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The crystal structure of β-glycine, C2H5NO2, has been refined. Single crystals of the metastable β-polymorph of glycine were obtained by cooling a saturated solution of glycine containing acetic acid. The crystal of the β-polymorph was preserved in dry air for several months. As the humidity of the air increased, a polymorphic transformation into the α-form was observed. The cell parameters of β-glycine have already been determined by Kozhin [Kristallografiya (1978), 23, 1211–1215], but the coordinates have not been published so far.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680200836X/bt6144sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680200836X/bt6144Isup2.hkl
Contains datablock I

CCDC reference: 189379

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](C-C) = 0.001 Å
  • R factor = 0.025
  • wR factor = 0.076
  • Data-to-parameter ratio = 13.3

checkCIF results

No syntax errors found


Amber Alert Alert Level B:
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 80 Perc Fit PLAT_113 Alert B ADDSYM suggests Pseudo/New Spacegroup ........ P21/m
Author response: See response to previous problem (see _publ_section_exptl_refinement).
General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 37.52 From the CIF: _reflns_number_total 894 Count of symmetry unique reflns 894 Completeness (_total/calc) 100.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: STADI4 (Stoe & Cie, 1997); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-STEP (Stoe & Cie, 1998) and Pcw (Kraus & Nolze, 1999); software used to prepare material for publication: SHELXL97.

aminoacetic acid top
Crystal data top
C2H5NO2F(000) = 80
Mr = 75.07Dx = 1.576 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71069 Å
a = 5.0935 (11) ÅCell parameters from 26 reflections
b = 6.274 (2) Åθ = 15.1–24.7°
c = 5.3847 (12) ŵ = 0.14 mm1
β = 113.19 (2)°T = 294 K
V = 158.18 (8) Å3Prism, colourless
Z = 20.5 × 0.4 × 0.2 mm
Data collection top
Stoe STADI4 four-circle
diffractometer
823 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.039
Planar graphite monochromatorθmax = 37.5°, θmin = 3.3°
Scan width (ω) = 1.42° – 1.87°, scan ratio 2θ:ω = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987)h = 88
Absorption correction: ψ scan
(X-RED; Stoe, 1998)
k = 1010
Tmin = 0.909, Tmax = 0.998l = 99
6548 measured reflections2 standard reflections every 180 min
894 independent reflections intensity decay: 4.3%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025All H-atom parameters refined
wR(F2) = 0.076 w = 1/[σ2(Fo2) + (0.0501P)2 + 0.0031P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
894 reflectionsΔρmax = 0.29 e Å3
67 parametersΔρmin = 0.18 e Å3
1 restraintExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.58 (7)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.09265 (13)0.40990 (13)0.59741 (13)0.02586 (16)
N10.35024 (16)0.28161 (13)0.23730 (13)0.02090 (14)
H30.349 (4)0.301 (3)0.071 (3)0.029 (4)*
H40.520 (4)0.324 (3)0.353 (4)0.029 (4)*
H50.340 (4)0.142 (4)0.266 (3)0.034 (4)*
C10.13352 (15)0.38405 (13)0.56103 (15)0.01851 (13)
O20.37739 (15)0.35815 (17)0.74274 (12)0.0298 (2)
C20.11150 (17)0.39417 (16)0.26993 (14)0.02195 (15)
H10.123 (4)0.538 (4)0.222 (4)0.035 (5)*
H20.063 (4)0.332 (3)0.143 (4)0.029 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0234 (3)0.0326 (4)0.0268 (3)0.0000 (2)0.0154 (2)0.0038 (2)
N10.0218 (3)0.0272 (3)0.0151 (2)0.0026 (2)0.0087 (2)0.0000 (2)
C10.0204 (3)0.0210 (3)0.0163 (2)0.0023 (3)0.0096 (2)0.0014 (2)
O20.0208 (2)0.0532 (5)0.0156 (2)0.0029 (3)0.00725 (19)0.0007 (3)
C20.0232 (3)0.0286 (4)0.0151 (3)0.0055 (3)0.0087 (2)0.0023 (3)
Geometric parameters (Å, º) top
O1—C11.2528 (9)C1—O21.2529 (11)
N1—C21.4753 (11)C1—C21.5281 (11)
N1—H30.899 (16)C2—H10.95 (3)
N1—H40.88 (2)C2—H20.964 (18)
N1—H50.89 (3)
C2—N1—H3111.6 (12)O2—C1—C2117.15 (7)
C2—N1—H4113.3 (12)N1—C2—C1111.79 (6)
H3—N1—H4106.5 (16)N1—C2—H1106.4 (10)
C2—N1—H5110.1 (11)C1—C2—H1109.3 (11)
H3—N1—H5109.1 (17)N1—C2—H2107.2 (11)
H4—N1—H5106.1 (17)C1—C2—H2112.6 (11)
O1—C1—O2125.78 (8)H1—C2—H2109.4 (16)
O1—C1—C2117.03 (7)
O1—C1—C2—N1157.41 (8)O2—C1—C2—N125.03 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H4···O1i0.88 (2)1.97 (2)2.8509 (13)176.6 (17)
N1—H3···O2ii0.899 (16)1.866 (16)2.7626 (11)174.4 (17)
N1—H5···O2iii0.89 (3)2.30 (2)2.9795 (15)132.6 (14)
N1—H5···O1iv0.89 (3)2.23 (2)2.9785 (13)140.7 (16)
Symmetry codes: (i) x+1, y, z; (ii) x, y, z1; (iii) x+1, y1/2, z+1; (iv) x, y1/2, z+1.
 

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