Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802012564/ya6107sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536802012564/ya6107Isup2.rtv |
CCDC reference: 193774
Data collection: local program; data reduction: local program; program(s) used to solve structure: MRIA (Zlokazov & Chernyshev, 1992); program(s) used to refine structure: MRIA; molecular graphics: PCMODEL (Version 7.0) [Reference?]; software used to prepare material for publication: MRIA and PARST (Nardelli, 1983).
C9H7NO·2H2O | F(000) = 384 |
Mr = 181.19 | Dx = 1.285 Mg m−3 |
Monoclinic, P21/n | Melting point: 51(1) K |
a = 9.484 (3) Å | Cu Kα radiation, λ = 1.5418 Å |
b = 16.235 (5) Å | T = 293 K |
c = 6.907 (2) Å | Particle morphology: no specific habit |
β = 118.25 (2)° | light grey |
V = 936.8 (5) Å3 | flat_sheet, 12 × 12 mm |
Z = 4 |
X-ray powder diffractometer DRON-4.07 | Data collection mode: reflection |
Radiation source: BSV-28, line-focus sealed tube | Scan method: step |
Pyrolitic graphite crystal monochromator | 2θmin = 10°, 2θmax = 60°, 2θstep = 0.02° |
Specimen mounting: The powder was sprinkled on the sample holder. |
Refinement on Inet | 126 parameters |
Least-squares matrix: full with fixed elements per cycle | 1 constraint |
Rp = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
Rwp = 0.040 | Weighting scheme based on measured s.u.'s |
Rexp = 0.012 | (Δ/σ)max = 0.02 |
2501 data points | Background function: Chebyshev polynomial up to the 5th order' |
Profile function: split-type pseudo-Voigt (Toraya, 1986) | Preferred orientation correction: Spherical harmonics expansion (Ahtee et al., 1989) up to the 6th order. |
Experimental. specimen was rotated in its plane |
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 | ||
C1 | −0.0298 (9) | −0.0533 (3) | 0.2292 (13) | 0.143 (4)* | |
C2 | −0.2676 (5) | 0.0249 (3) | 0.0699 (6) | 0.056 (3)* | |
C3 | −0.0121 (8) | 0.0980 (3) | 0.2405 (11) | 0.100 (3)* | |
C4 | 0.2258 (6) | 0.0126 (3) | 0.3986 (9) | 0.080 (4)* | |
C5 | 0.2409 (11) | 0.1629 (5) | 0.4134 (15) | 0.160 (4)* | |
O6 | 0.0141 (6) | 0.2410 (3) | 0.2452 (9) | 0.119 (2)* | |
C7 | −0.1906 (6) | −0.0485 (3) | 0.1189 (9) | 0.102 (3)* | |
C8 | −0.1796 (8) | 0.0981 (3) | 0.1177 (11) | 0.158 (4)* | |
C9 | 0.0664 (6) | 0.0207 (3) | 0.2929 (9) | 0.099 (4)* | |
C10 | 0.3182 (7) | 0.0853 (4) | 0.4675 (11) | 0.150 (3)* | |
N11 | 0.0828 (6) | 0.1714 (3) | 0.3009 (9) | 0.144 (3)* | |
H1 | 0.0200 | −0.1040 | 0.2702 | 0.051* | |
H2 | −0.3797 | 0.0279 | −0.0154 | 0.051* | |
H4 | 0.2761 | −0.0379 | 0.4423 | 0.051* | |
H5 | 0.3049 | 0.2106 | 0.4562 | 0.051* | |
H7 | −0.2514 | −0.0986 | 0.0830 | 0.051* | |
H8 | −0.2343 | 0.1475 | 0.0809 | 0.051* | |
H10 | 0.4296 | 0.0816 | 0.5447 | 0.051* | |
OW1 | −0.0545 (3) | 0.2796 (2) | 0.5565 (4) | 0.039 (2)* | |
OW2 | 0.1435 (5) | 0.2862 (2) | −0.0136 (7) | 0.118 (2)* |
O6—N11 | 1.269 (7) | C3—C8 | 1.403 (9) |
N11—C3 | 1.431 (7) | C4—C9 | 1.338 (7) |
N11—C5 | 1.33 (1) | C4—C10 | 1.412 (8) |
O6—OW1 | 2.601 (7) | C5—C10 | 1.42 (1) |
O6—OW2 | 2.705 (8) | C1—H1 | 0.92 |
OW1—OW2i | 2.660 (9) | C2—H2 | 0.94 |
OW1—OW2ii | 2.875 (9) | C8—H8 | 0.92 |
C1—C7 | 1.346 (9) | C4—H4 | 0.92 |
C1—C9 | 1.445 (8) | C10—H10 | 0.93 |
C2—C7 | 1.354 (7) | C5—H5 | 0.94 |
C2—C8 | 1.399 (7) | C7—H7 | 0.94 |
C3—N11—O6 | 119.4 (5) | C7—C1—H1 | 120 |
C5—N11—O6 | 123.0 (7) | C7—C2—H2 | 121 |
C3—N11—C5 | 117.6 (7) | C8—C2—H2 | 118 |
N11—C5—C10 | 123.1 (8) | C9—C4—H4 | 123 |
C5—C10—C4 | 119.6 (6) | C10—C4—H4 | 119 |
C10—C4—C9 | 117.6 (6) | N11—C5—H5 | 119 |
C4—C9—C3 | 123.2 (6) | C10—C5—H5 | 118 |
C9—C1—C7 | 120.5 (6) | C1—C7—H7 | 119 |
C1—C7—C2 | 121.7 (5) | C2—C7—H7 | 120 |
C7—C2—C8 | 119.8 (5) | C2—C8—H8 | 119 |
C2—C8—C3 | 121.3 (6) | C3—C8—H8 | 120 |
C8—C3—C9 | 117.6 (6) | C4—C10—H10 | 120 |
C3—C9—C1 | 118.6 (4) | C5—C10—H10 | 121 |
C9—C1—H1 | 119 |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, z+1/2. |