The structure of potassium dinitramide (KDN), KN3O4, has been refined in the temperature range 85–298 K from single-crystal X-ray diffraction data. The unit-cell axial lengths and the cell volume decrease linearly on cooling with the b axis being the most sensitive to the change of temperature. The β cell angle increases with decreasing temperature. The thermal expansion of KDN is significantly anisotropic, expanding along the b axis [010] more than three times the amount parallel to any other crystallographic direction. Other eigenvectors of the thermal expansion tensor lie approximately parallel to the diagonals of the ac plane. A rigid-body analysis of the dinitramide ion using the TLS formalism was performed and shows that the thermal motion of the anion is well represented by the rigid-body model. The eigenvalues of the libration tensor show significant anisotropy, whereas the translation tensor is close to isotropic. The variation of all descriptions of the thermal motion with respect to temperature indicates an anharmonic contribution to the mean field potential. The direction of greatest unit-cell expansion coincides with the largest components of the displacement tensor of the potassium ions and the direction of the largest atomic amplitudes due to the libration of the dinitramide anions.
Supporting information
For all compounds, data collection: Siemens SMART; cell refinement: Siemens SAINT; data reduction: Siemens SAINT; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: Siemens SHELXTL; software used to prepare material for publication: Siemens SHELXTL and the Toledo cifomatic.
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.280 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.5891 (4) Å | Cell parameters from 2897 reflections |
| b = 9.0653 (5) Å | θ = 6.4–24.4° |
| c = 7.1459 (4) Å | µ = 1.17 mm−1 |
| β = 97.975 (2)° | T = 85 K |
| V = 422.71 (4) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1034 independent reflections |
| Radiation source: Sealed Tube | 902 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.048 |
| ω scans | θmax = 28.3°, θmin = 3.7° |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | h = −8→7 |
| Tmin = 0.791, Tmax = 0.990 | k = −12→12 |
| 3515 measured reflections | l = −8→9 |
Refinement top
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.031 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.075 | Calculated w = 1/[σ2(Fo2) + (0.0423P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.02 | (Δ/σ)max < 0.001 |
| 1034 reflections | Δρmax = 0.55 e Å−3 |
| 73 parameters | Δρmin = −0.60 e Å−3 |
Crystal data top
| KN3O4 | V = 422.71 (4) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.5891 (4) Å | µ = 1.17 mm−1 |
| b = 9.0653 (5) Å | T = 85 K |
| c = 7.1459 (4) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.975 (2)° | |
Data collection top
Platform
diffractometer | 1034 independent reflections |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | 902 reflections with I > 2σ(I) |
| Tmin = 0.791, Tmax = 0.990 | Rint = 0.048 |
| 3515 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.031 | 73 parameters |
| wR(F2) = 0.075 | 0 restraints |
| S = 1.02 | Δρmax = 0.55 e Å−3 |
| 1034 reflections | Δρmin = −0.60 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.86050 (5) | 0.34347 (3) | 0.83221 (4) | 0.01092 (13) | |
| O4 | 1.0107 (2) | 0.34344 (12) | 1.2155 (2) | 0.0126 (3) | |
| O2 | 0.7261 (2) | 0.53857 (12) | 1.1548 (2) | 0.0141 (3) | |
| N2 | 0.6489 (2) | 0.46229 (13) | 1.2687 (2) | 0.0105 (3) | |
| O1 | 0.4635 (2) | 0.46164 (13) | 1.2807 (2) | 0.0143 (3) | |
| N1 | 0.7602 (2) | 0.37658 (15) | 1.4085 (2) | 0.0117 (3) | |
| N3 | 0.9507 (2) | 0.34065 (13) | 1.3723 (2) | 0.0090 (3) | |
| O3 | 1.0634 (2) | 0.29447 (12) | 1.51469 (15) | 0.0129 (2) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0094 (2) | 0.0135 (2) | 0.0099 (2) | −0.00124 (10) | 0.00183 (13) | 0.00015 (10) |
| O4 | 0.0111 (6) | 0.0184 (6) | 0.0088 (5) | 0.0013 (4) | 0.0031 (4) | 0.0005 (4) |
| O2 | 0.0147 (6) | 0.0142 (6) | 0.0135 (5) | −0.0008 (4) | 0.0025 (4) | 0.0044 (4) |
| N2 | 0.0104 (6) | 0.0107 (6) | 0.0105 (6) | 0.0001 (4) | 0.0014 (5) | −0.0016 (4) |
| O1 | 0.0072 (6) | 0.0181 (6) | 0.0176 (6) | 0.0021 (4) | 0.0020 (4) | −0.0016 (4) |
| N1 | 0.0098 (7) | 0.0144 (6) | 0.0112 (6) | 0.0028 (5) | 0.0024 (5) | 0.0016 (5) |
| N3 | 0.0086 (6) | 0.0095 (6) | 0.0092 (6) | −0.0014 (4) | 0.0017 (5) | −0.0003 (4) |
| O3 | 0.0117 (6) | 0.0160 (6) | 0.0101 (5) | 0.0018 (4) | −0.0011 (4) | 0.0008 (4) |
Geometric parameters (Å, º) top
| K1—O4 | 2.7800 (12) | O2—N2 | 1.231 (2) |
| K1—O3i | 2.7938 (11) | O2—K1v | 2.9159 (12) |
| K1—O1ii | 2.8022 (12) | N2—O1 | 1.236 (2) |
| K1—O3iii | 2.8238 (11) | N2—N1 | 1.391 (2) |
| K1—O1iv | 2.8837 (12) | N2—K1vii | 3.4262 (13) |
| K1—O4i | 2.8888 (12) | O1—K1ii | 2.8023 (12) |
| K1—O2v | 2.9159 (12) | O1—K1vii | 2.8837 (12) |
| K1—O4v | 2.9954 (11) | N1—N3 | 1.356 (2) |
| K1—N1iii | 3.0232 (14) | N1—K1viii | 3.0232 (14) |
| K1—O2 | 3.1294 (12) | N1—K1vii | 3.2884 (14) |
| K1—N3i | 3.2208 (13) | N3—O3 | 1.246 (2) |
| K1—N1iv | 3.2884 (14) | N3—K1vi | 3.2208 (13) |
| O4—N3 | 1.239 (2) | N3—K1viii | 3.4203 (13) |
| O4—K1vi | 2.8888 (11) | O3—K1vi | 2.7937 (11) |
| O4—K1v | 2.9954 (11) | O3—K1viii | 2.8239 (11) |
| | | |
| O4—K1—O3i | 73.56 (3) | O4v—K1—N3i | 139.06 (3) |
| O4—K1—O1ii | 115.89 (3) | N1iii—K1—N3i | 94.07 (3) |
| O3i—K1—O1ii | 82.03 (3) | O2—K1—N3i | 84.32 (3) |
| O4—K1—O3iii | 130.39 (3) | O4—K1—N1iv | 70.68 (3) |
| O3i—K1—O3iii | 138.17 (2) | O3i—K1—N1iv | 104.36 (3) |
| O1ii—K1—O3iii | 107.13 (3) | O1ii—K1—N1iv | 172.24 (4) |
| O4—K1—O1iv | 93.88 (3) | O3iii—K1—N1iv | 65.18 (3) |
| O3i—K1—O1iv | 79.80 (3) | O1iv—K1—N1iv | 40.72 (3) |
| O1ii—K1—O1iv | 138.71 (2) | O4i—K1—N1iv | 106.30 (3) |
| O3iii—K1—O1iv | 66.45 (3) | O2v—K1—N1iv | 59.61 (3) |
| O4—K1—O4i | 116.43 (3) | O4v—K1—N1iv | 111.14 (3) |
| O3i—K1—O4i | 44.73 (3) | N1iii—K1—N1iv | 106.56 (4) |
| O1ii—K1—O4i | 75.00 (3) | O2—K1—N1iv | 121.52 (3) |
| O3iii—K1—O4i | 97.09 (3) | N3i—K1—N1iv | 109.45 (3) |
| O1iv—K1—O4i | 65.99 (3) | N3—O4—K1 | 140.90 (9) |
| O4—K1—O2v | 76.43 (3) | N3—O4—K1vi | 93.95 (8) |
| O3i—K1—O2v | 149.47 (3) | K1—O4—K1vi | 116.44 (4) |
| O1ii—K1—O2v | 116.68 (3) | N3—O4—K1v | 104.67 (8) |
| O3iii—K1—O2v | 62.55 (3) | K1—O4—K1v | 87.46 (3) |
| O1iv—K1—O2v | 96.92 (3) | K1vi—O4—K1v | 111.18 (4) |
| O4i—K1—O2v | 158.23 (3) | N2—O2—K1v | 130.92 (10) |
| O4—K1—O4v | 92.54 (3) | N2—O2—K1 | 110.78 (8) |
| O3i—K1—O4v | 134.84 (3) | K1v—O2—K1 | 82.65 (3) |
| O1ii—K1—O4v | 65.57 (3) | O2—N2—O1 | 123.47 (13) |
| O3iii—K1—O4v | 83.37 (3) | O2—N2—N1 | 124.30 (13) |
| O1iv—K1—O4v | 144.98 (3) | O1—N2—N1 | 112.03 (12) |
| O4i—K1—O4v | 138.60 (2) | O2—N2—K1vii | 146.09 (10) |
| O2v—K1—O4v | 51.54 (3) | O1—N2—K1vii | 54.23 (7) |
| O4—K1—N1iii | 170.13 (4) | N1—N2—K1vii | 72.54 (8) |
| O3i—K1—N1iii | 116.22 (3) | N2—O1—K1ii | 134.24 (9) |
| O1ii—K1—N1iii | 66.24 (3) | N2—O1—K1vii | 105.41 (8) |
| O3iii—K1—N1iii | 43.36 (3) | K1ii—O1—K1vii | 117.26 (4) |
| O1iv—K1—N1iii | 89.43 (3) | N3—N1—N2 | 114.00 (12) |
| O4i—K1—N1iii | 73.39 (3) | N3—N1—K1viii | 95.04 (8) |
| O2v—K1—N1iii | 93.95 (3) | N2—N1—K1viii | 142.62 (9) |
| O4v—K1—N1iii | 79.51 (3) | N3—N1—K1vii | 124.32 (9) |
| O4—K1—O2 | 51.16 (3) | N2—N1—K1vii | 83.66 (8) |
| O3i—K1—O2 | 67.72 (3) | K1viii—N1—K1vii | 99.47 (4) |
| O1ii—K1—O2 | 64.76 (3) | O4—N3—O3 | 121.10 (13) |
| O3iii—K1—O2 | 153.47 (3) | O4—N3—N1 | 126.00 (12) |
| O1iv—K1—O2 | 137.04 (3) | O3—N3—N1 | 112.78 (12) |
| O4i—K1—O2 | 104.37 (3) | O4—N3—K1vi | 63.48 (7) |
| O2v—K1—O2 | 97.35 (3) | O3—N3—K1vi | 59.11 (7) |
| O4v—K1—O2 | 70.24 (3) | N1—N3—K1vi | 162.01 (9) |
| N1iii—K1—O2 | 129.55 (3) | O4—N3—K1viii | 171.32 (9) |
| O4—K1—N3i | 95.78 (3) | O3—N3—K1viii | 51.75 (7) |
| O3i—K1—N3i | 22.50 (3) | N1—N3—K1viii | 61.70 (7) |
| O1ii—K1—N3i | 74.79 (3) | K1vi—N3—K1viii | 110.42 (4) |
| O3iii—K1—N3i | 119.08 (3) | N3—O3—K1vi | 98.39 (8) |
| O1iv—K1—N3i | 74.30 (3) | N3—O3—K1viii | 107.97 (9) |
| O4i—K1—N3i | 22.57 (3) | K1vi—O3—K1viii | 152.37 (4) |
| O2v—K1—N3i | 168.03 (3) | | |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.274 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.5918 (4) Å | Cell parameters from 2901 reflections |
| b = 9.0778 (5) Å | θ = 6.4–28.0° |
| c = 7.1540 (4) Å | µ = 1.17 mm−1 |
| β = 97.946 (2)° | T = 100 K |
| V = 423.98 (4) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1041 independent reflections |
| Radiation source: Sealed Tube | 918 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.046 |
| ω scans | θmax = 28.4°, θmin = 3.7° |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | h = −8→7 |
| Tmin = 0.768, Tmax = 0.990 | k = −12→12 |
| 3547 measured reflections | l = −8→9 |
Refinement top
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.029 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.068 | Calculated w = 1/[σ2(Fo2) + (0.038P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.00 | (Δ/σ)max < 0.001 |
| 1041 reflections | Δρmax = 0.53 e Å−3 |
| 73 parameters | Δρmin = −0.60 e Å−3 |
Crystal data top
| KN3O4 | V = 423.98 (4) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.5918 (4) Å | µ = 1.17 mm−1 |
| b = 9.0778 (5) Å | T = 100 K |
| c = 7.1540 (4) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.946 (2)° | |
Data collection top
Platform
diffractometer | 1041 independent reflections |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | 918 reflections with I > 2σ(I) |
| Tmin = 0.768, Tmax = 0.990 | Rint = 0.046 |
| 3547 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.029 | 73 parameters |
| wR(F2) = 0.068 | 0 restraints |
| S = 1.00 | Δρmax = 0.53 e Å−3 |
| 1041 reflections | Δρmin = −0.60 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.86034 (4) | 0.34332 (3) | 0.83205 (4) | 0.01160 (12) | |
| O4 | 1.0104 (2) | 0.34353 (11) | 1.21534 (15) | 0.0139 (2) | |
| O2 | 0.7262 (2) | 0.53844 (11) | 1.15502 (15) | 0.0148 (2) | |
| N2 | 0.6488 (2) | 0.46237 (12) | 1.2686 (2) | 0.0111 (3) | |
| O1 | 0.4636 (2) | 0.46163 (12) | 1.2804 (2) | 0.0155 (2) | |
| N1 | 0.7599 (2) | 0.37665 (14) | 1.4081 (2) | 0.0122 (3) | |
| N3 | 0.9506 (2) | 0.34062 (12) | 1.3721 (2) | 0.0100 (3) | |
| O3 | 1.06313 (15) | 0.29457 (11) | 1.51450 (13) | 0.0132 (2) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0107 (2) | 0.0152 (2) | 0.0092 (2) | −0.00139 (10) | 0.00223 (12) | 0.00025 (10) |
| O4 | 0.0130 (5) | 0.0215 (6) | 0.0080 (5) | 0.0017 (4) | 0.0041 (4) | 0.0008 (4) |
| O2 | 0.0158 (6) | 0.0154 (5) | 0.0133 (5) | −0.0012 (4) | 0.0019 (4) | 0.0043 (4) |
| N2 | 0.0114 (6) | 0.0115 (6) | 0.0104 (6) | 0.0004 (4) | 0.0013 (4) | −0.0018 (4) |
| O1 | 0.0081 (5) | 0.0196 (6) | 0.0188 (5) | 0.0024 (4) | 0.0019 (4) | −0.0016 (4) |
| N1 | 0.0113 (6) | 0.0150 (6) | 0.0108 (6) | 0.0033 (4) | 0.0031 (5) | 0.0022 (4) |
| N3 | 0.0104 (6) | 0.0106 (6) | 0.0091 (6) | −0.0012 (4) | 0.0022 (4) | −0.0006 (4) |
| O3 | 0.0131 (5) | 0.0167 (5) | 0.0090 (5) | 0.0022 (4) | −0.0012 (4) | 0.0009 (4) |
Geometric parameters (Å, º) top
| K1—O4 | 2.7834 (11) | O2—N2 | 1.230 (2) |
| K1—O3i | 2.7957 (11) | O2—K1v | 2.9188 (11) |
| K1—O1ii | 2.8049 (11) | N2—O1 | 1.235 (2) |
| K1—O3iii | 2.8255 (10) | N2—N1 | 1.391 (2) |
| K1—O1iv | 2.8868 (11) | N2—K1vii | 3.4295 (12) |
| K1—O4i | 2.8920 (11) | O1—K1ii | 2.8049 (11) |
| K1—O2v | 2.9188 (11) | O1—K1vii | 2.8868 (11) |
| K1—O4v | 3.0003 (11) | N1—N3 | 1.357 (2) |
| K1—N1iii | 3.0289 (12) | N1—K1viii | 3.0289 (12) |
| K1—O2 | 3.1341 (11) | N1—K1vii | 3.2901 (13) |
| K1—N3i | 3.2219 (12) | N3—O3 | 1.2467 (15) |
| K1—N1iv | 3.2900 (13) | N3—K1vi | 3.2219 (12) |
| O4—N3 | 1.239 (2) | N3—K1viii | 3.4239 (12) |
| O4—K1vi | 2.8919 (11) | O3—K1vi | 2.7957 (11) |
| O4—K1v | 3.0003 (11) | O3—K1viii | 2.8255 (10) |
| | | |
| O4—K1—O3i | 73.55 (3) | O4v—K1—N3i | 139.10 (3) |
| O4—K1—O1ii | 115.77 (3) | N1iii—K1—N3i | 94.07 (3) |
| O3i—K1—O1ii | 82.04 (3) | O2—K1—N3i | 84.37 (3) |
| O4—K1—O3iii | 130.47 (3) | O4—K1—N1iv | 70.74 (3) |
| O3i—K1—O3iii | 138.18 (2) | O3i—K1—N1iv | 104.34 (3) |
| O1ii—K1—O3iii | 107.12 (3) | O1ii—K1—N1iv | 172.27 (3) |
| O4—K1—O1iv | 93.95 (3) | O3iii—K1—N1iv | 65.23 (3) |
| O3i—K1—O1iv | 79.83 (3) | O1iv—K1—N1iv | 40.67 (3) |
| O1ii—K1—O1iv | 138.79 (2) | O4i—K1—N1iv | 106.27 (3) |
| O3iii—K1—O1iv | 66.46 (3) | O2v—K1—N1iv | 59.69 (3) |
| O4—K1—O4i | 116.45 (3) | O4v—K1—N1iv | 111.12 (3) |
| O3i—K1—O4i | 44.74 (3) | N1iii—K1—N1iv | 106.58 (4) |
| O1ii—K1—O4i | 75.06 (3) | O2—K1—N1iv | 121.48 (3) |
| O3iii—K1—O4i | 97.07 (3) | N3i—K1—N1iv | 109.43 (3) |
| O1iv—K1—O4i | 66.01 (3) | N3—O4—K1 | 141.01 (9) |
| O4—K1—O2v | 76.44 (3) | N3—O4—K1vi | 93.85 (7) |
| O3i—K1—O2v | 149.48 (3) | K1—O4—K1vi | 116.40 (4) |
| O1ii—K1—O2v | 116.59 (3) | N3—O4—K1v | 104.67 (8) |
| O3iii—K1—O2v | 62.59 (3) | K1—O4—K1v | 87.54 (3) |
| O1iv—K1—O2v | 96.95 (3) | K1vi—O4—K1v | 111.14 (4) |
| O4i—K1—O2v | 158.27 (3) | N2—O2—K1v | 131.02 (9) |
| O4—K1—O4v | 92.46 (3) | N2—O2—K1 | 110.79 (8) |
| O3i—K1—O4v | 134.85 (3) | K1v—O2—K1 | 82.75 (3) |
| O1ii—K1—O4v | 65.57 (3) | O2—N2—O1 | 123.51 (12) |
| O3iii—K1—O4v | 83.35 (3) | O2—N2—N1 | 124.26 (12) |
| O1iv—K1—O4v | 144.93 (3) | O1—N2—N1 | 112.05 (11) |
| O4i—K1—O4v | 138.66 (2) | O2—N2—K1vii | 146.11 (9) |
| O2v—K1—O4v | 51.43 (3) | O1—N2—K1vii | 54.22 (7) |
| O4—K1—N1iii | 170.12 (3) | N1—N2—K1vii | 72.48 (7) |
| O3i—K1—N1iii | 116.23 (3) | N2—O1—K1ii | 134.23 (8) |
| O1ii—K1—N1iii | 66.27 (3) | N2—O1—K1vii | 105.47 (8) |
| O3iii—K1—N1iii | 43.34 (3) | K1ii—O1—K1vii | 117.28 (4) |
| O1iv—K1—N1iii | 89.44 (3) | N3—N1—N2 | 114.09 (11) |
| O4i—K1—N1iii | 73.40 (3) | N3—N1—K1viii | 94.93 (7) |
| O2v—K1—N1iii | 93.95 (3) | N2—N1—K1viii | 142.62 (9) |
| O4v—K1—N1iii | 79.54 (3) | N3—N1—K1vii | 124.30 (8) |
| O4—K1—O2 | 51.05 (3) | N2—N1—K1vii | 83.74 (7) |
| O3i—K1—O2 | 67.76 (3) | K1viii—N1—K1vii | 99.45 (4) |
| O1ii—K1—O2 | 64.75 (3) | O4—N3—O3 | 121.25 (12) |
| O3iii—K1—O2 | 153.42 (3) | O4—N3—N1 | 125.82 (11) |
| O1iv—K1—O2 | 137.05 (3) | O3—N3—N1 | 112.82 (11) |
| O4i—K1—O2 | 104.43 (3) | O4—N3—K1vi | 63.58 (7) |
| O2v—K1—O2 | 97.25 (3) | O3—N3—K1vi | 59.16 (7) |
| O4v—K1—O2 | 70.21 (3) | N1—N3—K1vi | 162.06 (8) |
| N1iii—K1—O2 | 129.56 (3) | O4—N3—K1viii | 171.38 (9) |
| O4—K1—N3i | 95.79 (3) | O3—N3—K1viii | 51.67 (7) |
| O3i—K1—N3i | 22.51 (3) | N1—N3—K1viii | 61.80 (7) |
| O1ii—K1—N3i | 74.82 (3) | K1vi—N3—K1viii | 110.38 (3) |
| O3iii—K1—N3i | 119.07 (3) | N3—O3—K1vi | 98.33 (8) |
| O1iv—K1—N3i | 74.33 (3) | N3—O3—K1viii | 108.07 (8) |
| O4i—K1—N3i | 22.57 (3) | K1vi—O3—K1viii | 152.31 (4) |
| O2v—K1—N3i | 168.08 (3) | | |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.255 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.6010 (3) Å | Cell parameters from 2857 reflections |
| b = 9.1253 (5) Å | θ = 5.0–28.3° |
| c = 7.1657 (4) Å | µ = 1.16 mm−1 |
| β = 97.890 (1)° | T = 150 K |
| V = 427.55 (4) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1046 independent reflections |
| Radiation source: Sealed Tube | 917 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.040 |
| ω scans | θmax = 28.3°, θmin = 3.6° |
Absorption correction: empirical: Multipole Expansion (Blessing, 1995)
? | h = −7→8 |
| Tmin = 0.780, Tmax = 0.990 | k = −12→12 |
| 3517 measured reflections | l = −9→8 |
Refinement top
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.030 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.072 | Calculated w = 1/[σ2(Fo2) + (0.0401P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.04 | (Δ/σ)max < 0.001 |
| 1046 reflections | Δρmax = 0.36 e Å−3 |
| 73 parameters | Δρmin = −0.39 e Å−3 |
Crystal data top
| KN3O4 | V = 427.55 (4) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.6010 (3) Å | µ = 1.16 mm−1 |
| b = 9.1253 (5) Å | T = 150 K |
| c = 7.1657 (4) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.890 (1)° | |
Data collection top
Platform
diffractometer | 1046 independent reflections |
Absorption correction: empirical: Multipole Expansion (Blessing, 1995)
? | 917 reflections with I > 2σ(I) |
| Tmin = 0.780, Tmax = 0.990 | Rint = 0.040 |
| 3517 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.030 | 73 parameters |
| wR(F2) = 0.072 | 0 restraints |
| S = 1.04 | Δρmax = 0.36 e Å−3 |
| 1046 reflections | Δρmin = −0.39 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.85986 (5) | 0.34296 (3) | 0.83151 (4) | 0.01590 (13) | |
| O4 | 1.0097 (2) | 0.34379 (12) | 1.2150 (2) | 0.0190 (3) | |
| O2 | 0.7268 (2) | 0.53839 (12) | 1.1558 (2) | 0.0207 (3) | |
| N2 | 0.6489 (2) | 0.46223 (13) | 1.2683 (2) | 0.0152 (3) | |
| O1 | 0.4639 (2) | 0.46152 (13) | 1.2799 (2) | 0.0219 (3) | |
| N1 | 0.7594 (2) | 0.37658 (14) | 1.4071 (2) | 0.0163 (3) | |
| N3 | 0.9499 (2) | 0.34079 (12) | 1.3713 (2) | 0.0131 (3) | |
| O3 | 1.0620 (2) | 0.29468 (12) | 1.51298 (14) | 0.0178 (2) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0148 (2) | 0.0202 (2) | 0.0133 (2) | −0.00209 (11) | 0.00379 (13) | 0.00038 (10) |
| O4 | 0.0172 (6) | 0.0290 (6) | 0.0120 (5) | 0.0023 (4) | 0.0058 (4) | 0.0011 (4) |
| O2 | 0.0219 (6) | 0.0203 (6) | 0.0198 (6) | −0.0019 (4) | 0.0023 (4) | 0.0065 (4) |
| N2 | 0.0160 (6) | 0.0147 (6) | 0.0149 (6) | 0.0003 (4) | 0.0023 (5) | −0.0021 (4) |
| O1 | 0.0126 (6) | 0.0268 (6) | 0.0264 (6) | 0.0039 (4) | 0.0029 (5) | −0.0024 (4) |
| N1 | 0.0150 (7) | 0.0185 (6) | 0.0160 (6) | 0.0044 (5) | 0.0050 (5) | 0.0030 (5) |
| N3 | 0.0136 (6) | 0.0138 (6) | 0.0124 (6) | −0.0014 (4) | 0.0035 (5) | −0.0006 (4) |
| O3 | 0.0178 (6) | 0.0224 (6) | 0.0127 (5) | 0.0036 (4) | 0.0000 (4) | 0.0014 (4) |
Geometric parameters (Å, º) top
| K1—O4 | 2.7900 (12) | O2—N2 | 1.230 (2) |
| K1—O3i | 2.7991 (11) | O2—K1v | 2.9250 (12) |
| K1—O1ii | 2.8139 (12) | N2—O1 | 1.236 (2) |
| K1—O3iii | 2.8321 (11) | N2—N1 | 1.390 (2) |
| K1—O1iv | 2.8979 (12) | N2—K1vii | 3.4406 (13) |
| K1—O4i | 2.9006 (12) | O1—K1ii | 2.8140 (12) |
| K1—O2v | 2.9250 (12) | O1—K1vii | 2.8979 (12) |
| K1—O4v | 3.0170 (12) | N1—N3 | 1.357 (2) |
| K1—N1iii | 3.0381 (13) | N1—K1viii | 3.0380 (13) |
| K1—O2 | 3.1480 (12) | N1—K1vii | 3.2968 (13) |
| K1—N3i | 3.2292 (13) | N3—O3 | 1.245 (2) |
| K1—N1iv | 3.2968 (13) | N3—K1vi | 3.2293 (13) |
| O4—N3 | 1.238 (2) | N3—K1viii | 3.4303 (13) |
| O4—K1vi | 2.9006 (11) | O3—K1vi | 2.7992 (11) |
| O4—K1v | 3.0170 (12) | O3—K1viii | 2.8321 (11) |
| | | |
| O4—K1—O3i | 73.76 (3) | O4v—K1—N3i | 139.20 (3) |
| O4—K1—O1ii | 115.49 (3) | N1iii—K1—N3i | 94.03 (3) |
| O3i—K1—O1ii | 82.06 (3) | O2—K1—N3i | 84.66 (3) |
| O4—K1—O3iii | 130.67 (3) | O4—K1—N1iv | 70.88 (3) |
| O3i—K1—O3iii | 138.01 (2) | O3i—K1—N1iv | 104.36 (3) |
| O1ii—K1—O3iii | 107.07 (3) | O1ii—K1—N1iv | 172.33 (4) |
| O4—K1—O1iv | 94.03 (3) | O3iii—K1—N1iv | 65.36 (3) |
| O3i—K1—O1iv | 79.80 (3) | O1iv—K1—N1iv | 40.55 (3) |
| O1ii—K1—O1iv | 139.09 (2) | O4i—K1—N1iv | 106.15 (3) |
| O3iii—K1—O1iv | 66.54 (3) | O2v—K1—N1iv | 59.88 (3) |
| O4—K1—O4i | 116.48 (3) | O4v—K1—N1iv | 111.09 (3) |
| O3i—K1—O4i | 44.55 (3) | N1iii—K1—N1iv | 106.60 (4) |
| O1ii—K1—O4i | 75.33 (3) | O2—K1—N1iv | 121.39 (3) |
| O3iii—K1—O4i | 96.99 (3) | N3i—K1—N1iv | 109.34 (3) |
| O1iv—K1—O4i | 66.00 (3) | N3—O4—K1 | 140.99 (9) |
| O4—K1—O2v | 76.42 (3) | N3—O4—K1vi | 93.85 (8) |
| O3i—K1—O2v | 149.68 (3) | K1—O4—K1vi | 116.27 (4) |
| O1ii—K1—O2v | 116.29 (3) | N3—O4—K1v | 104.61 (8) |
| O3iii—K1—O2v | 62.75 (3) | K1—O4—K1v | 87.81 (3) |
| O1iv—K1—O2v | 97.04 (3) | K1vi—O4—K1v | 111.12 (4) |
| O4i—K1—O2v | 158.35 (4) | N2—O2—K1v | 131.39 (9) |
| O4—K1—O4v | 92.19 (3) | N2—O2—K1 | 110.38 (8) |
| O3i—K1—O4v | 134.89 (3) | K1v—O2—K1 | 83.07 (3) |
| O1ii—K1—O4v | 65.48 (3) | O2—N2—O1 | 123.59 (12) |
| O3iii—K1—O4v | 83.41 (3) | O2—N2—N1 | 124.15 (13) |
| O1iv—K1—O4v | 144.90 (3) | O1—N2—N1 | 112.06 (12) |
| O4i—K1—O4v | 138.86 (2) | O2—N2—K1vii | 146.43 (9) |
| O2v—K1—O4v | 51.22 (3) | O1—N2—K1vii | 54.26 (7) |
| O4—K1—N1iii | 170.04 (4) | N1—N2—K1vii | 72.34 (8) |
| O3i—K1—N1iii | 116.08 (3) | N2—O1—K1ii | 134.18 (9) |
| O1ii—K1—N1iii | 66.37 (3) | N2—O1—K1vii | 105.50 (8) |
| O3iii—K1—N1iii | 43.21 (3) | K1ii—O1—K1vii | 117.40 (4) |
| O1iv—K1—N1iii | 89.54 (3) | N3—N1—N2 | 114.12 (11) |
| O4i—K1—N1iii | 73.46 (3) | N3—N1—K1viii | 94.83 (8) |
| O2v—K1—N1iii | 93.92 (3) | N2—N1—K1viii | 142.55 (9) |
| O4v—K1—N1iii | 79.64 (3) | N3—N1—K1vii | 124.31 (9) |
| O4—K1—O2 | 50.84 (3) | N2—N1—K1vii | 83.97 (8) |
| O3i—K1—O2 | 68.07 (3) | K1viii—N1—K1vii | 99.38 (4) |
| O1ii—K1—O2 | 64.67 (3) | O4—N3—O3 | 121.17 (12) |
| O3iii—K1—O2 | 153.25 (3) | O4—N3—N1 | 125.77 (12) |
| O1iv—K1—O2 | 137.09 (3) | O3—N3—N1 | 112.94 (12) |
| O4i—K1—O2 | 104.67 (3) | O4—N3—K1vi | 63.66 (7) |
| O2v—K1—O2 | 96.93 (3) | O3—N3—K1vi | 58.99 (7) |
| O4v—K1—O2 | 69.97 (3) | N1—N3—K1vi | 161.99 (9) |
| N1iii—K1—O2 | 129.57 (3) | O4—N3—K1viii | 171.30 (9) |
| O4—K1—N3i | 95.89 (3) | O3—N3—K1viii | 51.68 (7) |
| O3i—K1—N3i | 22.40 (3) | N1—N3—K1viii | 61.95 (7) |
| O1ii—K1—N3i | 75.01 (3) | K1vi—N3—K1viii | 110.22 (3) |
| O3iii—K1—N3i | 118.92 (3) | N3—O3—K1vi | 98.61 (8) |
| O1iv—K1—N3i | 74.31 (3) | N3—O3—K1viii | 108.15 (8) |
| O4i—K1—N3i | 22.49 (3) | K1vi—O3—K1viii | 151.99 (4) |
| O2v—K1—N3i | 168.19 (3) | | |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.240 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.6029 (4) Å | Cell parameters from 2788 reflections |
| b = 9.1694 (5) Å | θ = 5.9–23.8° |
| c = 7.1731 (4) Å | µ = 1.15 mm−1 |
| β = 97.805 (1)° | T = 200 K |
| V = 430.27 (4) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1060 independent reflections |
| Radiation source: Sealed Tube | 911 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.040 |
| ω scans | θmax = 28.3°, θmin = 3.6° |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | h = −8→7 |
| Tmin = 0.723, Tmax = 0.990 | k = −12→12 |
| 3510 measured reflections | l = −8→9 |
Refinement top
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.032 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.077 | Calculated w = 1/[σ2(Fo2) + (0.0462P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.00 | (Δ/σ)max = −0.001 |
| 1060 reflections | Δρmax = 0.36 e Å−3 |
| 73 parameters | Δρmin = −0.35 e Å−3 |
Crystal data top
| KN3O4 | V = 430.27 (4) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.6029 (4) Å | µ = 1.15 mm−1 |
| b = 9.1694 (5) Å | T = 200 K |
| c = 7.1731 (4) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.805 (1)° | |
Data collection top
Platform
diffractometer | 1060 independent reflections |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | 911 reflections with I > 2σ(I) |
| Tmin = 0.723, Tmax = 0.990 | Rint = 0.040 |
| 3510 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.032 | 73 parameters |
| wR(F2) = 0.077 | 0 restraints |
| S = 1.00 | Δρmax = 0.36 e Å−3 |
| 1060 reflections | Δρmin = −0.35 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.85932 (5) | 0.34264 (4) | 0.83074 (5) | 0.02090 (14) | |
| O4 | 1.0087 (2) | 0.34421 (13) | 1.2144 (2) | 0.0251 (3) | |
| O2 | 0.7270 (2) | 0.53812 (13) | 1.1565 (2) | 0.0277 (3) | |
| N2 | 0.6490 (2) | 0.46223 (14) | 1.2684 (2) | 0.0198 (3) | |
| O1 | 0.4642 (2) | 0.46145 (14) | 1.2792 (2) | 0.0287 (3) | |
| N1 | 0.7587 (2) | 0.3766 (2) | 1.4063 (2) | 0.0212 (3) | |
| N3 | 0.9489 (2) | 0.34099 (13) | 1.3703 (2) | 0.0170 (3) | |
| O3 | 1.0607 (2) | 0.29491 (13) | 1.5113 (2) | 0.0233 (3) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0205 (2) | 0.0264 (2) | 0.0162 (2) | −0.00291 (12) | 0.00371 (13) | 0.00034 (11) |
| O4 | 0.0227 (6) | 0.0392 (7) | 0.0144 (6) | 0.0030 (5) | 0.0065 (5) | 0.0009 (4) |
| O2 | 0.0301 (7) | 0.0266 (6) | 0.0256 (6) | −0.0020 (5) | 0.0014 (5) | 0.0090 (5) |
| N2 | 0.0218 (7) | 0.0182 (6) | 0.0189 (6) | 0.0008 (5) | 0.0014 (5) | −0.0021 (5) |
| O1 | 0.0178 (6) | 0.0345 (7) | 0.0336 (7) | 0.0055 (5) | 0.0030 (5) | −0.0029 (5) |
| N1 | 0.0208 (7) | 0.0240 (7) | 0.0196 (7) | 0.0055 (5) | 0.0061 (5) | 0.0033 (5) |
| N3 | 0.0192 (7) | 0.0180 (6) | 0.0140 (6) | −0.0015 (4) | 0.0031 (5) | −0.0008 (4) |
| O3 | 0.0244 (6) | 0.0295 (6) | 0.0150 (5) | 0.0043 (5) | −0.0012 (4) | 0.0014 (5) |
Geometric parameters (Å, º) top
| K1—O4 | 2.7945 (13) | O2—N2 | 1.227 (2) |
| K1—O3i | 2.8020 (12) | O2—K1v | 2.9318 (13) |
| K1—O1ii | 2.8206 (13) | N2—O1 | 1.233 (2) |
| K1—O3iii | 2.8348 (12) | N2—N1 | 1.388 (2) |
| K1—O1iv | 2.9087 (13) | N2—K1vii | 3.4503 (14) |
| K1—O4i | 2.9097 (13) | O1—K1ii | 2.8206 (13) |
| K1—O2v | 2.9318 (13) | O1—K1vii | 2.9086 (13) |
| K1—O4v | 3.0309 (13) | N1—N3 | 1.356 (2) |
| K1—N1iii | 3.0427 (14) | N1—K1viii | 3.0427 (14) |
| K1—O2 | 3.1610 (14) | N1—K1vii | 3.3014 (15) |
| K1—N3i | 3.2354 (13) | N3—O3 | 1.242 (2) |
| K1—N1iv | 3.3014 (15) | N3—K1vi | 3.2354 (13) |
| O4—N3 | 1.236 (2) | N3—K1viii | 3.4335 (13) |
| O4—K1vi | 2.9097 (13) | O3—K1vi | 2.8020 (12) |
| O4—K1v | 3.0309 (13) | O3—K1viii | 2.8348 (12) |
| | | |
| O4—K1—O3i | 73.95 (4) | O4v—K1—N3i | 139.36 (3) |
| O4—K1—O1ii | 115.14 (4) | N1iii—K1—N3i | 93.97 (4) |
| O3i—K1—O1ii | 82.07 (4) | O2—K1—N3i | 84.92 (3) |
| O4—K1—O3iii | 130.94 (4) | O4—K1—N1iv | 70.99 (3) |
| O3i—K1—O3iii | 137.81 (3) | O3i—K1—N1iv | 104.29 (4) |
| O1ii—K1—O3iii | 107.02 (4) | O1ii—K1—N1iv | 172.49 (4) |
| O4—K1—O1iv | 94.11 (4) | O3iii—K1—N1iv | 65.60 (3) |
| O3i—K1—O1iv | 79.74 (4) | O1iv—K1—N1iv | 40.41 (3) |
| O1ii—K1—O1iv | 139.41 (3) | O4i—K1—N1iv | 105.98 (4) |
| O3iii—K1—O1iv | 66.64 (4) | O2v—K1—N1iv | 60.13 (3) |
| O4—K1—O4i | 116.50 (4) | O4v—K1—N1iv | 111.07 (4) |
| O3i—K1—O4i | 44.36 (3) | N1iii—K1—N1iv | 106.71 (4) |
| O1ii—K1—O4i | 75.63 (4) | O2—K1—N1iv | 121.24 (3) |
| O3iii—K1—O4i | 96.86 (4) | N3i—K1—N1iv | 109.19 (3) |
| O1iv—K1—O4i | 65.99 (3) | N3—O4—K1 | 141.04 (10) |
| O4—K1—O2v | 76.39 (4) | N3—O4—K1vi | 93.78 (8) |
| O3i—K1—O2v | 149.84 (4) | K1—O4—K1vi | 116.11 (4) |
| O1ii—K1—O2v | 115.99 (4) | N3—O4—K1v | 104.54 (9) |
| O3iii—K1—O2v | 62.97 (3) | K1—O4—K1v | 88.16 (3) |
| O1iv—K1—O2v | 97.16 (4) | K1vi—O4—K1v | 111.06 (4) |
| O4i—K1—O2v | 158.44 (4) | N2—O2—K1v | 131.56 (10) |
| O4—K1—O4v | 91.84 (3) | N2—O2—K1 | 110.16 (9) |
| O3i—K1—O4v | 134.94 (4) | K1v—O2—K1 | 83.38 (4) |
| O1ii—K1—O4v | 65.45 (4) | O2—N2—O1 | 123.48 (13) |
| O3iii—K1—O4v | 83.50 (3) | O2—N2—N1 | 124.19 (14) |
| O1iv—K1—O4v | 144.86 (4) | O1—N2—N1 | 112.15 (13) |
| O4i—K1—O4v | 139.14 (3) | O2—N2—K1vii | 146.47 (10) |
| O2v—K1—O4v | 50.94 (3) | O1—N2—K1vii | 54.30 (8) |
| O4—K1—N1iii | 169.98 (4) | N1—N2—K1vii | 72.18 (8) |
| O3i—K1—N1iii | 115.90 (4) | N2—O1—K1ii | 134.19 (10) |
| O1ii—K1—N1iii | 66.48 (4) | N2—O1—K1vii | 105.56 (9) |
| O3iii—K1—N1iii | 43.08 (3) | K1ii—O1—K1vii | 117.49 (4) |
| O1iv—K1—N1iii | 89.67 (4) | N3—N1—N2 | 114.07 (12) |
| O4i—K1—N1iii | 73.51 (4) | N3—N1—K1viii | 94.82 (8) |
| O2v—K1—N1iii | 93.95 (4) | N2—N1—K1viii | 142.47 (10) |
| O4v—K1—N1iii | 79.81 (4) | N3—N1—K1vii | 124.21 (9) |
| O4—K1—O2 | 50.58 (3) | N2—N1—K1vii | 84.23 (9) |
| O3i—K1—O2 | 68.34 (3) | K1viii—N1—K1vii | 99.38 (4) |
| O1ii—K1—O2 | 64.58 (3) | O4—N3—O3 | 121.16 (13) |
| O3iii—K1—O2 | 153.14 (3) | O4—N3—N1 | 125.77 (12) |
| O1iv—K1—O2 | 137.05 (3) | O3—N3—N1 | 112.95 (12) |
| O4i—K1—O2 | 104.89 (3) | O4—N3—K1vi | 63.82 (8) |
| O2v—K1—O2 | 96.62 (4) | O3—N3—K1vi | 58.83 (7) |
| O4v—K1—O2 | 69.76 (3) | N1—N3—K1vi | 161.88 (9) |
| N1iii—K1—O2 | 129.58 (3) | O4—N3—K1viii | 171.22 (10) |
| O4—K1—N3i | 95.98 (3) | O3—N3—K1viii | 51.62 (7) |
| O3i—K1—N3i | 22.30 (3) | N1—N3—K1viii | 62.01 (7) |
| O1ii—K1—N3i | 75.19 (4) | K1vi—N3—K1viii | 110.02 (4) |
| O3iii—K1—N3i | 118.74 (4) | N3—O3—K1vi | 98.87 (9) |
| O1iv—K1—N3i | 74.28 (3) | N3—O3—K1viii | 108.28 (9) |
| O4i—K1—N3i | 22.41 (3) | K1vi—O3—K1viii | 151.63 (4) |
| O2v—K1—N3i | 168.29 (3) | | |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.217 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.6114 (1) Å | Cell parameters from 2693 reflections |
| b = 9.2299 (2) Å | θ = 6.3–23.4° |
| c = 7.1878 (2) Å | µ = 1.14 mm−1 |
| β = 97.639 (1)° | T = 250 K |
| V = 434.73 (2) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1073 independent reflections |
| Radiation source: Sealed Tube | 882 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.045 |
| ω scans | θmax = 28.3°, θmin = 3.6° |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | h = −7→8 |
| Tmin = 0.685, Tmax = 0.990 | k = −12→12 |
| 3613 measured reflections | l = −9→8 |
Refinement top
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
| R[F2 > 2σ(F2)] = 0.033 | Secondary atom site location: difference Fourier map |
| wR(F2) = 0.081 | Calculated w = 1/[σ2(Fo2) + (0.045P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.00 | (Δ/σ)max = −0.001 |
| 1073 reflections | Δρmax = 0.31 e Å−3 |
| 73 parameters | Δρmin = −0.43 e Å−3 |
Crystal data top
| KN3O4 | V = 434.73 (2) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.6114 (1) Å | µ = 1.14 mm−1 |
| b = 9.2299 (2) Å | T = 250 K |
| c = 7.1878 (2) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.639 (1)° | |
Data collection top
Platform
diffractometer | 1073 independent reflections |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | 882 reflections with I > 2σ(I) |
| Tmin = 0.685, Tmax = 0.990 | Rint = 0.045 |
| 3613 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.033 | 73 parameters |
| wR(F2) = 0.081 | 0 restraints |
| S = 1.00 | Δρmax = 0.31 e Å−3 |
| 1073 reflections | Δρmin = −0.43 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.85870 (6) | 0.34234 (4) | 0.82994 (5) | 0.02730 (15) | |
| O4 | 1.0075 (2) | 0.34456 (14) | 1.2139 (2) | 0.0323 (3) | |
| O2 | 0.7276 (2) | 0.53794 (14) | 1.1571 (2) | 0.0363 (3) | |
| N2 | 0.6491 (2) | 0.46221 (15) | 1.2686 (2) | 0.0259 (3) | |
| O1 | 0.4645 (2) | 0.46136 (15) | 1.2790 (2) | 0.0377 (3) | |
| N1 | 0.7581 (2) | 0.3764 (2) | 1.4055 (2) | 0.0270 (3) | |
| N3 | 0.9479 (2) | 0.34133 (14) | 1.3694 (2) | 0.0220 (3) | |
| O3 | 1.0592 (2) | 0.29509 (14) | 1.5097 (2) | 0.0302 (3) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0263 (2) | 0.0343 (2) | 0.0216 (2) | −0.00368 (13) | 0.00464 (14) | 0.00040 (13) |
| O4 | 0.0283 (7) | 0.0506 (8) | 0.0193 (6) | 0.0042 (5) | 0.0078 (5) | 0.0017 (5) |
| O2 | 0.0385 (8) | 0.0343 (7) | 0.0349 (7) | −0.0024 (5) | 0.0009 (6) | 0.0117 (5) |
| N2 | 0.0276 (7) | 0.0244 (7) | 0.0252 (7) | 0.0010 (5) | 0.0017 (6) | −0.0030 (5) |
| O1 | 0.0236 (7) | 0.0456 (8) | 0.0435 (8) | 0.0074 (5) | 0.0035 (6) | −0.0045 (6) |
| N1 | 0.0263 (8) | 0.0312 (8) | 0.0248 (7) | 0.0065 (6) | 0.0076 (6) | 0.0040 (6) |
| N3 | 0.0236 (7) | 0.0238 (7) | 0.0188 (7) | −0.0017 (5) | 0.0038 (5) | −0.0008 (5) |
| O3 | 0.0301 (7) | 0.0390 (7) | 0.0202 (6) | 0.0061 (5) | −0.0015 (5) | 0.0019 (5) |
Geometric parameters (Å, º) top
| K1—O4 | 2.8043 (14) | O2—N2 | 1.229 (2) |
| K1—O3i | 2.8070 (13) | O2—K1v | 2.9398 (14) |
| K1—O1ii | 2.8313 (13) | N2—O1 | 1.233 (2) |
| K1—O3iii | 2.8386 (13) | N2—N1 | 1.387 (2) |
| K1—O4i | 2.9235 (13) | N2—K1vii | 3.4652 (15) |
| K1—O1iv | 2.9238 (15) | O1—K1ii | 2.8313 (13) |
| K1—O2v | 2.9399 (14) | O1—K1vii | 2.9238 (15) |
| K1—O4v | 3.0508 (14) | N1—N3 | 1.354 (2) |
| K1—N1iii | 3.051 (2) | N1—K1viii | 3.051 (2) |
| K1—O2 | 3.175 (2) | N1—K1vii | 3.311 (2) |
| K1—N3i | 3.2457 (14) | N3—O3 | 1.242 (2) |
| K1—N1iv | 3.311 (2) | N3—K1vi | 3.2457 (14) |
| O4—N3 | 1.233 (2) | N3—K1viii | 3.4391 (14) |
| O4—K1vi | 2.9235 (13) | O3—K1vi | 2.8070 (13) |
| O4—K1v | 3.0508 (14) | O3—K1viii | 2.8385 (13) |
| | | |
| O4—K1—O3i | 74.16 (4) | O4v—K1—N3i | 139.57 (4) |
| O4—K1—O1ii | 114.88 (4) | N1iii—K1—N3i | 93.86 (4) |
| O3i—K1—O1ii | 82.18 (4) | O2—K1—N3i | 85.32 (3) |
| O4—K1—O3iii | 131.20 (4) | O4—K1—N1iv | 71.05 (3) |
| O3i—K1—O3iii | 137.55 (3) | O3i—K1—N1iv | 104.18 (4) |
| O1ii—K1—O3iii | 106.89 (4) | O1ii—K1—N1iv | 172.59 (4) |
| O4—K1—O4i | 116.52 (4) | O3iii—K1—N1iv | 65.86 (4) |
| O3i—K1—O4i | 44.16 (3) | O4i—K1—N1iv | 105.82 (4) |
| O1ii—K1—O4i | 75.95 (4) | O1iv—K1—N1iv | 40.28 (3) |
| O3iii—K1—O4i | 96.71 (4) | O2v—K1—N1iv | 60.38 (4) |
| O4—K1—O1iv | 94.11 (4) | O4v—K1—N1iv | 111.03 (4) |
| O3i—K1—O1iv | 79.60 (4) | N1iii—K1—N1iv | 106.86 (4) |
| O1ii—K1—O1iv | 139.74 (3) | O2—K1—N1iv | 121.04 (4) |
| O3iii—K1—O1iv | 66.79 (4) | N3i—K1—N1iv | 108.99 (3) |
| O4i—K1—O1iv | 65.96 (4) | N3—O4—K1 | 141.14 (10) |
| O4—K1—O2v | 76.28 (4) | N3—O4—K1vi | 93.71 (9) |
| O3i—K1—O2v | 149.94 (4) | K1—O4—K1vi | 115.97 (4) |
| O1ii—K1—O2v | 115.66 (4) | N3—O4—K1v | 104.38 (10) |
| O3iii—K1—O2v | 63.30 (4) | K1—O4—K1v | 88.50 (4) |
| O4i—K1—O2v | 158.60 (4) | K1vi—O4—K1v | 111.00 (4) |
| O1iv—K1—O2v | 97.32 (4) | N2—O2—K1v | 131.65 (11) |
| O4—K1—O4v | 91.50 (4) | N2—O2—K1 | 109.88 (10) |
| O3i—K1—O4v | 135.04 (4) | K1v—O2—K1 | 83.85 (4) |
| O1ii—K1—O4v | 65.40 (4) | O2—N2—O1 | 123.39 (14) |
| O3iii—K1—O4v | 83.61 (4) | O2—N2—N1 | 124.24 (14) |
| O4i—K1—O4v | 139.43 (3) | O1—N2—N1 | 112.22 (14) |
| O1iv—K1—O4v | 144.86 (4) | O2—N2—K1vii | 146.44 (11) |
| O2v—K1—O4v | 50.65 (4) | O1—N2—K1vii | 54.36 (8) |
| O4—K1—N1iii | 169.96 (4) | N1—N2—K1vii | 72.00 (9) |
| O3i—K1—N1iii | 115.68 (4) | N2—O1—K1ii | 134.11 (11) |
| O1ii—K1—N1iii | 66.50 (4) | N2—O1—K1vii | 105.60 (10) |
| O3iii—K1—N1iii | 42.97 (3) | K1ii—O1—K1vii | 117.64 (4) |
| O4i—K1—N1iii | 73.52 (4) | N3—N1—N2 | 114.05 (13) |
| O1iv—K1—N1iii | 89.86 (4) | N3—N1—K1viii | 94.73 (9) |
| O2v—K1—N1iii | 94.09 (4) | N2—N1—K1viii | 142.32 (10) |
| O4v—K1—N1iii | 80.02 (4) | N3—N1—K1vii | 124.19 (10) |
| O4—K1—O2 | 50.33 (4) | N2—N1—K1vii | 84.51 (9) |
| O3i—K1—O2 | 68.74 (4) | K1viii—N1—K1vii | 99.45 (4) |
| O1ii—K1—O2 | 64.58 (4) | O4—N3—O3 | 121.17 (14) |
| O3iii—K1—O2 | 152.97 (4) | O4—N3—N1 | 125.71 (13) |
| O4i—K1—O2 | 105.20 (4) | O3—N3—N1 | 112.98 (13) |
| O1iv—K1—O2 | 136.99 (4) | O4—N3—K1vi | 64.01 (8) |
| O2v—K1—O2 | 96.15 (4) | O3—N3—K1vi | 58.63 (8) |
| O4v—K1—O2 | 69.47 (3) | N1—N3—K1vi | 161.65 (10) |
| N1iii—K1—O2 | 129.58 (4) | O4—N3—K1viii | 171.18 (11) |
| O4—K1—N3i | 96.09 (4) | O3—N3—K1viii | 51.55 (8) |
| O3i—K1—N3i | 22.20 (3) | N1—N3—K1viii | 62.16 (8) |
| O1ii—K1—N3i | 75.46 (4) | K1vi—N3—K1viii | 109.76 (4) |
| O3iii—K1—N3i | 118.48 (4) | N3—O3—K1vi | 99.17 (9) |
| O4i—K1—N3i | 22.29 (3) | N3—O3—K1viii | 108.40 (9) |
| O1iv—K1—N3i | 74.16 (3) | K1vi—O3—K1viii | 151.25 (5) |
| O2v—K1—N3i | 168.32 (4) | | |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Crystal data top
| KN3O4 | F(000) = 288 |
| Mr = 145.13 | Dx = 2.199 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| a = 6.6162 (2) Å | Cell parameters from 2568 reflections |
| b = 9.2831 (2) Å | θ = 5.0–27.9° |
| c = 7.2000 (3) Å | µ = 1.13 mm−1 |
| β = 97.583 (1)° | T = 298 K |
| V = 438.35 (2) Å3 | 0.34 × 0.14 × 0.08 mm |
| Z = 4 | |
Data collection top
Platform
diffractometer | 1084 independent reflections |
| Radiation source: Sealed Tube | 854 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.057 |
| ω scans | θmax = 28.3°, θmin = 3.6° |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | h = −8→7 |
| Tmin = 0.283, 0.231297, 0.279919, 0.867434, 0.000387, 0.319426, 0.255290, 0.282944, Tmax = 0.990, 0.830643, 0.977935, 3.122036, 0.219526, 1.116071, 0.904643, 0.990283 | k = −12→12 |
| 3648 measured reflections | l = −8→9 |
Refinement top
| 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) = 0.100 | Calculated w = 1/[σ2(Fo2) + (0.0528P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 0.98 | (Δ/σ)max < 0.001 |
| 1084 reflections | Δρmax = 0.43 e Å−3 |
| 73 parameters | Δρmin = −0.38 e Å−3 |
Crystal data top
| KN3O4 | V = 438.35 (2) Å3 |
| Mr = 145.13 | Z = 4 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.6162 (2) Å | µ = 1.13 mm−1 |
| b = 9.2831 (2) Å | T = 298 K |
| c = 7.2000 (3) Å | 0.34 × 0.14 × 0.08 mm |
| β = 97.583 (1)° | |
Data collection top
Platform
diffractometer | 1084 independent reflections |
Absorption correction: empirical :Multipole Expansion (Blessing, 1995)
? | 854 reflections with I > 2σ(I) |
| Tmin = 0.283, 0.231297, 0.279919, 0.867434, 0.000387, 0.319426, 0.255290, 0.282944, Tmax = 0.990, 0.830643, 0.977935, 3.122036, 0.219526, 1.116071, 0.904643, 0.990283 | Rint = 0.057 |
| 3648 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.039 | 73 parameters |
| wR(F2) = 0.100 | 0 restraints |
| S = 0.98 | Δρmax = 0.43 e Å−3 |
| 1084 reflections | Δρmin = −0.38 e Å−3 |
Special details top
Experimental. The decay correction was applied simultaneously with the absorption correction
in SADABS. No formal measure of the extent of decay is printed out by
this program. The final unit cell is obtained from the refinement of the XYZ
weighted centroids of reflections above 20 σ(I). |
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 on F2 for ALL reflections except for 0 with very negative
F2 or flagged by the user for potential systematic errors. Weighted
R-factors wR and all goodnesses of fit S are based on
F2, conventional R-factors R are based on F,
with F set to zero for negative F2. The observed criterion of
F2 > σ(F2) is used only for calculating _R_factor_obs
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| | x | y | z | Uiso*/Ueq | |
| K1 | 0.85793 (7) | 0.34205 (5) | 0.82918 (7) | 0.0341 (2) | |
| O4 | 1.0067 (3) | 0.3452 (2) | 1.2134 (2) | 0.0409 (4) | |
| O2 | 0.7282 (3) | 0.5379 (2) | 1.1588 (3) | 0.0455 (4) | |
| N2 | 0.6491 (3) | 0.4622 (2) | 1.2679 (3) | 0.0321 (4) | |
| O1 | 0.4650 (2) | 0.4611 (2) | 1.2786 (3) | 0.0472 (5) | |
| N1 | 0.7576 (3) | 0.3765 (2) | 1.4044 (3) | 0.0328 (4) | |
| N3 | 0.9470 (3) | 0.3414 (2) | 1.3683 (2) | 0.0279 (4) | |
| O3 | 1.0578 (2) | 0.2952 (2) | 1.5078 (2) | 0.0377 (4) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| K1 | 0.0340 (3) | 0.0406 (3) | 0.0296 (3) | −0.0047 (2) | 0.0113 (2) | 0.0006 (2) |
| O4 | 0.0374 (9) | 0.0612 (11) | 0.0269 (9) | 0.0045 (7) | 0.0148 (7) | 0.0022 (7) |
| O2 | 0.0484 (11) | 0.0407 (9) | 0.0472 (11) | −0.0032 (7) | 0.0053 (8) | 0.0145 (7) |
| N2 | 0.0337 (9) | 0.0285 (9) | 0.0346 (10) | 0.0009 (7) | 0.0065 (8) | −0.0033 (7) |
| O1 | 0.0327 (9) | 0.0525 (10) | 0.0575 (12) | 0.0101 (7) | 0.0100 (8) | −0.0044 (8) |
| N1 | 0.0330 (10) | 0.0364 (10) | 0.0316 (10) | 0.0073 (7) | 0.0146 (8) | 0.0047 (7) |
| N3 | 0.0300 (9) | 0.0294 (9) | 0.0259 (9) | −0.0016 (6) | 0.0102 (7) | −0.0021 (6) |
| O3 | 0.0388 (9) | 0.0458 (9) | 0.0285 (8) | 0.0076 (7) | 0.0042 (7) | 0.0022 (7) |
Geometric parameters (Å, º) top
| K1—O3i | 2.810 (2) | O2—N2 | 1.222 (3) |
| K1—O4 | 2.812 (2) | O2—K1v | 2.947 (2) |
| K1—O1ii | 2.841 (2) | N2—O1 | 1.230 (2) |
| K1—O3iii | 2.846 (2) | N2—N1 | 1.388 (2) |
| K1—O4i | 2.933 (2) | O1—K1ii | 2.841 (2) |
| K1—O1iv | 2.936 (2) | O1—K1vii | 2.936 (2) |
| K1—O2v | 2.947 (2) | N1—N3 | 1.353 (2) |
| K1—N1iii | 3.060 (2) | N1—K1viii | 3.060 (2) |
| K1—O4v | 3.066 (2) | N1—K1vii | 3.320 (2) |
| K1—O2 | 3.196 (2) | N3—O3 | 1.239 (2) |
| K1—N3i | 3.252 (2) | N3—K1vi | 3.251 (2) |
| K1—N1iv | 3.320 (2) | N3—K1viii | 3.446 (2) |
| O4—N3 | 1.232 (2) | O3—K1vi | 2.810 (2) |
| O4—K1vi | 2.933 (2) | O3—K1viii | 2.846 (2) |
| O4—K1v | 3.066 (2) | | |
| | | |
| O3i—K1—O4 | 74.39 (5) | O1iv—K1—N3i | 74.17 (4) |
| O3i—K1—O1ii | 82.25 (5) | O2v—K1—N3i | 168.46 (5) |
| O4—K1—O1ii | 114.53 (5) | N1iii—K1—N3i | 93.89 (5) |
| O3i—K1—O3iii | 137.32 (4) | O4v—K1—N3i | 139.76 (4) |
| O4—K1—O3iii | 131.43 (5) | O2—K1—N3i | 85.63 (4) |
| O1ii—K1—O3iii | 106.85 (5) | O3i—K1—N1iv | 104.12 (5) |
| O3i—K1—O4i | 43.96 (4) | O4—K1—N1iv | 71.22 (4) |
| O4—K1—O4i | 116.55 (5) | O1ii—K1—N1iv | 172.66 (5) |
| O1ii—K1—O4i | 76.38 (5) | O3iii—K1—N1iv | 66.02 (4) |
| O3iii—K1—O4i | 96.55 (5) | O4i—K1—N1iv | 105.56 (5) |
| O3i—K1—O1iv | 79.57 (5) | O1iv—K1—N1iv | 40.05 (4) |
| O4—K1—O1iv | 94.19 (5) | O2v—K1—N1iv | 60.62 (4) |
| O1ii—K1—O1iv | 140.16 (4) | N1iii—K1—N1iv | 106.86 (5) |
| O3iii—K1—O1iv | 66.85 (5) | O4v—K1—N1iv | 110.99 (5) |
| O4i—K1—O1iv | 65.92 (5) | O2—K1—N1iv | 120.85 (5) |
| O3i—K1—O2v | 150.23 (5) | N3i—K1—N1iv | 108.83 (4) |
| O4—K1—O2v | 76.35 (5) | N3—O4—K1 | 141.10 (14) |
| O1ii—K1—O2v | 115.29 (5) | N3—O4—K1vi | 93.57 (12) |
| O3iii—K1—O2v | 63.39 (5) | K1—O4—K1vi | 115.77 (5) |
| O4i—K1—O2v | 158.53 (5) | N3—O4—K1v | 104.52 (12) |
| O1iv—K1—O2v | 97.33 (5) | K1—O4—K1v | 88.87 (5) |
| O3i—K1—N1iii | 115.58 (5) | K1vi—O4—K1v | 111.02 (6) |
| O4—K1—N1iii | 169.78 (5) | N2—O2—K1v | 132.35 (14) |
| O1ii—K1—N1iii | 66.64 (5) | N2—O2—K1 | 109.28 (13) |
| O3iii—K1—N1iii | 42.79 (4) | K1v—O2—K1 | 84.10 (5) |
| O4i—K1—N1iii | 73.66 (5) | O2—N2—O1 | 123.8 (2) |
| O1iv—K1—N1iii | 90.02 (5) | O2—N2—N1 | 124.0 (2) |
| O2v—K1—N1iii | 93.90 (5) | O1—N2—N1 | 112.0 (2) |
| O3i—K1—O4v | 135.12 (5) | N2—O1—K1ii | 133.82 (14) |
| O4—K1—O4v | 91.13 (5) | N2—O1—K1vii | 105.85 (12) |
| O1ii—K1—O4v | 65.33 (5) | K1ii—O1—K1vii | 117.73 (6) |
| O3iii—K1—O4v | 83.70 (5) | N3—N1—N2 | 114.1 (2) |
| O4i—K1—O4v | 139.79 (4) | N3—N1—K1viii | 94.71 (12) |
| O1iv—K1—O4v | 144.76 (5) | N2—N1—K1viii | 142.29 (13) |
| O2v—K1—O4v | 50.37 (5) | N3—N1—K1vii | 124.01 (12) |
| N1iii—K1—O4v | 80.14 (5) | N2—N1—K1vii | 84.75 (11) |
| O3i—K1—O2 | 69.05 (4) | K1viii—N1—K1vii | 99.33 (5) |
| O4—K1—O2 | 49.97 (4) | O4—N3—O3 | 121.2 (2) |
| O1ii—K1—O2 | 64.58 (5) | O4—N3—N1 | 125.6 (2) |
| O3iii—K1—O2 | 152.87 (5) | O3—N3—N1 | 113.1 (2) |
| O4i—K1—O2 | 105.53 (5) | O4—N3—K1vi | 64.21 (11) |
| O1iv—K1—O2 | 136.90 (5) | O3—N3—K1vi | 58.48 (10) |
| O2v—K1—O2 | 95.90 (5) | N1—N3—K1vi | 161.67 (12) |
| N1iii—K1—O2 | 129.70 (4) | O4—N3—K1viii | 171.05 (14) |
| O4v—K1—O2 | 69.28 (4) | O3—N3—K1viii | 51.55 (10) |
| O3i—K1—N3i | 22.09 (4) | N1—N3—K1viii | 62.25 (10) |
| O4—K1—N3i | 96.21 (5) | K1vi—N3—K1viii | 109.61 (5) |
| O1ii—K1—N3i | 75.71 (5) | N3—O3—K1vi | 99.44 (12) |
| O3iii—K1—N3i | 118.29 (5) | N3—O3—K1viii | 108.51 (12) |
| O4i—K1—N3i | 22.22 (4) | K1vi—O3—K1viii | 150.91 (6) |
| Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z+1/2; (viii) x, y, z+1. |
Experimental details
| | (kdn85) | (kdn100) | (kdn150) | (kdn200) |
| Crystal data |
| Chemical formula | KN3O4 | KN3O4 | KN3O4 | KN3O4 |
| Mr | 145.13 | 145.13 | 145.13 | 145.13 |
| Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
| Temperature (K) | 85 | 100 | 150 | 200 |
| a, b, c (Å) | 6.5891 (4), 9.0653 (5), 7.1459 (4) | 6.5918 (4), 9.0778 (5), 7.1540 (4) | 6.6010 (3), 9.1253 (5), 7.1657 (4) | 6.6029 (4), 9.1694 (5), 7.1731 (4) |
| β (°) | 97.975 (2) | 97.946 (2) | 97.890 (1) | 97.805 (1) |
| V (Å3) | 422.71 (4) | 423.98 (4) | 427.55 (4) | 430.27 (4) |
| Z | 4 | 4 | 4 | 4 |
| Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
| µ (mm−1) | 1.17 | 1.17 | 1.16 | 1.15 |
| Crystal size (mm) | 0.34 × 0.14 × 0.08 | 0.34 × 0.14 × 0.08 | 0.34 × 0.14 × 0.08 | 0.34 × 0.14 × 0.08 |
| |
| Data collection |
| Diffractometer | Platform
diffractometer | Platform
diffractometer | Platform
diffractometer | Platform
diffractometer |
| Absorption correction | Empirical :Multipole Expansion (Blessing, 1995) | Empirical :Multipole Expansion (Blessing, 1995) | Empirical: Multipole Expansion (Blessing, 1995) | Empirical :Multipole Expansion (Blessing, 1995) |
| Tmin, Tmax | 0.791, 0.990 | 0.768, 0.990 | 0.780, 0.990 | 0.723, 0.990 |
No. of measured, independent and
observed [I > 2σ(I)] reflections | 3515, 1034, 902 | 3547, 1041, 918 | 3517, 1046, 917 | 3510, 1060, 911 |
| Rint | 0.048 | 0.046 | 0.040 | 0.040 |
| (sin θ/λ)max (Å−1) | 0.668 | 0.668 | 0.667 | 0.667 |
| |
| Refinement |
| R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.075, 1.02 | 0.029, 0.068, 1.00 | 0.030, 0.072, 1.04 | 0.032, 0.077, 1.00 |
| No. of reflections | 1034 | 1041 | 1046 | 1060 |
| No. of parameters | 73 | 73 | 73 | 73 |
| Δρmax, Δρmin (e Å−3) | 0.55, −0.60 | 0.53, −0.60 | 0.36, −0.39 | 0.36, −0.35 |
| | (kdn250) | (kdn298) |
| Crystal data |
| Chemical formula | KN3O4 | KN3O4 |
| Mr | 145.13 | 145.13 |
| Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n |
| Temperature (K) | 250 | 298 |
| a, b, c (Å) | 6.6114 (1), 9.2299 (2), 7.1878 (2) | 6.6162 (2), 9.2831 (2), 7.2000 (3) |
| β (°) | 97.639 (1) | 97.583 (1) |
| V (Å3) | 434.73 (2) | 438.35 (2) |
| Z | 4 | 4 |
| Radiation type | Mo Kα | Mo Kα |
| µ (mm−1) | 1.14 | 1.13 |
| Crystal size (mm) | 0.34 × 0.14 × 0.08 | 0.34 × 0.14 × 0.08 |
| |
| Data collection |
| Diffractometer | Platform
diffractometer | Platform
diffractometer |
| Absorption correction | Empirical :Multipole Expansion (Blessing, 1995) | Empirical :Multipole Expansion (Blessing, 1995) |
| Tmin, Tmax | 0.685, 0.990 | 0.283, 0.231297, 0.279919, 0.867434, 0.000387, 0.319426, 0.255290, 0.282944, 0.990, 0.830643, 0.977935, 3.122036, 0.219526, 1.116071, 0.904643, 0.990283 |
No. of measured, independent and
observed [I > 2σ(I)] reflections | 3613, 1073, 882 | 3648, 1084, 854 |
| Rint | 0.045 | 0.057 |
| (sin θ/λ)max (Å−1) | 0.668 | 0.667 |
| |
| Refinement |
| R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.081, 1.00 | 0.039, 0.100, 0.98 |
| No. of reflections | 1073 | 1084 |
| No. of parameters | 73 | 73 |
| Δρmax, Δρmin (e Å−3) | 0.31, −0.43 | 0.43, −0.38 |
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![[Figure 1]](http://journals.iucr.org/b/issues/2001/02/00/br0101/br0101fig1thm.gif)
![[Figure 2]](http://journals.iucr.org/b/issues/2001/02/00/br0101/br0101fig2thm.gif)
![[Figure 3]](http://journals.iucr.org/b/issues/2001/02/00/br0101/br0101fig3thm.gif)
![[Figure 4]](http://journals.iucr.org/b/issues/2001/02/00/br0101/br0101fig4thm.gif)
![[Figure 5]](http://journals.iucr.org/b/issues/2001/02/00/br0101/br0101fig5thm.gif)
