Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108767304015120/xc5013sup1.cif | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767304015120/xc5013sup2.pdf | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767304015120/xc5013sup3.pdf | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767304015120/xc5013sup4.pdf | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767304015120/xc5013sup5.pdf | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767304015120/xc5013sup6.pdf | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108767304015120/xc5013Isup7.hkl |
CCDC reference: 1047783
Data collection: KM6-CH software; cell refinement: KM6-CH software; data reduction: XD_RED; program(s) used to refine structure: VALRAY.
CH4N2O | F(000) = 64 |
Mr = 60.06 | Dx = 1.368 Mg m−3 |
Tetragonal, P421m | Synchrotron radiation, λ = 0.5996 (1) Å |
Hall symbol: P -4 2ab | Cell parameters from 17 reflections |
a = 5.5780 (6) Å | T = 123 K |
c = 4.6860 (7) Å | Block, colourless |
V = 145.80 (3) Å3 | 0.23 × 0.13 × 0.09 mm |
Z = 2 |
KM6-CH six-circle κ diffractometer operated as standard four-circle κ diffractometer with detector circle in the vertical plane to profit from the linear polarization of the synchrotron beam. | 817 reflections with I > 2σ(I) |
Radiation source: bending magnet | Rint = 0.014 |
Si(111) double crystal monochromator | θmax = 59.8°, θmin = 3.7° |
ω–scan | h = −15→15 |
3942 measured reflections | k = −15→0 |
1045 independent reflections | l = −13→0 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
wR(F2) = 0.010 | Hydrogen site location: inferred from neighbouring sites |
S = 1.17 | All H-atom parameters refined |
1045 reflections | w = 1/[σ2(Fo2] |
77 parameters | (Δ/σ)max < 0.001 |
0 restraints |
CH4N2O | V = 145.80 (3) Å3 |
Mr = 60.06 | Z = 2 |
Tetragonal, P421m | Synchrotron radiation, λ = 0.5996 (1) Å |
a = 5.5780 (6) Å | T = 123 K |
c = 4.6860 (7) Å | 0.23 × 0.13 × 0.09 mm |
KM6-CH six-circle κ diffractometer operated as standard four-circle κ diffractometer with detector circle in the vertical plane to profit from the linear polarization of the synchrotron beam. | 817 reflections with I > 2σ(I) |
3942 measured reflections | Rint = 0.014 |
1045 independent reflections |
wR(F2) = 0.010 | 77 parameters |
S = 1.17 | 0 restraints |
1045 reflections | All H-atom parameters refined |
Refinement. Charge density refinement. H positional and displacement parameters fixed at values from neutron study (Swaminathan et al. (1984) Acta Cryst. B40, 300–306. |
x | y | z | Uiso*/Ueq | ||
C | 0.0 | 0.5 | 0.32821 (3) | 0.01238 (2) | |
O | 0.0 | 0.5 | 0.59634 (10) | 0.01527 (2) | |
N | 0.14468 (7) | 0.64468 (7) | 0.17901 (10) | 0.02273 (3) | |
H1 | 0.2557 (4) | 0.7557 (4) | 0.2841 (4) | 0.0365 (6) | |
H2 | 0.1431 (4) | 0.6431 (4) | −0.0348 (3) | 0.0333 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
O | 0.01958 (4) | 0.01958 (4) | 0.00665 (3) | 0.00164 (8) | 0.000 | 0.000 |
C | 0.01519 (4) | 0.01519 (4) | 0.00675 (4) | −0.00035 (6) | 0.000 | 0.000 |
N | 0.02931 (6) | 0.02931 (6) | 0.00956 (4) | −0.01570 (7) | 0.00002 (3) | 0.00002 (3) |
H1 | 0.0440 (11) | 0.0440 (11) | 0.0216 (7) | −0.0222 (8) | −0.0031 (9) | −0.0031 (9) |
H2 | 0.0430 (10) | 0.0430 (10) | 0.0140 (6) | −0.0158 (8) | 0.0019 (8) | 0.0019 (8) |
O—C | 1.2565 (5) | N—H1 | 1.005 (2) |
C—N | 1.3384 (4) | N—H2 | 1.0020 (15) |
O—C—N | 121.49 (2) | C—N—H2 | 120.78 (13) |
C—N—H1 | 119.16 (12) | H1—N—H2 | 120.06 (17) |
Experimental details
Crystal data | |
Chemical formula | CH4N2O |
Mr | 60.06 |
Crystal system, space group | Tetragonal, P421m |
Temperature (K) | 123 |
a, c (Å) | 5.5780 (6), 4.6860 (7) |
V (Å3) | 145.80 (3) |
Z | 2 |
Radiation type | Synchrotron, λ = 0.5996 (1) Å |
µ (mm−1) | ? |
Crystal size (mm) | 0.23 × 0.13 × 0.09 |
Data collection | |
Diffractometer | KM6-CH six-circle κ diffractometer operated as standard four-circle κ diffractometer with detector circle in the vertical plane to profit from the linear polarization of the synchrotron beam. |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3942, 1045, 817 |
Rint | 0.014 |
(sin θ/λ)max (Å−1) | 1.442 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | ?, 0.010, 1.17 |
No. of reflections | 1045 |
No. of parameters | 77 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | ?, ? |
Computer programs: KM6-CH software, XD_RED, VALRAY.