Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807027195/hk2267sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807027195/hk2267Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (O-N) = 0.004 Å
- R factor = 0.039
- wR factor = 0.163
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
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.
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.
For related literature, see: Ben Hamida & Wickleder (2005); Berdonosov et al. (2000); Christensen et al. (1996); Lipp & Schleid (2005); Nimmo & Lucas (1976); Ruck & Schmidt (2003); Soltzberg et al. (1994); Swaminathan & Srinivasan (1975).
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.
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 |
R[F2 > 2σ(F2)] = 0.039 | 28 parameters |
wR(F2) = 0.163 | 0 restraints |
S = 1.06 | Δρmax = 0.37 e Å−3 |
372 reflections | Δρmin = −0.55 e Å−3 |
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. |
Experimental details
Crystal data | |
Chemical formula | KNOF2 |
Mr | 107.11 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 273 |
a, b, c (Å) | 6.429 (4), 5.417 (3), 9.164 (5) |
V (Å3) | 319.1 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.51 |
Crystal size (mm) | 0.27 × 0.10 × 0.06 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.686, 0.915 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2043, 372, 304 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.638 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.163, 1.06 |
No. of reflections | 372 |
No. of parameters | 28 |
Δρmax, Δρmin (e Å−3) | 0.37, −0.55 |
Computer programs: APEX2 (Bruker, YEAR?), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996), SHELXTL.
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. |
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.