symmetry, with a Pt—O bond length of 2.016 (9) Å, and three types of W—O bonds, with distances of 1.74 (1) and 1.78 (1) (Ot), 1.95 (1) (Ob), and 2.17 (1) (Oc) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680300360X/lh6036sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680300360X/lh6036Isup2.hkl
Contains datablock I

CCDC reference: 206741

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](N-C) = 0.024 Å
  • R factor = 0.049
  • wR factor = 0.106
  • Data-to-parameter ratio = 17.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998).

(I) top
Crystal data top
(CH6N3)8[PtW6O24]Dx = 3.387 Mg m3
Mr = 2162.89Mo Kα radiation, λ = 0.71069 Å
Hexagonal, R3Cell parameters from 25 reflections
Hall symbol: -R 3θ = 13.7–15.7°
a = 12.928 (2) ŵ = 19.59 mm1
c = 21.981 (5) ÅT = 298 K
V = 3181.6 (10) Å3Cubic, yellow
Z = 30.10 × 0.10 × 0.10 mm
F(000) = 2934
Data collection top
Stoe STADI4
diffractometer
1108 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 27.5°, θmin = 2.0°
ω/2–θ scansh = 168
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1996)
k = 016
Tmin = 0.120, Tmax = 0.143l = 028
1629 measured reflections3 standard reflections every 60 min
1629 independent reflections intensity decay: 3.5%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.0325P)2 + 60.3628P]
where P = (Fo2 + 2Fc2)/3
1629 reflections(Δ/σ)max < 0.001
96 parametersΔρmax = 1.46 e Å3
0 restraintsΔρmin = 2.72 e Å3
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
Pt0.00000.00000.00000.0113 (3)
W0.18149 (5)0.10481 (5)0.00160 (3)0.01744 (17)
Oc0.0221 (9)0.1236 (9)0.0449 (4)0.0172 (19)
Ob0.0468 (9)0.2294 (9)0.0431 (5)0.020 (2)
Ot10.2872 (10)0.0929 (10)0.0541 (5)0.030 (3)
Ot20.1935 (10)0.1915 (11)0.0585 (5)0.031 (3)
C10.1038 (17)0.4444 (17)0.1332 (8)0.036 (4)
C20.33330.33330.0785 (16)0.039 (8)
N10.0599 (15)0.3850 (14)0.1615 (7)0.040 (4)
H1A0.06330.37950.20050.049*
H1B0.02780.35170.14090.049*
N20.0943 (17)0.4541 (14)0.0730 (6)0.046 (5)
H2A0.06000.42190.05340.055*
H2B0.12240.49250.05370.055*
N30.1537 (12)0.4966 (13)0.1633 (6)0.030 (3)
H3A0.15810.49230.20230.036*
H3B0.18180.53490.14380.036*
N40.4163 (15)0.2181 (16)0.0808 (9)0.057 (5)
H4A0.39530.16470.08380.069*
H4B0.49070.19700.07930.069*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.0103 (4)0.0103 (4)0.0132 (6)0.00515 (19)0.0000.000
W0.0157 (3)0.0180 (3)0.0210 (3)0.0103 (3)0.0004 (3)0.0013 (3)
Oc0.015 (5)0.016 (5)0.020 (5)0.007 (4)0.005 (4)0.007 (4)
Ob0.012 (5)0.018 (5)0.024 (6)0.004 (4)0.002 (4)0.001 (4)
Ot10.029 (7)0.032 (7)0.039 (7)0.023 (6)0.015 (5)0.004 (5)
Ot20.027 (6)0.033 (7)0.030 (6)0.012 (6)0.006 (5)0.009 (5)
C10.043 (11)0.039 (11)0.027 (9)0.022 (9)0.000 (8)0.006 (7)
C20.032 (11)0.032 (11)0.05 (2)0.016 (5)0.0000.000
N10.065 (11)0.045 (10)0.029 (8)0.040 (9)0.014 (8)0.001 (7)
N20.096 (15)0.051 (10)0.019 (7)0.058 (11)0.008 (8)0.008 (7)
N30.044 (9)0.046 (9)0.014 (6)0.033 (8)0.000 (6)0.002 (6)
N40.032 (10)0.044 (11)0.099 (15)0.022 (9)0.003 (10)0.005 (11)
Geometric parameters (Å, º) top
W—Wi3.2443 (7)W—Oc2.17 (1)
Pt—W3.2437 (7)C1—N11.32 (2)
Pt—Oc2.016 (9)C1—N21.33 (2)
W—Ot11.78 (1)C1—N31.32 (2)
W—Ot21.74 (1)C2—N41.33 (2)
W—Ob1.95 (1)
Ocii—Pt—Ociii81.9 (3)Ot2—W—Oc89.9 (5)
Ocii—Pt—Oc180.0 (7)Ot1—W—Oc162.6 (5)
Ociii—Pt—Oc98.1 (3)Obiv—W—Oc89.5 (4)
Ot2—W—Ot1103.8 (5)Ob—W—Oc73.8 (4)
Ot2—W—Obiv95.7 (5)Ociv—W—Oc75.0 (5)
Ot1—W—Obiv99.6 (5)Pt—W—Wi60.0
Ot2—W—Ob99.2 (5)N1—C1—N3122 (2)
Ot1—W—Ob93.1 (5)N1—C1—N2119 (2)
Obiv—W—Ob157.5 (6)N3—C1—N2120 (2)
Ot2—W—Ociv161.5 (5)N4v—C2—N4119.9 (2)
Ot1—W—Ociv93.2 (4)N4v—C2—N4vi119.9 (2)
Obiv—W—Ociv74.0 (4)N4—C2—N4vi119.9 (2)
Ob—W—Ociv87.0 (4)
Symmetry codes: (i) y, x+y, z; (ii) x, y, z; (iii) x+y, x, z; (iv) xy, x, z; (v) y, xy+1, z; (vi) x+y1, x, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Obvii0.861.972.83 (2)175
N1—H1B···Ot1i0.862.373.10 (2)142
N2—H2A···Ot1i0.862.303.04 (3)145
N2—H2B···Ot2v0.862.182.94 (2)147
N2—H2A···Ot20.862.592.99 (2)109
N3—H3A···Ocviii0.861.992.83 (2)165
N3—H3B···Ot2v0.862.182.94 (2)148
N4—H4A···Ot10.862.132.91 (2)150
Symmetry codes: (i) y, x+y, z; (v) y, xy+1, z; (vii) x+y1/3, x+1/3, z+1/3; (viii) y1/3, x+y+1/3, z+1/3.
 

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