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Acta Crystallogr Sect E Struct Rep Online. 2010 August 1; 66(Pt 8): m928.
Published online 2010 July 14. doi:  10.1107/S1600536810027133
PMCID: PMC3007281

Poly[diaqua­[3,5-bis­(trifluoro­meth­yl)pyrazolido]potassium]

Abstract

The asymmetric unit of the title compound, [K(C5HF6N2)(H2O)2]n, is composed of two 3,5-bis­(trifluoro­meth­yl)pyrazol­ide anions, two potassium cations and four water mol­ecules. The water mol­ecules and 3,5-bis­(trifluoro­meth­yl)pyrazolide anions act as bridges between the potassium cations. Each potassium cation is surrounded by four O atoms [K—O = 2.705 (3)–2.767 (3) Å] and four F atoms [K—F = 2.870 (7)–3.215 (13) Å]. The water mol­ecules and the 3,5-bis­(trifluoro­meth­yl)pyrazolide anions are connected by O—H(...)N hydrogen bonds, forming layers in the ab plane. All –CF3 groups show rotational disorder between two orientations each.

Related literature

For related literature on pyrazolides, see: Bieller et al. (2006 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m928-scheme1.jpg

Experimental

Crystal data

  • [K(C5HF6N2)(H2O)2]
  • M r = 278.21
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m928-efi1.jpg
  • a = 9.7453 (9) Å
  • b = 9.8179 (10) Å
  • c = 12.5243 (14) Å
  • α = 67.756 (8)°
  • β = 78.178 (8)°
  • γ = 88.758 (8)°
  • V = 1083.53 (19) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.56 mm−1
  • T = 173 K
  • 0.41 × 0.40 × 0.38 mm

Data collection

  • Stoe IPDS II two-circle diffractometer
  • Absorption correction: multi-scan (MULABS; Spek, 2009 [triangle]; Blessing, 1995 [triangle]) T min = 0.802, T max = 0.815
  • 11313 measured reflections
  • 4027 independent reflections
  • 3316 reflections with I > 2σ(I)
  • R int = 0.039

Refinement

  • R[F 2 > 2σ(F 2)] = 0.049
  • wR(F 2) = 0.124
  • S = 1.13
  • 4027 reflections
  • 425 parameters
  • 704 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.55 e Å−3
  • Δρmin = −0.34 e Å−3

Data collection: X-AREA (Stoe & Cie, 2001 [triangle]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: XP (Sheldrick, 2008 [triangle]) and Mercury (Macrae et al., 2006 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810027133/cv2744sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810027133/cv2744Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

Recently we have reported the structures of pyrazolides which possess substituents in a 3- or 4-position (Bieller et al., 2006). In this paper we report the synthesis and the crystal structure of the 3,5-substituted potassium pyrazolide [K(H2O)2][3,5-(CF3)2C3HN2] (I). The starting matrial for the synthesis of (I), 3,5-bis(trifluoromethyl)pyrazole, was prepared from hexafluoroacetylacetone CF3COCH2COCF3 and hydrazine hydrate N2H4.H2O. By a following reaction of one equivalent of KH and one equivalent of 3,5-bis(trifluoromethyl)pyrazole in ethanol the potassium pyrazolide (I) was accessible in nearly quantitive yield.

The asymmetric unit of the title compound is composed of two 3,5-bis(trifluoromethyl)pyrazolide anions, two potassium cations and four water molecules. The water molecules and 3,5-bis(trifluoromethyl)pyrazolide anions act as bridges between the potassium cations. Each potassium cation is bonded to four O atoms and four F atoms. The K—O distances range from 2.705 (3)Å (K2—O4) to 2.767 (3)Å (K1—O3) and the K—F distances range from 2.870 (7)Å (K2—F162) to 3.215 (13)Å (K2—F17'). The water molecules and the 3,5-bis(trifluoromethyl)pyrazolide anions are connected by O—H···N hydrogen bonds forming layers in the ab plane The CF3 groups show rotational disorder.

Experimental

3,5-Bis(trifluoromethyl)pyrazole: Hydrazine hydrate N2H4.H2O (2.65 g, 52.87 mmol) and hexafluoroacetylacetone CF3COCH2COCF3 (10.0 g, 6.8 ml, 48.06 mmol) were combined in ethanol (100 ml) under ambient conditions, forming a clear solution. The solution was heated under reflux for 5 h. After addition of a small amount of Na2SO4 the reaction mixture was heated again for 6 h. After removing the solvent pure, colorless 3,5-bis(trifluoromethyl)pyrazole was obtained by sublimation (373 K, normal pressure) in 79% yield.

Potassium 3,5-bis(trifluoromethyl)pyrazolide (I): To a slurry of KH (138 mg, 3.44 mmol) in 15 ml of tetrahydrofuran was added a solution of 3,5-bis(trifluoromethyl)pyrazole (820 mg, 4.02 mmol) in 15 ml tetrahydrofuran at 273 K. The resulting solution was allowed to warm up to room temperature. After removing the solvent in vacuo the obtained residue was recrystallized from wet tetrahydrofuran (yield 92%).

Refinement

H atoms were found in a difference map but those bonded to C were refined with fixed individual displacement parameters [Uiso(H) = 1.2 Ueq(C)] using a riding model with C—H = 0.95 Å. H atoms bonded to O were refined with Uiso(H) = 1.2 Ueq(O) and a distance restraint of 0.82 (1) Å. The four trifluoromethyl groups are disordered over two positions each with site occupation factors of 0.69 (4), 0.52 (3), 0.57 (3) and 0.69 (3) for the major occupied sites. The C—F bond lengths and the equivalent F···F distances were restrained to be equal with an effective s.u. of 0.02 Å. The anisotropic displacement ellipsoids of the F atoms were restrained to an isotropic behaviour.

Figures

Fig. 1.
Perspective view of the asymmetric unit of the title compound with the atom numbering scheme; displacement ellipsoids are at the 50% probability level; H atoms are drawn as small spheres of arbitrary radii. Only major components of the disordered CF3 ...
Fig. 2.
A portion of the packing diagram showing the layer structure. Only major components of the disordered CF3 groups are shown.

Crystal data

[K(C5HF6N2)(H2O)2]Z = 4
Mr = 278.21F(000) = 552
Triclinic, P1Dx = 1.705 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.7453 (9) ÅCell parameters from 10340 reflections
b = 9.8179 (10) Åθ = 3.6–25.7°
c = 12.5243 (14) ŵ = 0.56 mm1
α = 67.756 (8)°T = 173 K
β = 78.178 (8)°Block, colourless
γ = 88.758 (8)°0.41 × 0.40 × 0.38 mm
V = 1083.53 (19) Å3

Data collection

Stoe IPDS II two-circle diffractometer4027 independent reflections
Radiation source: fine-focus sealed tube3316 reflections with I > 2σ(I)
graphiteRint = 0.039
ω scansθmax = 25.6°, θmin = 3.6°
Absorption correction: multi-scan (MULABS; Spek, 2009; Blessing, 1995)h = −11→11
Tmin = 0.802, Tmax = 0.815k = −11→11
11313 measured reflectionsl = −15→15

Refinement

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) = 0.124H atoms treated by a mixture of independent and constrained refinement
S = 1.13w = 1/[σ2(Fo2) + (0.0432P)2 + 1.5007P] where P = (Fo2 + 2Fc2)/3
4027 reflections(Δ/σ)max < 0.001
425 parametersΔρmax = 0.55 e Å3
704 restraintsΔρmin = −0.34 e Å3

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 (Å2)

xyzUiso*/UeqOcc. (<1)
K10.39698 (8)0.67416 (8)0.37909 (7)0.0306 (2)
K20.08656 (8)0.81180 (8)0.61839 (8)0.0317 (2)
O10.3599 (3)0.8616 (3)0.4958 (2)0.0302 (6)
H1A0.368 (5)0.9497 (17)0.455 (3)0.036*
H1B0.410 (4)0.841 (5)0.544 (3)0.036*
O20.1232 (3)0.6242 (3)0.5002 (3)0.0341 (6)
H2A0.104 (5)0.539 (2)0.547 (3)0.041*
H2B0.075 (4)0.630 (5)0.453 (3)0.041*
O30.3856 (3)0.3788 (3)0.5015 (2)0.0298 (6)
H3A0.407 (4)0.337 (4)0.456 (3)0.036*
H3B0.314 (3)0.335 (4)0.549 (3)0.036*
O40.1246 (3)1.1129 (3)0.4996 (3)0.0322 (6)
H4A0.199 (3)1.128 (5)0.452 (3)0.039*
H4B0.128 (5)1.152 (4)0.546 (3)0.039*
N10.1337 (3)0.2318 (3)0.6765 (3)0.0326 (7)
N20.0336 (3)0.3299 (3)0.6808 (3)0.0338 (7)
C3−0.0136 (4)0.3079 (4)0.7954 (4)0.0359 (9)
C40.0550 (4)0.1969 (4)0.8683 (4)0.0378 (9)
H40.04280.16060.95180.045*
C50.1458 (4)0.1523 (4)0.7882 (3)0.0306 (8)
C6−0.1252 (5)0.3993 (5)0.8265 (4)0.0512 (12)
C70.2477 (4)0.0352 (5)0.8098 (4)0.0435 (10)
N110.3789 (3)0.1607 (3)0.3208 (3)0.0332 (7)
N120.4741 (3)0.2560 (3)0.3258 (3)0.0319 (7)
C130.5380 (4)0.3394 (4)0.2138 (3)0.0287 (8)
C140.4871 (4)0.3002 (4)0.1328 (3)0.0356 (9)
H140.51420.33980.04910.043*
C150.3864 (4)0.1881 (4)0.2058 (3)0.0339 (8)
C160.6470 (4)0.4559 (4)0.1921 (3)0.0367 (9)
C170.2902 (5)0.1001 (5)0.1750 (4)0.0492 (11)
F61−0.2511 (7)0.3608 (16)0.8164 (17)0.083 (3)0.69 (4)
F62−0.141 (2)0.3797 (16)0.9412 (6)0.083 (3)0.69 (4)
F63−0.1015 (14)0.5433 (9)0.7639 (14)0.072 (3)0.69 (4)
F61'−0.233 (2)0.413 (3)0.768 (3)0.064 (6)0.31 (4)
F62'−0.188 (3)0.354 (2)0.9391 (12)0.062 (5)0.31 (4)
F63'−0.076 (3)0.5390 (19)0.796 (2)0.053 (5)0.31 (4)
F710.259 (2)−0.040 (2)0.7424 (16)0.073 (4)0.48 (3)
F720.3831 (9)0.0999 (13)0.7868 (15)0.063 (4)0.48 (3)
F730.2264 (18)−0.053 (2)0.9224 (9)0.053 (3)0.48 (3)
F71'0.1992 (18)−0.0831 (11)0.7881 (14)0.062 (3)0.52 (3)
F72'0.3724 (13)0.0738 (14)0.7403 (16)0.085 (5)0.52 (3)
F73'0.2595 (19)−0.0300 (18)0.9222 (9)0.048 (3)0.52 (3)
F1610.6176 (13)0.5317 (19)0.2597 (15)0.074 (4)0.56 (3)
F1620.7721 (8)0.3939 (10)0.2141 (13)0.060 (3)0.56 (3)
F1630.6807 (15)0.5469 (16)0.0798 (8)0.056 (3)0.56 (3)
F16'0.5838 (12)0.5759 (11)0.2114 (14)0.052 (3)0.44 (3)
F16"0.737 (2)0.4186 (15)0.2627 (18)0.077 (5)0.44 (3)
F16*0.7155 (19)0.5199 (18)0.0808 (10)0.051 (3)0.44 (3)
F1710.1522 (14)0.085 (3)0.240 (3)0.072 (6)0.31 (3)
F1720.327 (3)−0.0401 (16)0.204 (2)0.054 (5)0.31 (3)
F1730.276 (3)0.147 (2)0.0655 (13)0.069 (5)0.31 (3)
F17'0.1599 (10)0.1422 (15)0.1863 (15)0.083 (3)0.69 (3)
F17"0.2852 (16)−0.0440 (8)0.2354 (12)0.071 (3)0.69 (3)
F17*0.3321 (18)0.1236 (12)0.0586 (5)0.083 (3)0.69 (3)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
K10.0294 (4)0.0256 (4)0.0395 (5)0.0024 (3)−0.0082 (3)−0.0150 (3)
K20.0276 (4)0.0264 (4)0.0422 (5)0.0031 (3)−0.0106 (3)−0.0126 (4)
O10.0291 (13)0.0230 (12)0.0404 (16)0.0028 (10)−0.0151 (11)−0.0101 (12)
O20.0285 (14)0.0260 (13)0.0490 (18)0.0002 (11)−0.0149 (12)−0.0122 (13)
O30.0251 (13)0.0299 (14)0.0362 (16)−0.0018 (10)−0.0002 (11)−0.0177 (12)
O40.0236 (13)0.0334 (14)0.0474 (18)0.0031 (11)−0.0082 (12)−0.0238 (13)
N10.0297 (16)0.0310 (16)0.0386 (19)0.0058 (13)−0.0028 (13)−0.0176 (15)
N20.0324 (16)0.0315 (17)0.0379 (19)0.0099 (13)−0.0064 (14)−0.0147 (15)
C30.034 (2)0.0299 (19)0.038 (2)−0.0014 (16)0.0058 (16)−0.0143 (17)
C40.047 (2)0.034 (2)0.027 (2)0.0008 (17)0.0003 (17)−0.0107 (17)
C50.0298 (18)0.0280 (19)0.032 (2)0.0000 (14)−0.0046 (15)−0.0102 (16)
C60.050 (3)0.040 (2)0.058 (3)0.005 (2)0.009 (2)−0.022 (2)
C70.049 (3)0.038 (2)0.037 (2)0.0113 (19)−0.0088 (19)−0.0077 (19)
N110.0379 (17)0.0306 (16)0.0335 (18)−0.0010 (13)−0.0097 (14)−0.0134 (14)
N120.0391 (17)0.0276 (16)0.0333 (18)0.0013 (13)−0.0119 (14)−0.0141 (14)
C130.0320 (18)0.0254 (18)0.0281 (19)0.0057 (14)−0.0059 (15)−0.0101 (15)
C140.052 (2)0.031 (2)0.0240 (19)0.0079 (17)−0.0116 (17)−0.0091 (16)
C150.047 (2)0.0271 (19)0.032 (2)0.0101 (16)−0.0173 (17)−0.0121 (16)
C160.037 (2)0.034 (2)0.033 (2)−0.0007 (16)−0.0033 (17)−0.0082 (18)
C170.065 (3)0.041 (2)0.052 (3)0.005 (2)−0.029 (2)−0.019 (2)
F610.041 (3)0.077 (5)0.118 (7)0.014 (3)0.012 (4)−0.040 (5)
F620.096 (7)0.077 (5)0.065 (4)0.016 (5)0.023 (3)−0.038 (3)
F630.071 (5)0.039 (3)0.084 (6)0.020 (3)0.012 (4)−0.015 (3)
F61'0.045 (7)0.082 (10)0.084 (10)0.027 (6)−0.025 (6)−0.048 (8)
F62'0.057 (9)0.052 (7)0.050 (7)0.007 (6)0.033 (5)−0.013 (5)
F63'0.061 (8)0.029 (6)0.066 (9)0.008 (5)0.001 (6)−0.021 (5)
F710.094 (8)0.079 (7)0.074 (7)0.056 (6)−0.040 (6)−0.052 (6)
F720.033 (3)0.061 (5)0.068 (6)0.009 (3)0.001 (4)0.000 (4)
F730.044 (6)0.048 (6)0.048 (5)−0.003 (4)−0.014 (3)0.007 (4)
F71'0.087 (7)0.050 (4)0.067 (6)0.030 (4)−0.036 (5)−0.033 (4)
F72'0.060 (5)0.068 (5)0.080 (7)0.038 (4)0.018 (5)0.007 (5)
F73'0.052 (7)0.049 (5)0.048 (4)0.008 (4)−0.027 (3)−0.015 (3)
F1610.070 (5)0.080 (7)0.084 (7)−0.031 (4)0.018 (5)−0.061 (6)
F1620.044 (3)0.052 (4)0.074 (6)−0.004 (3)−0.031 (3)−0.004 (3)
F1630.049 (5)0.046 (5)0.048 (4)−0.002 (4)−0.010 (3)0.009 (3)
F16'0.054 (5)0.042 (4)0.060 (6)−0.006 (3)0.005 (4)−0.027 (4)
F16"0.080 (7)0.058 (5)0.083 (8)−0.026 (5)−0.052 (7)0.003 (5)
F16*0.049 (7)0.049 (6)0.047 (5)−0.006 (4)0.016 (4)−0.022 (4)
F1710.046 (6)0.090 (10)0.094 (11)−0.011 (6)−0.009 (6)−0.053 (8)
F1720.067 (9)0.030 (6)0.073 (9)−0.003 (5)−0.029 (7)−0.022 (5)
F1730.082 (9)0.069 (8)0.056 (7)−0.011 (6)−0.054 (6)−0.003 (5)
F17'0.070 (4)0.080 (5)0.126 (7)0.011 (3)−0.064 (4)−0.046 (5)
F17"0.089 (6)0.041 (3)0.088 (6)−0.010 (3)−0.048 (5)−0.013 (3)
F17*0.126 (7)0.085 (4)0.062 (4)−0.007 (5)−0.049 (4)−0.040 (3)

Geometric parameters (Å, °)

K1—O32.711 (3)C5—C71.486 (5)
K1—O12.729 (3)C6—F62'1.319 (12)
K1—O22.738 (3)C6—F631.330 (8)
K1—O3i2.767 (3)C6—F611.336 (8)
K1—F16'2.923 (9)C6—F63'1.347 (12)
K1—F72i2.953 (8)C6—F621.351 (8)
K1—F1612.992 (10)C6—F61'1.382 (11)
K1—F17"ii2.998 (7)C7—F711.304 (8)
K1—F172ii3.004 (14)C7—F72'1.309 (8)
K1—F61'iii3.016 (11)C7—F731.321 (10)
K1—F72'i3.078 (14)C7—F73'1.336 (10)
K1—F61iii3.196 (14)C7—F71'1.401 (9)
K1—H2B3.08 (4)C7—F721.403 (9)
K1—H3A3.08 (4)N11—C151.347 (5)
K2—O4iv2.705 (3)N11—N121.359 (4)
K2—O12.739 (3)N12—C131.349 (5)
K2—O22.745 (3)C13—C141.391 (5)
K2—O42.754 (3)C13—C161.486 (5)
K2—F162i2.870 (7)C14—C151.388 (6)
K2—F16"i2.938 (13)C14—H140.9500
K2—F632.972 (8)C15—C171.487 (6)
K2—F63'2.978 (15)C16—F1611.312 (7)
K2—F171iii3.026 (12)C16—F16"1.319 (9)
K2—F71'ii3.075 (8)C16—F1631.325 (9)
K2—F71ii3.199 (13)C16—F16*1.326 (10)
K2—F17'iii3.215 (13)C16—F1621.383 (7)
K2—H1A3.05 (4)C16—F16'1.396 (8)
K2—H1B3.08 (4)C17—F1731.309 (12)
K2—H4A3.08 (4)C17—F17'1.323 (8)
O1—H1A0.817 (12)C17—F17"1.324 (8)
O1—H1B0.818 (12)C17—F1721.344 (12)
O2—H2A0.817 (12)C17—F17*1.360 (8)
O2—H2B0.813 (12)C17—F1711.401 (11)
O3—K1i2.767 (3)F61—K1iii3.196 (14)
O3—H3A0.818 (12)F61'—K1iii3.016 (11)
O3—H3B0.819 (12)F71—K2v3.199 (13)
O4—K2iv2.705 (3)F72—K1i2.953 (8)
O4—H4A0.816 (12)F71'—K2v3.075 (8)
O4—H4B0.817 (12)F72'—K1i3.078 (14)
N1—C51.348 (5)F162—K2i2.870 (7)
N1—N21.363 (4)F16"—K2i2.938 (13)
N2—C31.349 (5)F171—K2iii3.026 (12)
C3—C41.390 (6)F172—K1v3.004 (14)
C3—C61.480 (6)F17'—K2iii3.215 (13)
C4—C51.390 (5)F17"—K1v2.998 (7)
C4—H40.9500
O3—K1—O1120.18 (8)F71'ii—K2—F17'iii67.3 (4)
O3—K1—O279.20 (8)F71ii—K2—F17'iii78.5 (4)
O1—K1—O274.08 (8)O4iv—K2—H1A110.8 (7)
O3—K1—O3i73.56 (8)O1—K2—H1A15.0 (4)
O1—K1—O3i75.98 (7)O2—K2—H1A82.4 (7)
O2—K1—O3i120.62 (9)O4—K2—H1A60.0 (5)
O3—K1—F16'78.1 (2)F162i—K2—H1A90.6 (6)
O1—K1—F16'147.4 (2)F16"i—K2—H1A82.5 (6)
O2—K1—F16'138.4 (2)F63—K2—H1A148.9 (6)
O3i—K1—F16'85.3 (4)F63'—K2—H1A146.8 (7)
O3—K1—F72i135.5 (3)F171iii—K2—H1A135.2 (7)
O1—K1—F72i83.5 (4)F71'ii—K2—H1A82.8 (9)
O2—K1—F72i145.3 (3)F71ii—K2—H1A69.8 (9)
O3i—K1—F72i77.4 (3)F17'iii—K2—H1A142.1 (7)
F16'—K1—F72i66.4 (4)O4iv—K2—H1B134.5 (5)
O3—K1—F16168.8 (3)O1—K2—H1B14.7 (5)
O1—K1—F161142.8 (2)O2—K2—H1B81.1 (7)
O2—K1—F161140.27 (17)O4—K2—H1B80.8 (8)
O3i—K1—F16172.6 (4)F162i—K2—H1B65.2 (6)
F16'—K1—F16114.2 (2)F16"i—K2—H1B57.7 (8)
F72i—K1—F16170.7 (4)F63—K2—H1B128.9 (8)
O3—K1—F17"ii154.3 (3)F63'—K2—H1B123.7 (9)
O1—K1—F17"ii69.4 (3)F171iii—K2—H1B140.6 (8)
O2—K1—F17"ii81.3 (3)F71'ii—K2—H1B72.3 (7)
O3i—K1—F17"ii131.5 (2)F71ii—K2—H1B61.4 (7)
F16'—K1—F17"ii106.5 (5)F17'iii—K2—H1B139.6 (6)
F72i—K1—F17"ii66.0 (4)H1A—K2—H1B25.4 (8)
F161—K1—F17"ii119.6 (5)O4iv—K2—H4A81.5 (8)
O3—K1—F172ii157.4 (5)O1—K2—H4A60.5 (5)
O1—K1—F172ii74.9 (5)O2—K2—H4A110.9 (7)
O2—K1—F172ii90.2 (5)O4—K2—H4A14.8 (5)
O3i—K1—F172ii128.7 (5)F162i—K2—H4A125.7 (8)
F16'—K1—F172ii97.7 (6)F16"i—K2—H4A123.9 (7)
F72i—K1—F172ii58.1 (5)F63—K2—H4A163.1 (7)
F161—K1—F172ii110.5 (6)F63'—K2—H4A167.5 (7)
F17"ii—K1—F172ii9.5 (4)F171iii—K2—H4A93.4 (7)
O3—K1—F61'iii83.0 (6)F71'ii—K2—H4A79.4 (9)
O1—K1—F61'iii135.1 (3)F71ii—K2—H4A68.9 (9)
O2—K1—F61'iii73.7 (6)F17'iii—K2—H4A104.0 (6)
O3i—K1—F61'iii148.4 (3)H1A—K2—H4A45.5 (7)
F16'—K1—F61'iii69.2 (5)H1B—K2—H4A67.6 (9)
F72i—K1—F61'iii107.0 (8)K1—O1—K2106.24 (9)
F161—K1—F61'iii79.4 (5)K1—O1—H1A116 (3)
F17"ii—K1—F61'iii75.5 (6)K2—O1—H1A105 (3)
F172ii—K1—F61'iii74.8 (8)K1—O1—H1B110 (3)
O3—K1—F72'i136.4 (2)K2—O1—H1B107 (3)
O1—K1—F72'i71.0 (4)H1A—O1—H1B111 (4)
O2—K1—F72'i139.7 (2)K1—O2—K2105.85 (9)
O3i—K1—F72'i68.9 (4)K1—O2—H2A113 (3)
F16'—K1—F72'i77.5 (4)K2—O2—H2A110 (3)
F72i—K1—F72'i14.0 (2)K1—O2—H2B107 (3)
F161—K1—F72'i79.4 (3)K2—O2—H2B119 (3)
F17"ii—K1—F72'i68.2 (4)H2A—O2—H2B102 (4)
F172ii—K1—F72'i62.0 (6)K1—O3—K1i106.44 (8)
F61'iii—K1—F72'i120.2 (9)K1—O3—H3A110 (3)
O3—K1—F61iii92.7 (3)K1i—O3—H3A103 (3)
O1—K1—F61iii132.49 (19)K1—O3—H3B121 (3)
O2—K1—F61iii80.5 (2)K1i—O3—H3B108 (3)
O3i—K1—F61iii150.58 (15)H3A—O3—H3B108 (4)
F16'—K1—F61iii66.2 (4)K2iv—O4—K2105.09 (9)
F72i—K1—F61iii96.5 (5)K2iv—O4—H4A109 (3)
F161—K1—F61iii78.2 (4)K2—O4—H4A106 (3)
F17"ii—K1—F61iii67.5 (4)K2iv—O4—H4B116 (3)
F172ii—K1—F61iii65.6 (5)K2—O4—H4B110 (3)
F61'iii—K1—F61iii11.0 (5)H4A—O4—H4B111 (5)
F72'i—K1—F61iii109.4 (5)C5—N1—N2107.6 (3)
O3—K1—H2B83.5 (8)C3—N2—N1107.1 (3)
O1—K1—H2B83.4 (7)N2—C3—C4111.6 (3)
O2—K1—H2B14.6 (5)N2—C3—C6118.8 (4)
O3i—K1—H2B134.9 (5)C4—C3—C6129.6 (4)
F16'—K1—H2B127.6 (7)C5—C4—C3102.4 (3)
F72i—K1—H2B139.6 (8)C5—C4—H4128.8
F161—K1—H2B133.5 (8)C3—C4—H4128.8
F17"ii—K1—H2B73.7 (8)N1—C5—C4111.3 (3)
F172ii—K1—H2B81.7 (9)N1—C5—C7119.1 (3)
F61'iii—K1—H2B60.1 (7)C4—C5—C7129.6 (4)
F72'i—K1—H2B139.5 (8)F62'—C6—F63118.9 (12)
F61iii—K1—H2B66.2 (5)F62'—C6—F6182.4 (10)
O3—K1—H3A14.5 (5)F63—C6—F61107.1 (6)
O1—K1—H3A134.5 (5)F62'—C6—F63'105.6 (11)
O2—K1—H3A87.1 (7)F63—C6—F62106.9 (7)
O3i—K1—H3A79.2 (8)F61—C6—F62104.9 (6)
F16'—K1—H3A64.9 (6)F62'—C6—F61'104.8 (9)
F72i—K1—H3A127.0 (7)F63'—C6—F61'104.6 (10)
F161—K1—H3A57.1 (7)F62'—C6—C3116.1 (11)
F17"ii—K1—H3A148.8 (8)F63—C6—C3114.6 (6)
F172ii—K1—H3A147.5 (8)F61—C6—C3112.7 (5)
F61'iii—K1—H3A73.4 (9)F63'—C6—C3111.6 (12)
F72'i—K1—H3A132.1 (8)F62—C6—C3110.0 (6)
F61iii—K1—H3A82.1 (7)F61'—C6—C3113.1 (8)
H2B—K1—H3A88.1 (11)F71—C7—F73111.2 (9)
O4iv—K2—O1119.89 (9)F72'—C7—F73'110.1 (8)
O4iv—K2—O279.81 (8)F72'—C7—F71'104.3 (7)
O1—K2—O273.82 (8)F73'—C7—F71'101.9 (7)
O4iv—K2—O474.91 (9)F71—C7—F72104.5 (7)
O1—K2—O474.86 (8)F73—C7—F72103.4 (7)
O2—K2—O4121.46 (9)F71—C7—C5115.6 (5)
O4iv—K2—F162i152.75 (19)F72'—C7—C5115.0 (5)
O1—K2—F162i78.0 (2)F73—C7—C5111.8 (9)
O2—K2—F162i86.8 (3)F73'—C7—C5114.7 (8)
O4—K2—F162i132.0 (2)F71'—C7—C5109.6 (5)
O4iv—K2—F16"i148.2 (3)F72—C7—C5109.3 (6)
O1—K2—F16"i68.5 (4)C15—N11—N12107.1 (3)
O2—K2—F16"i73.4 (5)C13—N12—N11107.4 (3)
O4—K2—F16"i134.2 (2)N12—C13—C14111.5 (3)
F162i—K2—F16"i14.9 (3)N12—C13—C16119.3 (3)
O4iv—K2—F6382.9 (4)C14—C13—C16129.2 (3)
O1—K2—F63134.4 (2)C15—C14—C13102.1 (3)
O2—K2—F6372.5 (3)C15—C14—H14129.0
O4—K2—F63150.2 (3)C13—C14—H14129.0
F162i—K2—F6370.4 (4)N11—C15—C14111.9 (3)
F16"i—K2—F6373.0 (4)N11—C15—C17118.3 (4)
O4iv—K2—F63'91.8 (6)C14—C15—C17129.8 (4)
O1—K2—F63'131.8 (6)F161—C16—F16"74.0 (7)
O2—K2—F63'78.0 (5)F161—C16—F163109.9 (8)
O4—K2—F63'152.7 (5)F161—C16—F16*120.8 (10)
F162i—K2—F63'62.0 (6)F16"—C16—F16*110.0 (8)
F16"i—K2—F63'66.3 (7)F161—C16—F162104.9 (6)
F63—K2—F63'9.8 (4)F163—C16—F162103.5 (6)
O4iv—K2—F171iii70.5 (5)F16"—C16—F16'103.7 (7)
O1—K2—F171iii147.0 (3)F16*—C16—F16'101.1 (7)
O2—K2—F171iii138.2 (3)F161—C16—C13114.8 (5)
O4—K2—F171iii78.8 (6)F16"—C16—C13115.6 (5)
F162i—K2—F171iii106.5 (7)F163—C16—C13112.7 (7)
F16"i—K2—F171iii120.8 (9)F16*—C16—C13114.9 (9)
F63—K2—F171iii75.2 (5)F162—C16—C13110.3 (5)
F63'—K2—F171iii74.3 (7)F16'—C16—C13110.0 (5)
O4iv—K2—F71'ii135.0 (2)F17'—C17—F17"107.7 (6)
O1—K2—F71'ii84.2 (4)F173—C17—F172106.8 (12)
O2—K2—F71'ii145.2 (2)F17'—C17—F17*104.7 (6)
O4—K2—F71'ii76.3 (2)F17"—C17—F17*107.3 (7)
F162i—K2—F71'ii62.0 (3)F173—C17—F171103.8 (9)
F16"i—K2—F71'ii73.6 (4)F172—C17—F171103.0 (9)
F63—K2—F71'ii107.6 (5)F173—C17—C15118.0 (9)
F63'—K2—F71'ii98.4 (6)F17'—C17—C15112.7 (5)
F171iii—K2—F71'ii70.4 (5)F17"—C17—C15114.7 (6)
O4iv—K2—F71ii136.31 (19)F172—C17—C15111.1 (11)
O1—K2—F71ii72.3 (4)F17*—C17—C15109.0 (6)
O2—K2—F71ii140.0 (2)F171—C17—C15112.9 (8)
O4—K2—F71ii68.3 (3)C6—F61—K1iii139.0 (9)
F162i—K2—F71ii66.0 (4)C6—F63—K2152.7 (9)
F16"i—K2—F71ii75.0 (4)C6—F61'—K1iii153.2 (11)
F63—K2—F71ii119.9 (6)C6—F63'—K2149.8 (16)
F63'—K2—F71ii110.4 (7)C7—F71—K2v144.1 (11)
F171iii—K2—F71ii79.7 (5)C7—F72—K1i147.6 (8)
F71'ii—K2—F71ii13.2 (2)C7—F71'—K2v147.7 (7)
O4iv—K2—F17'iii78.53 (18)C7—F72'—K1i143.7 (12)
O1—K2—F17'iii150.29 (16)C16—F161—K1146.9 (10)
O2—K2—F17'iii135.21 (19)C16—F162—K2i146.9 (8)
O4—K2—F17'iii89.6 (3)C16—F16'—K1145.8 (8)
F162i—K2—F17'iii95.1 (4)C16—F16"—K2i145.9 (13)
F16"i—K2—F17'iii109.1 (6)C17—F171—K2iii151.7 (11)
F63—K2—F17'iii66.3 (4)C17—F172—K1v151.2 (16)
F63'—K2—F17'iii64.1 (6)C17—F17'—K2iii139.8 (8)
F171iii—K2—F17'iii12.2 (5)C17—F17"—K1v154.6 (8)
O3—K1—O1—K2−66.68 (11)F61'—C6—F61—K1iii40 (2)
O2—K1—O1—K20.29 (9)C3—C6—F61—K1iii−56.9 (15)
O3i—K1—O1—K2−127.82 (10)F62'—C6—F63—K2119 (3)
F16'—K1—O1—K2175.4 (6)F61—C6—F63—K2−151 (3)
F72i—K1—O1—K2153.5 (2)F63'—C6—F63—K262 (4)
F161—K1—O1—K2−160.9 (7)F62—C6—F63—K297 (3)
F17"ii—K1—O1—K286.8 (3)F61'—C6—F63—K2−138 (3)
F172ii—K1—O1—K294.9 (5)C3—C6—F63—K2−25 (3)
F61'iii—K1—O1—K245.9 (10)O4iv—K2—F63—C6143 (3)
F72'i—K1—O1—K2160.0 (4)O1—K2—F63—C618 (3)
F61iii—K1—O1—K260.8 (4)O2—K2—F63—C662 (3)
O4iv—K2—O1—K1−68.00 (11)O4—K2—F63—C6−175 (2)
O2—K2—O1—K1−0.29 (9)F162i—K2—F63—C6−31 (3)
O4—K2—O1—K1−130.19 (10)F16"i—K2—F63—C6−16 (3)
F162i—K2—O1—K189.8 (3)F63'—K2—F63—C6−61 (4)
F16"i—K2—O1—K177.8 (4)F171iii—K2—F63—C6−145 (3)
F63—K2—O1—K143.4 (6)F71'ii—K2—F63—C6−82 (3)
F63'—K2—O1—K156.3 (7)F71ii—K2—F63—C6−76 (3)
F171iii—K2—O1—K1−168.3 (12)F17'iii—K2—F63—C6−136 (3)
F71'ii—K2—O1—K1152.4 (2)F62'—C6—F61'—K1iii−113 (5)
F71ii—K2—O1—K1158.2 (3)F63—C6—F61'—K1iii128 (5)
F17'iii—K2—O1—K1169.0 (5)F61—C6—F61'—K1iii−81 (5)
O3—K1—O2—K2125.63 (10)F63'—C6—F61'—K1iii136 (5)
O1—K1—O2—K2−0.29 (9)F62—C6—F61'—K1iii−125 (5)
O3i—K1—O2—K262.23 (12)C3—C6—F61'—K1iii14 (5)
F16'—K1—O2—K2−176.3 (5)F62'—C6—F63'—K2176 (4)
F72i—K1—O2—K2−52.0 (7)F63—C6—F63'—K2−54 (3)
F161—K1—O2—K2162.0 (7)F61—C6—F63'—K2−93 (4)
F17"ii—K1—O2—K2−71.3 (3)F62—C6—F63'—K2160 (4)
F172ii—K1—O2—K2−74.5 (5)F61'—C6—F63'—K2−74 (4)
F61'iii—K1—O2—K2−148.6 (6)C3—C6—F63'—K249 (4)
F72'i—K1—O2—K2−30.8 (7)O4iv—K2—F63'—C676 (4)
F61iii—K1—O2—K2−139.7 (3)O1—K2—F63'—C6−58 (4)
O4iv—K2—O2—K1125.69 (10)O2—K2—F63'—C6−3(4)
O1—K2—O2—K10.29 (9)O4—K2—F63'—C6136 (3)
O4—K2—O2—K160.53 (12)F162i—K2—F63'—C6−95 (4)
F162i—K2—O2—K1−78.2 (2)F16"i—K2—F63'—C6−80 (4)
F16"i—K2—O2—K1−71.6 (4)F63—K2—F63'—C652 (3)
F63—K2—O2—K1−148.6 (4)F171iii—K2—F63'—C6146 (4)
F63'—K2—O2—K1−140.2 (6)F71'ii—K2—F63'—C6−148 (4)
F171iii—K2—O2—K1170.5 (10)F71ii—K2—F63'—C6−142 (3)
F71'ii—K2—O2—K1−52.8 (6)F17'iii—K2—F63'—C6153 (4)
F71ii—K2—O2—K1−32.7 (7)F72'—C7—F71—K2v−150 (3)
F17'iii—K2—O2—K1−172.2 (3)F73—C7—F71—K2v90 (2)
O1—K1—O3—K1i−62.37 (11)F73'—C7—F71—K2v106 (2)
O2—K1—O3—K1i−126.65 (10)F71'—C7—F71—K2v46.7 (18)
O3i—K1—O3—K1i0.0F72—C7—F71—K2v−159 (2)
F16'—K1—O3—K1i88.5 (3)C5—C7—F71—K2v−39 (3)
F72i—K1—O3—K1i51.4 (5)F71—C7—F72—K1i73 (2)
F161—K1—O3—K1i77.3 (4)F72'—C7—F72—K1i55.2 (18)
F17"ii—K1—O3—K1i−168.1 (7)F73—C7—F72—K1i−171 (2)
F172ii—K1—O3—K1i169.9 (13)F73'—C7—F72—K1i−166 (2)
F61'iii—K1—O3—K1i158.6 (5)F71'—C7—F72—K1i90 (2)
F72'i—K1—O3—K1i31.3 (7)C5—C7—F72—K1i−51 (2)
F61iii—K1—O3—K1i153.52 (18)F71—C7—F71'—K2v−56.2 (17)
O4iv—K2—O4—K2iv0.0F72'—C7—F71'—K2v−72 (2)
O1—K2—O4—K2iv127.42 (11)F73—C7—F71'—K2v164 (2)
O2—K2—O4—K2iv67.68 (11)F73'—C7—F71'—K2v173 (2)
F162i—K2—O4—K2iv−174.8 (4)F72—C7—F71'—K2v−91 (2)
F16"i—K2—O4—K2iv165.0 (7)C5—C7—F71'—K2v51 (2)
F63—K2—O4—K2iv−43.3 (8)F71—C7—F72'—K1i152 (3)
F63'—K2—O4—K2iv−63.2 (12)F73—C7—F72'—K1i−102 (2)
F171iii—K2—O4—K2iv−72.7 (5)F73'—C7—F72'—K1i−91 (2)
F71'ii—K2—O4—K2iv−145.0 (4)F71'—C7—F72'—K1i161 (2)
F71ii—K2—O4—K2iv−156.0 (4)F72—C7—F72'—K1i−45.6 (19)
F17'iii—K2—O4—K2iv−78.21 (16)C5—C7—F72'—K1i41 (3)
C5—N1—N2—C3−0.2 (4)F16"—C16—F161—K1−150 (3)
N1—N2—C3—C40.7 (4)F163—C16—F161—K189 (2)
N1—N2—C3—C6−179.3 (3)F16*—C16—F161—K1106 (2)
N2—C3—C4—C5−0.9 (4)F162—C16—F161—K1−160 (2)
C6—C3—C4—C5179.1 (4)F16'—C16—F161—K149 (2)
N2—N1—C5—C4−0.4 (4)C13—C16—F161—K1−39 (3)
N2—N1—C5—C7179.5 (3)O3—K1—F161—C1679 (2)
C3—C4—C5—N10.8 (4)O1—K1—F161—C16−168.4 (17)
C3—C4—C5—C7−179.2 (4)O2—K1—F161—C1641 (3)
N2—C3—C6—F62'166.4 (16)O3i—K1—F161—C16158 (2)
C4—C3—C6—F62'−13.6 (17)F16'—K1—F161—C16−50.1 (19)
N2—C3—C6—F63−49.0 (12)F72i—K1—F161—C16−120 (2)
C4—C3—C6—F63131.0 (11)F17"ii—K1—F161—C16−74 (2)
N2—C3—C6—F6173.8 (10)F172ii—K1—F161—C16−77 (2)
C4—C3—C6—F61−106.2 (11)F61'iii—K1—F161—C16−7(2)
N2—C3—C6—F63'−72.5 (15)F72'i—K1—F161—C16−131 (2)
C4—C3—C6—F63'107.5 (14)F61iii—K1—F161—C16−18 (2)
N2—C3—C6—F62−169.4 (10)F161—C16—F162—K2i67 (2)
C4—C3—C6—F6210.6 (11)F16"—C16—F162—K2i48.6 (15)
N2—C3—C6—F61'45.1 (18)F163—C16—F162—K2i−178.1 (18)
C4—C3—C6—F61'−134.9 (18)F16*—C16—F162—K2i−172.5 (16)
N1—C5—C7—F71−37.7 (14)F16'—C16—F162—K2i86.4 (18)
C4—C5—C7—F71142.3 (14)C13—C16—F162—K2i−57.4 (17)
N1—C5—C7—F72'46.2 (14)F161—C16—F16'—K1−49.2 (15)
C4—C5—C7—F72'−133.9 (14)F16"—C16—F16'—K1−68 (2)
N1—C5—C7—F73−166.2 (10)F163—C16—F16'—K1168.2 (18)
C4—C5—C7—F7313.7 (11)F16*—C16—F16'—K1178 (2)
N1—C5—C7—F73'175.3 (9)F162—C16—F16'—K1−88.0 (19)
C4—C5—C7—F73'−4.7 (10)C13—C16—F16'—K155.9 (19)
N1—C5—C7—F71'−70.8 (9)O3—K1—F16'—C16−2.9 (16)
C4—C5—C7—F71'109.1 (9)O1—K1—F16'—C16125.8 (13)
N1—C5—C7—F7279.8 (9)O2—K1—F16'—C16−61 (2)
C4—C5—C7—F72−100.2 (10)O3i—K1—F16'—C1671.3 (17)
C15—N11—N12—C13−0.1 (4)F72i—K1—F16'—C16149.6 (19)
N11—N12—C13—C14−0.4 (4)F161—K1—F16'—C1644.6 (13)
N11—N12—C13—C16179.1 (3)F17"ii—K1—F16'—C16−156.8 (17)
N12—C13—C14—C150.7 (4)F172ii—K1—F16'—C16−160.3 (18)
C16—C13—C14—C15−178.7 (4)F61'iii—K1—F16'—C16−89.8 (18)
N12—N11—C15—C140.6 (4)F72'i—K1—F16'—C16140.7 (18)
N12—N11—C15—C17−178.8 (3)F61iii—K1—F16'—C16−101.3 (17)
C13—C14—C15—N11−0.8 (4)F161—C16—F16"—K2i153 (3)
C13—C14—C15—C17178.5 (4)F163—C16—F16"—K2i−104 (2)
N12—C13—C16—F161−40.9 (13)F16*—C16—F16"—K2i−90 (2)
C14—C13—C16—F161138.5 (12)F162—C16—F16"—K2i−46 (2)
N12—C13—C16—F16"42.5 (15)F16'—C16—F16"—K2i163 (2)
C14—C13—C16—F16"−138.1 (15)C13—C16—F16"—K2i42 (3)
N12—C13—C16—F163−167.7 (8)F173—C17—F171—K2iii−104 (4)
C14—C13—C16—F16311.8 (9)F17'—C17—F171—K2iii−71 (4)
N12—C13—C16—F16*172.3 (9)F17"—C17—F171—K2iii139 (4)
C14—C13—C16—F16*−8.2 (11)F172—C17—F171—K2iii145 (4)
N12—C13—C16—F16277.3 (8)F17*—C17—F171—K2iii−115 (4)
C14—C13—C16—F162−103.3 (8)C15—C17—F171—K2iii25 (5)
N12—C13—C16—F16'−74.5 (9)F173—C17—F172—K1v−177 (3)
C14—C13—C16—F16'105.0 (9)F17'—C17—F172—K1v−89 (4)
N11—C15—C17—F173165.3 (15)F17"—C17—F172—K1v−51 (3)
C14—C15—C17—F173−14.0 (16)F17*—C17—F172—K1v163 (3)
N11—C15—C17—F17'75.8 (9)F171—C17—F172—K1v−68 (4)
C14—C15—C17—F17'−103.5 (9)C15—C17—F172—K1v53 (3)
N11—C15—C17—F17"−48.0 (10)F173—C17—F17'—K2iii−171.6 (16)
C14—C15—C17—F17"132.7 (9)F17"—C17—F17'—K2iii71.9 (14)
N11—C15—C17—F172−70.9 (13)F172—C17—F17'—K2iii85.4 (18)
C14—C15—C17—F172109.8 (13)F17*—C17—F17'—K2iii−174.0 (10)
N11—C15—C17—F17*−168.3 (8)F171—C17—F17'—K2iii40.8 (17)
C14—C15—C17—F17*12.3 (9)C15—C17—F17'—K2iii−55.7 (14)
N11—C15—C17—F17144.2 (16)F173—C17—F17"—K1v123 (3)
C14—C15—C17—F171−135.2 (16)F17'—C17—F17"—K1v−150 (2)
F62'—C6—F61—K1iii−172.1 (17)F172—C17—F17"—K1v62 (4)
F63—C6—F61—K1iii70.0 (16)F17*—C17—F17"—K1v98 (3)
F63'—C6—F61—K1iii84.2 (19)F171—C17—F17"—K1v−135 (3)
F62—C6—F61—K1iii−176.6 (12)C15—C17—F17"—K1v−23 (3)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1—H1A···N11ii0.82 (2)2.10 (2)2.906 (4)167 (4)
O1—H1B···N12i0.82 (2)2.09 (2)2.896 (4)168 (4)
O2—H2A···N20.82 (2)2.12 (1)2.929 (4)173 (5)
O2—H2B···N2iii0.81 (2)2.07 (1)2.879 (4)173 (5)
O3—H3A···N120.82 (2)2.05 (1)2.868 (4)173 (4)
O3—H3B···N10.82 (2)2.09 (1)2.910 (4)177 (4)
O4—H4A···N11ii0.82 (2)2.08 (1)2.891 (4)175 (4)
O4—H4B···N1ii0.82 (2)2.07 (1)2.884 (4)174 (4)

Symmetry codes: (ii) x, y+1, z; (i) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV2744).

References

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  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
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  • Stoe & Cie (2001). X-AREA Stoe & Cie, Darmstadt, Germany.

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