Acta Cryst. (2007). E63, i170 [ doi:10.1107/S1600536807027195 ]
The title compound, poly[![[mu]](/logos/entities/mu_rmgif.gif)
-difluoridooxidonitrato-potassium], [KNOF2]n, crystallizes in the orthorhombic system and adopts the ordered KNO3 structure type. A crystallographic mirror plane passes through N, O and K. In the crystal structure, the polymer chains are linked by weak bonds into an infinite three-dimensional framework.
Crystals of the title compound were synthesized using solid-state reaction method. KF (58 mg, 1 mmol), NaNO3 (170 mg, 2 mmol), corresponding to a molar ratio of 1:2, were heated in a graphite crucible under a static atmosphere of a (98/2)% mixture of N2/H2 up to 1173 K over the course of 6 h. This temperature was held for 2 h and then decreased to 773 K within 20 h. After cooling to room temperature, the solidified melt was leached with demineralized water. From the remaining residue, colourless plates of KNOF2 could be isolated.
Data collection: APEX2 (Bruker, YEAR?); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL.
![[Figure 1]](./hk2267fig1thm.gif)
| Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level [symmetry code (A): -x + 1, -y + 1, -z + 1; (C): -x + 1, -y + 2, -z + 1; (E): x, -y + 3/2, z; (G): -x + 3/2, -y + 2, z + 1/2]. |
![[Figure 2]](./hk2267fig2thm.gif)
| Fig. 2. A packing diagram for (I). |
| KNOF2 | F(000) = 208 |
| Mr = 107.11 | Dx = 2.229 Mg m−3 |
| Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2ac 2n | Cell parameters from 1198 reflections |
| a = 6.429 (4) Å | θ = 4.4–28.3° |
| b = 5.417 (3) Å | µ = 1.51 mm−1 |
| c = 9.164 (5) Å | T = 273 K |
| V = 319.1 (3) Å3 | Block, colourless |
| Z = 4 | 0.27 × 0.10 × 0.06 mm |
| Bruker APEXII area-detector diffractometer | 372 independent reflections |
| Radiation source: fine-focus sealed tube | 304 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.018 |
| φ and ω scans | θmax = 27.0°, θmin = 3.9° |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→8 |
| Tmin = 0.686, Tmax = 0.915 | k = −6→6 |
| 2043 measured reflections | l = −11→11 |
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.039 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.163 | w = 1/[σ2(Fo2) + (0.128P)2 + 0.1109P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.06 | (Δ/σ)max < 0.001 |
| 372 reflections | Δρmax = 0.37 e Å−3 |
| 28 parameters | Δρmin = −0.55 e Å−3 |
| KNOF2 | V = 319.1 (3) Å3 |
| Mr = 107.11 | Z = 4 |
| Orthorhombic, Pnma | Mo Kα radiation |
| a = 6.429 (4) Å | µ = 1.51 mm−1 |
| b = 5.417 (3) Å | T = 273 K |
| c = 9.164 (5) Å | 0.27 × 0.10 × 0.06 mm |
| Bruker APEXII area-detector diffractometer | 372 independent reflections |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 304 reflections with I > 2σ(I) |
| Tmin = 0.686, Tmax = 0.915 | Rint = 0.018 |
| 2043 measured reflections | θmax = 27.0° |
| R[F2 > 2σ(F2)] = 0.039 | Δρmax = 0.37 e Å−3 |
| wR(F2) = 0.163 | Δρmin = −0.55 e Å−3 |
| S = 1.06 | Absolute structure: ? |
| 372 reflections | Flack parameter: ? |
| 28 parameters | Rogers parameter: ? |
| 0 restraints |
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. |
| x | y | z | Uiso*/Ueq | ||
| K1 | 0.75494 (11) | 0.7500 | 0.58346 (8) | 0.0285 (5) | |
| O1 | 0.4098 (5) | 0.7500 | 0.3901 (3) | 0.0392 (8) | |
| N1 | 0.4145 (5) | 0.7500 | 0.2554 (3) | 0.0244 (8) | |
| F1 | 0.4144 (3) | 0.9496 (4) | 0.1866 (2) | 0.0554 (8) |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| K1 | 0.0334 (8) | 0.0254 (8) | 0.0267 (7) | 0.000 | −0.0009 (3) | 0.000 |
| O1 | 0.051 (2) | 0.0380 (19) | 0.0285 (14) | 0.000 | −0.0061 (13) | 0.000 |
| N1 | 0.0198 (17) | 0.0232 (16) | 0.0303 (16) | 0.000 | 0.0008 (12) | 0.000 |
| F1 | 0.0757 (17) | 0.0402 (13) | 0.0502 (13) | −0.0044 (10) | 0.0045 (11) | 0.0050 (8) |
| K1—O1 | 2.840 (3) | K1—N1ii | 3.272 (2) |
| O1—N1 | 1.235 (4) | K1—N1iv | 3.272 (2) |
| N1—F1 | 1.251 (3) | O1—K1iv | 2.9185 (18) |
| K1—F1i | 2.839 (2) | O1—K1ii | 2.9185 (18) |
| K1—F1ii | 2.876 (2) | N1—F1viii | 1.251 (3) |
| K1—F1iii | 2.889 (2) | N1—K1ix | 3.270 (4) |
| K1—O1iv | 2.9185 (18) | N1—K1ii | 3.272 (2) |
| K1—F1v | 2.839 (2) | N1—K1iv | 3.272 (2) |
| K1—F1vi | 2.876 (2) | F1—K1x | 2.839 (2) |
| K1—F1vii | 2.889 (2) | F1—K1ii | 2.876 (2) |
| K1—O1ii | 2.9185 (18) | F1—K1ix | 2.889 (2) |
| K1—N1vii | 3.270 (4) | ||
| F1i—K1—O1 | 142.45 (5) | O1—K1—N1ii | 91.24 (7) |
| O1—K1—F1ii | 99.29 (8) | F1ii—K1—N1ii | 22.32 (7) |
| F1i—K1—F1v | 69.95 (10) | F1vi—K1—N1ii | 90.68 (8) |
| F1v—K1—O1 | 142.45 (5) | F1iii—K1—N1ii | 144.56 (7) |
| F1i—K1—F1ii | 73.45 (6) | F1vii—K1—N1ii | 101.25 (7) |
| F1v—K1—F1ii | 111.33 (6) | O1iv—K1—N1ii | 127.59 (8) |
| F1i—K1—F1vi | 111.33 (6) | O1ii—K1—N1ii | 22.07 (8) |
| F1v—K1—F1vi | 73.45 (6) | N1vii—K1—N1ii | 122.21 (6) |
| O1—K1—F1vi | 99.29 (8) | F1i—K1—N1iv | 124.99 (8) |
| F1ii—K1—F1vi | 68.92 (10) | F1v—K1—N1iv | 67.94 (7) |
| F1i—K1—F1iii | 103.54 (5) | O1—K1—N1iv | 91.24 (7) |
| F1v—K1—F1iii | 78.76 (7) | F1ii—K1—N1iv | 90.68 (8) |
| O1—K1—F1iii | 75.08 (8) | F1vi—K1—N1iv | 22.32 (7) |
| F1ii—K1—F1iii | 166.82 (9) | F1iii—K1—N1iv | 101.25 (7) |
| F1vi—K1—F1iii | 123.38 (4) | F1vii—K1—N1iv | 144.56 (7) |
| F1i—K1—F1vii | 78.76 (7) | O1iv—K1—N1iv | 22.07 (8) |
| F1v—K1—F1vii | 103.54 (5) | O1ii—K1—N1iv | 127.59 (8) |
| O1—K1—F1vii | 75.08 (8) | N1vii—K1—N1iv | 122.21 (6) |
| F1ii—K1—F1vii | 123.38 (4) | N1ii—K1—N1iv | 111.77 (10) |
| F1vi—K1—F1vii | 166.82 (9) | N1—O1—K1 | 127.2 (2) |
| F1iii—K1—F1vii | 43.96 (10) | N1—O1—K1iv | 95.27 (9) |
| F1i—K1—O1iv | 140.90 (7) | K1—O1—K1iv | 103.40 (6) |
| F1v—K1—O1iv | 73.27 (8) | N1—O1—K1ii | 95.27 (9) |
| O1—K1—O1iv | 76.60 (6) | K1—O1—K1ii | 103.40 (6) |
| F1ii—K1—O1iv | 109.08 (8) | K1iv—O1—K1ii | 136.28 (12) |
| F1vi—K1—O1iv | 43.67 (8) | O1—N1—F1viii | 120.23 (17) |
| F1iii—K1—O1iv | 81.53 (8) | O1—N1—F1 | 120.23 (17) |
| F1vii—K1—O1iv | 123.18 (7) | F1viii—N1—F1 | 119.5 (3) |
| F1i—K1—O1ii | 73.27 (8) | O1—N1—K1ix | 160.3 (2) |
| F1v—K1—O1ii | 140.90 (7) | F1viii—N1—K1ix | 61.43 (17) |
| O1—K1—O1ii | 76.60 (6) | F1—N1—K1ix | 61.43 (17) |
| F1ii—K1—O1ii | 43.67 (8) | O1—N1—K1ii | 62.66 (9) |
| F1vi—K1—O1ii | 109.08 (8) | F1viii—N1—K1ii | 160.5 (2) |
| F1iii—K1—O1ii | 123.18 (7) | F1—N1—K1ii | 60.79 (13) |
| F1vii—K1—O1ii | 81.53 (8) | K1ix—N1—K1ii | 108.92 (7) |
| O1iv—K1—O1ii | 136.28 (12) | O1—N1—K1iv | 62.66 (9) |
| F1i—K1—N1vii | 94.67 (7) | F1viii—N1—K1iv | 60.79 (13) |
| F1v—K1—N1vii | 94.67 (7) | F1—N1—K1iv | 160.5 (2) |
| O1—K1—N1vii | 69.66 (9) | K1ix—N1—K1iv | 108.92 (7) |
| F1ii—K1—N1vii | 144.52 (5) | K1ii—N1—K1iv | 111.77 (10) |
| F1vi—K1—N1vii | 144.52 (5) | N1—F1—K1x | 131.51 (18) |
| F1iii—K1—N1vii | 22.36 (5) | N1—F1—K1ii | 96.89 (17) |
| F1vii—K1—N1vii | 22.36 (5) | K1x—F1—K1ii | 101.71 (7) |
| O1iv—K1—N1vii | 101.11 (6) | N1—F1—K1ix | 96.21 (18) |
| O1ii—K1—N1vii | 101.11 (6) | K1x—F1—K1ix | 101.24 (7) |
| F1i—K1—N1ii | 67.94 (7) | K1ii—F1—K1ix | 134.83 (8) |
| F1v—K1—N1ii | 124.99 (8) |
| Symmetry codes: (i) −x+3/2, −y+2, z+1/2; (ii) −x+1, −y+2, −z+1; (iii) x+1/2, −y+3/2, −z+1/2; (iv) −x+1, −y+1, −z+1; (v) −x+3/2, y−1/2, z+1/2; (vi) −x+1, y−1/2, −z+1; (vii) x+1/2, y, −z+1/2; (viii) x, −y+3/2, z; (ix) x−1/2, y, −z+1/2; (x) −x+3/2, −y+2, z−1/2. |
| K1—O1 | 2.840 (3) | K1—F1ii | 2.876 (2) |
| O1—N1 | 1.235 (4) | K1—F1iii | 2.889 (2) |
| N1—F1 | 1.251 (3) | K1—O1iv | 2.9185 (18) |
| K1—F1i | 2.839 (2) | ||
| F1i—K1—O1 | 142.45 (5) | O1—K1—F1ii | 99.29 (8) |
| Symmetry codes: (i) −x+3/2, −y+2, z+1/2; (ii) −x+1, −y+2, −z+1; (iii) x+1/2, −y+3/2, −z+1/2; (iv) −x+1, −y+1, −z+1. |
The authors thank the Youth Programme of Jinggangshan University for financial support of this work.
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Inorganic compounds with various anions attract attention because of the features of their crystal chemistry (Berdonosov et al., 2000; Ruck & Schmidt, 2003; Lipp & Schleid, 2005; Ben Hamida & Wickleder, 2005).The first probable crystallographic path in single crystals of KNO3 was reported by Swaminathan et al. in 1975. In the following years, the compounds KNO3 were synthesized and characterized by Nimmo & Lucas (1976), Soltzberg et al. (1994) and Christensen et al. (1996). We herein report the crystal structure of the title compound, (I).
In the molecule of (I), the bond lengths and angles (Table 1) are within normal ranges. One of F atoms in KNOF2 (Fig. 1) is symmetry related with symmetry code (x, -y + 3/2, z). KNOF2 crystallizes in the orthorhombic system and adopts the ordered KNO3 structure type. The [KNOF2]n structure is a coordination network polymer, in which K+ cations are connected by the anions coordinated through F and O atoms.