Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614014498/ps5035sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614014498/ps5035Isup2.hkl | |
Text file https://doi.org/10.1107/S2052520614014498/ps5035sup3.txt | |
Zip compressed file https://doi.org/10.1107/S2052520614014498/ps5035sup4.zip | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614014498/ps5035sup5.pdf |
CCDC reference: 1009312
Data collection: Bruker APEX2 v2011.4-0; cell refinement: Bruker APEX2 v2011.4-0; data reduction: Bruker SAINT V7.60A; program(s) used to solve structure: Sir2011; program(s) used to refine structure: SHELXL2012 (Sheldrick, 2012); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.
C3H7NO2 | Dx = 1.405 Mg m−3 |
Mr = 89.10 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 7420 reflections |
a = 5.7890 (8) Å | θ = 7.5–62.4° |
b = 5.9387 (7) Å | µ = 0.12 mm−1 |
c = 12.2516 (14) Å | T = 100 K |
V = 421.20 (9) Å3 | Block, colourless |
Z = 4 | 0.4 × 0.4 × 0.3 mm |
F(000) = 192 |
Kappa 4-axis goniometer bruker-nonius diffractometer | 6425 independent reflections |
Radiation source: Rotating anode X-ray tube, Bruker-Nonius FR 591 | 6209 reflections with I > 2σ(I) |
Multilayer Montel 200 mirrors monochromator | Rint = 0.026 |
Detector resolution: 512 pixels mm-1 | θmax = 62.7°, θmin = 7.5° |
Fullsphere data collection, phi and ω scans | h = −13→12 |
Absorption correction: empirical (using intensity measurements) SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 | k = −14→14 |
Tmin = 0.743, Tmax = 0.966 | l = −30→30 |
31341 measured reflections |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.025 | w = 1/[σ2(Fo2) + (0.040P)2 + 0.0029P]
where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.066 | (Δ/σ)max = 0.002 |
S = 1.18 | Δρmax = 0.49 e Å−3 |
6425 reflections | Δρmin = −0.23 e Å−3 |
55 parameters | Absolute structure: Flack x determined using 2644 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). |
0 restraints | Absolute structure parameter: 0.05 (8) |
C3H7NO2 | V = 421.20 (9) Å3 |
Mr = 89.10 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 5.7890 (8) Å | µ = 0.12 mm−1 |
b = 5.9387 (7) Å | T = 100 K |
c = 12.2516 (14) Å | 0.4 × 0.4 × 0.3 mm |
Kappa 4-axis goniometer bruker-nonius diffractometer | 6425 independent reflections |
Absorption correction: empirical (using intensity measurements) SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 | 6209 reflections with I > 2σ(I) |
Tmin = 0.743, Tmax = 0.966 | Rint = 0.026 |
31341 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | H-atom parameters not refined |
wR(F2) = 0.066 | Δρmax = 0.49 e Å−3 |
S = 1.18 | Δρmin = −0.23 e Å−3 |
6425 reflections | Absolute structure: Flack x determined using 2644 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). |
55 parameters | Absolute structure parameter: 0.05 (8) |
0 restraints |
Experimental. It should be noted that the e.s.d.'s of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 |
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. |
x | y | z | Uiso*/Ueq | ||
O1 | −0.26127 (4) | 0.94249 (4) | 0.81575 (2) | 0.01282 (3) | |
O2 | −0.12499 (4) | 1.22736 (4) | 0.91615 (2) | 0.01287 (3) | |
N1 | 0.31650 (4) | 1.14850 (3) | 0.86234 (2) | 0.01033 (3) | |
C1 | −0.10016 (4) | 1.05514 (4) | 0.85909 (2) | 0.00919 (3) | |
C2 | 0.14545 (4) | 0.96797 (4) | 0.83885 (2) | 0.00930 (3) | |
C3 | 0.19665 (5) | 0.76231 (5) | 0.90917 (2) | 0.01349 (4) | |
H2 | 0.1624 | 0.9309 | 0.7617 | 0.021* | |
H11 | 0.3067 | 1.1953 | 0.9341 | 0.022* | |
H12 | 0.4527 | 1.0920 | 0.8541 | 0.028* | |
H13 | 0.2945 | 1.2591 | 0.8221 | 0.021* | |
H31 | 0.1957 | 0.8005 | 0.9881 | 0.026* | |
H32 | 0.0848 | 0.6442 | 0.8952 | 0.023* | |
H33 | 0.3491 | 0.7020 | 0.8936 | 0.022* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.00792 (6) | 0.01600 (6) | 0.01453 (6) | −0.00075 (5) | −0.00098 (4) | −0.00346 (5) |
O2 | 0.01146 (7) | 0.01409 (6) | 0.01306 (5) | 0.00160 (5) | 0.00097 (4) | −0.00414 (4) |
N1 | 0.00808 (6) | 0.01183 (5) | 0.01107 (5) | −0.00043 (4) | −0.00003 (4) | −0.00042 (4) |
C1 | 0.00762 (6) | 0.01138 (6) | 0.00858 (5) | 0.00061 (4) | 0.00000 (4) | −0.00038 (4) |
C2 | 0.00765 (6) | 0.01098 (6) | 0.00928 (5) | 0.00046 (4) | −0.00003 (4) | −0.00090 (4) |
C3 | 0.01147 (8) | 0.01255 (7) | 0.01646 (8) | 0.00113 (6) | −0.00050 (6) | 0.00241 (6) |
O1—C1 | 1.2647 (3) | C1—C2 | 1.5333 (4) |
O2—C1 | 1.2472 (3) | C2—C3 | 1.5238 (4) |
N1—C2 | 1.4876 (3) | ||
O2—C1—O1 | 125.75 (2) | N1—C2—C3 | 109.81 (2) |
O2—C1—C2 | 118.32 (2) | N1—C2—C1 | 110.04 (2) |
O1—C1—C2 | 115.93 (2) | C3—C2—C1 | 111.07 (2) |
O2—C1—C2—N1 | −18.27 (3) | O2—C1—C2—C3 | 103.54 (3) |
O1—C1—C2—N1 | 162.01 (2) | O1—C1—C2—C3 | −76.19 (3) |
Experimental details
Crystal data | |
Chemical formula | C3H7NO2 |
Mr | 89.10 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 100 |
a, b, c (Å) | 5.7890 (8), 5.9387 (7), 12.2516 (14) |
V (Å3) | 421.20 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.12 |
Crystal size (mm) | 0.4 × 0.4 × 0.3 |
Data collection | |
Diffractometer | Kappa 4-axis goniometer bruker-nonius diffractometer |
Absorption correction | Empirical (using intensity measurements) SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 |
Tmin, Tmax | 0.743, 0.966 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31341, 6425, 6209 |
Rint | 0.026 |
(sin θ/λ)max (Å−1) | 1.250 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.066, 1.18 |
No. of reflections | 6425 |
No. of parameters | 55 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.49, −0.23 |
Absolute structure | Flack x determined using 2644 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). |
Absolute structure parameter | 0.05 (8) |
Computer programs: Bruker APEX2 v2011.4-0, Bruker SAINT V7.60A, Sir2011, SHELXL2012 (Sheldrick, 2012), Bruker SHELXTL.