Download citation
Download citation
link to html
A pseudo single crystal (a composite of matrix resin and powder crystallites, wherein the individual crystallites are aligned three-dimensionally) was prepared from a powder of sucrose, and its X-ray diffraction pattern was studied. A powder of sucrose crystals suspended in a UV-curable resin precursor was subjected to magnetic alignment in order to align the individual crystallites three-dimensionally, and then the resin precursor was photopolymerized to maintain this orientation. The pseudo single crystal thus obtained produced a well resolved X-ray diffraction profile that is similar to that produced by a twin crystal. The origin of the twin orientation was explained in terms of the interplay between the symmetry of magnetic susceptibility axes and the crystal symmetry (point group 2) of sucrose. The crystal structure of sucrose solved using the pseudo single crystal was in excellent agreement with that solved using a single crystal.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889809048006/db5068sup1.cif
Contains datablocks General, _kimura_again

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889809048006/db5068sup2.hkl
Contains datablock _kimura_again

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889809048006/db5068sup3.pdf
X-ray measurements

CCDC reference: 775215

Comment top

ENTER TEXT

Experimental top

ENTER COMPOUND PREPARATION DETAILS

Refinement top

ENTER SPECIAL DETAILS OF THE REFINEMENT

Computing details top

Data collection: PROCESS-AUTO; cell refinement: PROCESS-AUTO; data reduction: CrystalStructure; program(s) used to solve structure: SIR92; program(s) used to refine structure: CRYSTALS; software used to prepare material for publication: CrystalStructure 3.8.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
ENTER FIGURE CAPTIONS
(_kimura_again) top
Crystal data top
C12H22O11F(000) = 364.00
Mr = 342.30Dx = 1.583 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71075 Å
Hall symbol: P 2ybCell parameters from 9286 reflections
a = 7.7735 (12) Åθ = 3.0–27.6°
b = 8.7169 (13) ŵ = 0.14 mm1
c = 10.8765 (17) ÅT = 293 K
β = 102.936 (4)°Block, colorless
V = 718.29 (19) Å30.80 × 0.80 × 0.80 mm
Z = 2
Data collection top
Rigaku RAXIS-RAPID
diffractometer
531 reflections with F2 > 2.0σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.166
ω scansθmax = 27.5°
Absorption correction: multi-scan
Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.
h = 1010
Tmin = 0.054, Tmax = 0.893k = 1111
15524 measured reflectionsl = 1414
1730 independent reflections
Refinement top
Refinement on F2All H-atom parameters refined
R[F2 > 2σ(F2)] = 0.079 w = 1/[0.0004Fo2 + 1.0000σ(Fo2)]/(4Fo2)
wR(F2) = 0.173(Δ/σ)max < 0.001
S = 1.01Δρmax = 0.87 e Å3
1730 reflectionsΔρmin = 0.78 e Å3
230 parameters
Crystal data top
C12H22O11V = 718.29 (19) Å3
Mr = 342.30Z = 2
Monoclinic, P21Mo Kα radiation
a = 7.7735 (12) ŵ = 0.14 mm1
b = 8.7169 (13) ÅT = 293 K
c = 10.8765 (17) Å0.80 × 0.80 × 0.80 mm
β = 102.936 (4)°
Data collection top
Rigaku RAXIS-RAPID
diffractometer
1730 independent reflections
Absorption correction: multi-scan
Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.
531 reflections with F2 > 2.0σ(F2)
Tmin = 0.054, Tmax = 0.893Rint = 0.166
15524 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.079230 parameters
wR(F2) = 0.173All H-atom parameters refined
S = 1.01Δρmax = 0.87 e Å3
1730 reflectionsΔρmin = 0.78 e Å3
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O(1)0.7461 (9)0.8285 (9)0.2283 (6)0.055 (2)
O(2)0.6192 (8)1.0306 (8)0.0320 (6)0.051 (2)
O(3)0.3914 (9)0.9212 (7)0.1713 (6)0.050 (2)
O(4)0.0931 (9)1.1657 (8)0.0170 (6)0.061 (2)
O(5)0.3142 (9)1.1739 (9)0.2121 (6)0.058 (2)
O(6)0.2828 (9)0.7237 (9)0.5800 (7)0.063 (2)
O(7)0.0428 (9)1.0289 (9)0.3237 (6)0.066 (2)
O(8)0.3707 (9)0.8661 (7)0.3784 (6)0.050 (2)
O(9)0.6975 (10)0.5227 (8)0.3042 (7)0.061 (2)
O(10)0.2053 (8)0.9446 (7)0.0723 (6)0.057 (2)
O(11)0.3558 (11)0.4497 (8)0.3488 (7)0.072 (3)
C(11)0.1274 (14)1.2027 (11)0.1751 (10)0.049 (3)
C(13)0.6333 (15)0.7885 (12)0.3167 (10)0.051 (3)
C(14)0.2145 (14)1.0718 (11)0.0073 (9)0.044 (3)
C(15)0.5418 (13)1.1406 (13)0.1062 (10)0.059 (4)
C(16)0.3670 (14)1.0722 (12)0.1239 (10)0.045 (3)
C(17)0.5652 (15)0.6319 (14)0.2830 (11)0.056 (4)
C(18)0.0410 (14)1.1855 (10)0.2854 (10)0.052 (3)
C(19)0.0584 (14)1.1027 (13)0.0668 (10)0.053 (3)
C(20)0.2957 (16)0.7145 (12)0.3612 (10)0.054 (3)
C(21)0.4840 (13)0.9119 (14)0.2986 (10)0.055 (3)
C(22)0.1835 (14)0.6960 (13)0.4547 (10)0.059 (4)
C(23)0.4477 (16)0.5989 (12)0.3748 (10)0.057 (4)
H(1)0.11031.30900.14570.057*
H(2)0.70280.79140.40380.061*
H(3)0.22791.16340.04190.056*
H(4)0.62201.15860.18700.072*
H(5)0.52091.23770.06190.072*
H(6)0.49800.62620.19540.068*
H(7)0.07901.22410.26380.062*
H(8)0.10661.24600.35520.062*
H(9)0.02231.00530.09830.062*
H(10)0.22060.70630.27620.064*
H(11)0.53451.01260.32570.066*
H(12)0.13490.59310.44890.072*
H(13)0.08600.76810.43550.072*
H(14)0.51880.60070.46150.071*
H(15)0.01491.02380.39200.082*
H(16)0.10420.93560.11440.067*
H(17)0.84450.85280.26870.067*
H(18)0.72511.02300.06340.062*
H(19)0.05801.21530.07050.074*
H(20)0.38270.68940.58680.077*
H(21)0.77440.54840.36540.074*
H(22)0.40040.39870.30070.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O(1)0.036 (4)0.076 (5)0.055 (5)0.009 (4)0.014 (4)0.008 (4)
O(2)0.033 (4)0.064 (4)0.056 (4)0.008 (4)0.013 (3)0.003 (4)
O(3)0.046 (5)0.047 (4)0.054 (5)0.011 (3)0.005 (4)0.001 (4)
O(4)0.076 (5)0.057 (4)0.053 (5)0.014 (4)0.019 (4)0.005 (4)
O(5)0.038 (4)0.068 (5)0.063 (5)0.000 (4)0.001 (3)0.016 (4)
O(6)0.046 (5)0.080 (5)0.065 (5)0.003 (4)0.018 (4)0.016 (5)
O(7)0.065 (5)0.087 (5)0.054 (5)0.006 (5)0.032 (4)0.011 (5)
O(8)0.053 (5)0.044 (4)0.063 (5)0.001 (3)0.031 (4)0.004 (4)
O(9)0.079 (6)0.043 (4)0.062 (5)0.007 (4)0.018 (4)0.004 (4)
O(10)0.035 (4)0.073 (5)0.059 (5)0.013 (4)0.005 (3)0.021 (4)
O(11)0.108 (7)0.038 (4)0.080 (6)0.024 (5)0.042 (5)0.014 (4)
C(11)0.043 (7)0.041 (7)0.060 (7)0.001 (5)0.002 (6)0.009 (6)
C(13)0.034 (7)0.079 (9)0.040 (7)0.001 (6)0.009 (6)0.005 (6)
C(14)0.050 (7)0.041 (6)0.048 (7)0.007 (5)0.027 (6)0.007 (5)
C(15)0.041 (7)0.069 (8)0.069 (8)0.001 (7)0.015 (6)0.002 (7)
C(16)0.039 (7)0.050 (7)0.051 (7)0.013 (5)0.020 (6)0.008 (6)
C(17)0.053 (8)0.078 (8)0.040 (7)0.010 (7)0.019 (6)0.009 (6)
C(18)0.057 (8)0.036 (6)0.063 (8)0.001 (6)0.015 (6)0.006 (6)
C(19)0.045 (7)0.067 (7)0.044 (6)0.001 (6)0.003 (5)0.010 (6)
C(20)0.062 (8)0.059 (7)0.040 (7)0.005 (7)0.011 (6)0.018 (6)
C(21)0.043 (7)0.080 (8)0.042 (7)0.003 (6)0.011 (6)0.016 (6)
C(22)0.064 (8)0.052 (7)0.063 (8)0.014 (6)0.021 (7)0.007 (6)
C(23)0.062 (8)0.063 (7)0.052 (8)0.021 (7)0.025 (6)0.004 (6)
Geometric parameters (Å, º) top
O(1)—C(13)1.481 (15)C(20)—C(23)1.535 (16)
O(2)—C(15)1.466 (14)O(1)—H(17)0.820
O(3)—C(16)1.411 (12)O(2)—H(18)0.820
O(3)—C(21)1.412 (12)O(4)—H(19)0.820
O(4)—C(19)1.428 (12)O(6)—H(20)0.820
O(5)—C(11)1.439 (12)O(7)—H(15)0.820
O(5)—C(16)1.432 (14)O(9)—H(21)0.820
O(6)—C(22)1.428 (12)O(10)—H(16)0.820
O(7)—C(18)1.426 (12)O(11)—H(22)0.820
O(8)—C(20)1.440 (12)C(11)—H(1)0.980
O(8)—C(21)1.424 (14)C(13)—H(2)0.980
O(9)—C(17)1.382 (14)C(14)—H(3)0.980
O(10)—C(14)1.398 (12)C(15)—H(4)0.970
O(11)—C(23)1.481 (13)C(15)—H(5)0.970
C(11)—C(18)1.508 (17)C(17)—H(6)0.980
C(11)—C(19)1.467 (15)C(18)—H(7)0.970
C(13)—C(17)1.480 (16)C(18)—H(8)0.970
C(13)—C(21)1.562 (16)C(19)—H(9)0.980
C(14)—C(16)1.530 (13)C(20)—H(10)0.980
C(14)—C(19)1.522 (17)C(21)—H(11)0.980
C(15)—C(16)1.535 (16)C(22)—H(12)0.970
C(17)—C(23)1.524 (18)C(22)—H(13)0.970
C(20)—C(22)1.489 (18)C(23)—H(14)0.980
O(1)···O(7)i2.894 (10)H(5)···O(4)i3.359
O(1)···C(14)ii3.467 (13)H(5)···O(10)iii2.773
O(2)···O(4)i2.684 (10)H(5)···H(6)iii2.935
O(2)···C(17)iii3.518 (13)H(5)···H(7)i3.384
O(2)···C(19)i3.408 (13)H(5)···H(16)iii3.324
O(3)···O(4)iv3.378 (9)H(5)···H(18)iii3.245
O(4)···O(2)v2.684 (10)H(5)···H(22)viii3.269
O(4)···O(3)vi3.378 (9)H(6)···O(2)ii2.576
O(4)···O(10)vi2.827 (10)H(6)···O(4)iv3.325
O(4)···C(15)v3.405 (14)H(6)···O(10)ii3.317
O(5)···O(6)vii3.456 (9)H(6)···C(14)ii3.505
O(5)···O(11)viii2.807 (10)H(6)···C(15)ii3.227
O(6)···O(5)ix3.456 (9)H(6)···H(3)ii3.004
O(6)···O(7)x3.402 (11)H(6)···H(5)ii2.935
O(6)···O(9)vii2.884 (10)H(6)···H(18)ii3.091
O(6)···O(11)vii3.377 (10)H(6)···H(19)iv3.474
O(6)···C(15)ix3.457 (13)H(7)···O(2)v3.472
O(6)···C(18)x3.200 (15)H(7)···O(6)xi2.570
O(6)···C(21)ix3.369 (13)H(7)···O(9)xiv3.215
O(7)···O(1)v2.894 (10)H(7)···O(10)vi2.842
O(7)···O(6)xi3.402 (11)H(7)···C(15)v3.145
O(7)···C(22)xi3.595 (14)H(7)···C(22)xi3.348
O(8)···O(11)vii3.322 (10)H(7)···H(4)v2.357
O(8)···C(23)vii3.409 (12)H(7)···H(5)v3.384
O(9)···O(6)ix2.884 (10)H(7)···H(12)xi3.445
O(9)···O(10)ii2.873 (11)H(7)···H(13)xi3.305
O(10)···O(4)iv2.827 (10)H(7)···H(16)vi2.436
O(10)···O(9)iii2.873 (11)H(7)···H(17)v3.293
O(10)···C(11)iv3.330 (12)H(7)···H(18)v2.942
O(10)···C(15)ii3.369 (13)H(7)···H(20)xi3.166
O(10)···C(17)iii3.596 (15)H(7)···H(21)xiv3.328
O(10)···C(18)iv3.486 (11)H(8)···O(6)xi3.263
O(11)···O(5)xii2.807 (10)H(8)···O(11)viii2.640
O(11)···O(6)ix3.377 (10)H(8)···C(22)xi3.412
O(11)···O(8)ix3.322 (10)H(8)···H(2)vii2.735
O(11)···C(11)xii3.139 (12)H(8)···H(12)viii3.184
O(11)···C(18)xii3.318 (12)H(8)···H(12)xi3.411
C(11)···O(10)vi3.330 (12)H(8)···H(13)xi2.997
C(11)···O(11)viii3.139 (12)H(8)···H(14)vii3.386
C(14)···O(1)iii3.467 (13)H(8)···H(16)vi3.218
C(15)···O(4)i3.405 (14)H(8)···H(21)vii3.435
C(15)···O(6)vii3.457 (13)H(8)···H(22)viii2.819
C(15)···O(10)iii3.369 (13)H(9)···O(1)v3.216
C(17)···O(2)ii3.518 (13)H(9)···O(2)v3.062
C(17)···O(10)ii3.596 (15)H(9)···O(4)iv3.173
C(18)···O(6)xi3.200 (15)H(9)···H(1)iv3.131
C(18)···O(10)vi3.486 (11)H(9)···H(3)iv3.537
C(18)···O(11)viii3.318 (12)H(9)···H(17)v2.874
C(19)···O(2)v3.408 (13)H(9)···H(18)v2.261
C(21)···O(6)vii3.369 (13)H(9)···H(19)iv2.569
C(22)···O(7)x3.595 (14)H(10)···O(4)iv2.794
C(23)···O(8)ix3.409 (12)H(10)···H(17)v3.174
O(1)···H(3)ii2.531H(10)···H(19)iv2.311
O(1)···H(5)ii3.459H(11)···O(6)vii2.409
O(1)···H(9)i3.216H(11)···O(11)vii3.494
O(1)···H(13)i3.110H(11)···C(22)vii3.275
O(1)···H(15)i2.961H(11)···C(23)vii3.315
O(1)···H(19)ii3.414H(11)···H(12)vii3.207
O(2)···H(3)ii3.408H(11)···H(14)vii2.559
O(2)···H(5)ii2.872H(11)···H(20)vii1.850
O(2)···H(6)iii2.576H(11)···H(22)viii3.516
O(2)···H(7)i3.472H(12)···O(7)x3.142
O(2)···H(9)i3.062H(12)···O(9)v3.467
O(2)···H(19)i3.374H(12)···C(18)x3.555
O(3)···H(5)ii3.198H(12)···H(2)ix3.189
O(3)···H(19)iv3.142H(12)···H(7)x3.445
O(4)···H(1)iv3.400H(12)···H(8)xii3.184
O(4)···H(4)v3.469H(12)···H(8)x3.411
O(4)···H(5)v3.359H(12)···H(11)ix3.207
O(4)···H(6)vi3.325H(12)···H(15)x2.371
O(4)···H(9)vi3.173H(12)···H(17)v3.475
O(4)···H(10)vi2.794H(12)···H(21)v2.773
O(4)···H(16)vi2.765H(13)···O(1)v3.110
O(4)···H(18)v2.204H(13)···C(13)v3.471
O(5)···H(14)vii3.554H(13)···C(18)x3.471
O(5)···H(20)vii2.836H(13)···H(2)v2.928
O(5)···H(22)viii2.220H(13)···H(7)x3.305
O(6)···H(4)ix2.540H(13)···H(8)x2.997
O(6)···H(7)x2.570H(13)···H(15)x3.054
O(6)···H(8)x3.263H(13)···H(17)v2.416
O(6)···H(11)ix2.409H(13)···H(21)v3.047
O(6)···H(15)x2.966H(13)···H(21)vii3.284
O(6)···H(21)vii2.947H(14)···O(5)ix3.554
O(6)···H(22)vii2.941H(14)···O(8)ix2.699
O(7)···H(4)v3.466H(14)···C(21)ix3.089
O(7)···H(12)xi3.142H(14)···H(8)ix3.386
O(7)···H(17)v2.163H(14)···H(11)ix2.559
O(7)···H(18)v3.315H(15)···O(1)v2.961
O(7)···H(21)vii3.366H(15)···O(6)xi2.966
O(8)···H(14)vii2.699H(15)···O(9)vii3.551
O(8)···H(20)vii3.382H(15)···C(13)v3.548
O(8)···H(22)vii3.557H(15)···C(22)xi2.927
O(9)···H(3)ii3.274H(15)···H(2)v3.185
O(9)···H(4)xii3.422H(15)···H(4)v3.554
O(9)···H(7)xiii3.215H(15)···H(12)xi2.371
O(9)···H(12)i3.467H(15)···H(13)xi3.054
O(9)···H(15)ix3.551H(15)···H(17)v2.231
O(9)···H(16)ii2.939H(15)···H(20)xi3.465
O(9)···H(20)ix3.250H(15)···H(21)vii2.785
O(10)···H(1)iv2.679H(16)···O(4)iv2.765
O(10)···H(4)ii3.213H(16)···O(9)iii2.939
O(10)···H(5)ii2.773H(16)···C(11)iv2.696
O(10)···H(6)iii3.317H(16)···C(18)iv2.924
O(10)···H(7)iv2.842H(16)···C(19)iv3.253
O(10)···H(19)iv2.918H(16)···H(1)iv1.965
O(10)···H(21)iii3.351H(16)···H(4)ii3.427
O(11)···H(1)xii2.853H(16)···H(5)ii3.324
O(11)···H(2)ix3.146H(16)···H(7)iv2.436
O(11)···H(8)xii2.640H(16)···H(8)iv3.218
O(11)···H(11)ix3.494H(16)···H(19)iv2.862
O(11)···H(20)ix3.022H(16)···H(21)iii3.234
C(11)···H(16)vi2.696H(17)···O(7)i2.163
C(11)···H(18)v3.465H(17)···C(18)i3.264
C(11)···H(22)viii2.827H(17)···C(22)i3.242
C(13)···H(3)ii3.568H(17)···H(3)ii2.916
C(13)···H(13)i3.471H(17)···H(7)i3.293
C(13)···H(15)i3.548H(17)···H(9)i2.874
C(14)···H(1)iv3.537H(17)···H(10)i3.174
C(14)···H(6)iii3.505H(17)···H(12)i3.475
C(14)···H(19)iv3.462H(17)···H(13)i2.416
C(15)···H(6)iii3.227H(17)···H(15)i2.231
C(15)···H(7)i3.145H(17)···H(19)ii3.231
C(15)···H(20)vii3.286H(18)···O(4)i2.204
C(15)···H(22)viii3.434H(18)···O(7)i3.315
C(16)···H(20)vii3.463H(18)···C(11)i3.465
C(16)···H(22)viii3.412H(18)···C(18)i3.348
C(17)···H(3)ii3.380H(18)···C(19)i2.675
C(18)···H(4)v3.202H(18)···H(1)ii3.405
C(18)···H(12)xi3.555H(18)···H(3)ii3.171
C(18)···H(13)xi3.471H(18)···H(5)ii3.245
C(18)···H(16)vi2.924H(18)···H(6)iii3.091
C(18)···H(17)v3.264H(18)···H(7)i2.942
C(18)···H(18)v3.348H(18)···H(9)i2.261
C(18)···H(22)viii3.329H(18)···H(19)i2.979
C(19)···H(1)iv3.501H(19)···O(1)iii3.414
C(19)···H(16)vi3.253H(19)···O(2)v3.374
C(19)···H(18)v2.675H(19)···O(3)vi3.142
C(19)···H(19)iv3.378H(19)···O(10)vi2.918
C(20)···H(19)iv3.286H(19)···C(14)vi3.462
C(21)···H(14)vii3.089H(19)···C(19)vi3.378
C(21)···H(20)vii2.811H(19)···C(20)vi3.286
C(22)···H(7)x3.348H(19)···H(6)vi3.474
C(22)···H(8)x3.412H(19)···H(9)vi2.569
C(22)···H(11)ix3.275H(19)···H(10)vi2.311
C(22)···H(15)x2.927H(19)···H(16)vi2.862
C(22)···H(17)v3.242H(19)···H(17)iii3.231
C(22)···H(21)v3.366H(19)···H(18)v2.979
C(23)···H(11)ix3.315H(20)···O(5)ix2.836
H(1)···O(4)vi3.400H(20)···O(8)ix3.382
H(1)···O(10)vi2.679H(20)···O(9)vii3.250
H(1)···O(11)viii2.853H(20)···O(11)vii3.022
H(1)···C(14)vi3.537H(20)···C(15)ix3.286
H(1)···C(19)vi3.501H(20)···C(16)ix3.463
H(1)···H(9)vi3.131H(20)···C(21)ix2.811
H(1)···H(16)vi1.965H(20)···H(2)ix3.539
H(1)···H(18)iii3.405H(20)···H(4)ix2.483
H(1)···H(22)viii2.615H(20)···H(7)x3.166
H(2)···O(11)vii3.146H(20)···H(11)ix1.850
H(2)···H(8)ix2.735H(20)···H(15)x3.465
H(2)···H(12)vii3.189H(20)···H(21)vii3.441
H(2)···H(13)i2.928H(20)···H(22)vii2.597
H(2)···H(15)i3.185H(21)···O(6)ix2.947
H(2)···H(20)vii3.539H(21)···O(7)ix3.366
H(3)···O(1)iii2.531H(21)···O(10)ii3.351
H(3)···O(2)iii3.408H(21)···C(22)i3.366
H(3)···O(9)iii3.274H(21)···H(7)xiii3.328
H(3)···C(13)iii3.568H(21)···H(8)ix3.435
H(3)···C(17)iii3.380H(21)···H(12)i2.773
H(3)···H(6)iii3.004H(21)···H(13)i3.047
H(3)···H(9)vi3.537H(21)···H(13)ix3.284
H(3)···H(17)iii2.916H(21)···H(15)ix2.785
H(3)···H(18)iii3.171H(21)···H(16)ii3.234
H(4)···O(4)i3.469H(21)···H(20)ix3.441
H(4)···O(6)vii2.540H(22)···O(5)xii2.220
H(4)···O(7)i3.466H(22)···O(6)ix2.941
H(4)···O(9)viii3.422H(22)···O(8)ix3.557
H(4)···O(10)iii3.213H(22)···C(11)xii2.827
H(4)···C(18)i3.202H(22)···C(15)xii3.434
H(4)···H(7)i2.357H(22)···C(16)xii3.412
H(4)···H(15)i3.554H(22)···C(18)xii3.329
H(4)···H(16)iii3.427H(22)···H(1)xii2.615
H(4)···H(20)vii2.483H(22)···H(4)xii3.135
H(4)···H(22)viii3.135H(22)···H(5)xii3.269
H(5)···O(1)iii3.459H(22)···H(8)xii2.819
H(5)···O(2)iii2.872H(22)···H(11)xii3.516
H(5)···O(3)iii3.198H(22)···H(20)ix2.597
C(16)—O(3)—C(21)114.2 (8)C(14)—O(10)—H(16)109.3
C(11)—O(5)—C(16)110.1 (7)C(23)—O(11)—H(22)110.1
C(20)—O(8)—C(21)117.7 (8)O(5)—C(11)—H(1)108.1
O(5)—C(11)—C(18)111.2 (8)C(18)—C(11)—H(1)107.6
O(5)—C(11)—C(19)106.6 (9)C(19)—C(11)—H(1)107.5
C(18)—C(11)—C(19)115.6 (9)O(1)—C(13)—H(2)110.1
O(1)—C(13)—C(17)106.7 (9)C(17)—C(13)—H(2)110.6
O(1)—C(13)—C(21)106.7 (8)C(21)—C(13)—H(2)109.7
C(17)—C(13)—C(21)112.9 (9)O(10)—C(14)—H(3)107.7
O(10)—C(14)—C(16)116.0 (8)C(16)—C(14)—H(3)107.1
O(10)—C(14)—C(19)117.9 (8)C(19)—C(14)—H(3)106.3
C(16)—C(14)—C(19)101.0 (8)O(2)—C(15)—H(4)110.2
O(2)—C(15)—C(16)107.4 (8)O(2)—C(15)—H(5)110.0
O(3)—C(16)—O(5)111.6 (8)C(16)—C(15)—H(4)110.8
O(3)—C(16)—C(14)108.5 (7)C(16)—C(15)—H(5)110.3
O(3)—C(16)—C(15)110.9 (8)H(4)—C(15)—H(5)108.1
O(5)—C(16)—C(14)105.8 (8)O(9)—C(17)—H(6)110.0
O(5)—C(16)—C(15)103.8 (8)C(13)—C(17)—H(6)111.8
C(14)—C(16)—C(15)116.1 (9)C(23)—C(17)—H(6)111.1
O(9)—C(17)—C(13)112.5 (9)O(7)—C(18)—H(7)110.4
O(9)—C(17)—C(23)107.1 (9)O(7)—C(18)—H(8)108.9
C(13)—C(17)—C(23)104.2 (10)C(11)—C(18)—H(7)110.4
O(7)—C(18)—C(11)110.5 (8)C(11)—C(18)—H(8)108.6
O(4)—C(19)—C(11)112.7 (9)H(7)—C(18)—H(8)108.0
O(4)—C(19)—C(14)114.8 (9)O(4)—C(19)—H(9)107.2
C(11)—C(19)—C(14)105.3 (8)C(11)—C(19)—H(9)108.4
O(8)—C(20)—C(22)107.0 (9)C(14)—C(19)—H(9)108.2
O(8)—C(20)—C(23)108.0 (9)O(8)—C(20)—H(10)109.1
C(22)—C(20)—C(23)114.8 (9)C(22)—C(20)—H(10)108.7
O(3)—C(21)—O(8)111.4 (7)C(23)—C(20)—H(10)109.0
O(3)—C(21)—C(13)111.4 (9)O(3)—C(21)—H(11)109.0
O(8)—C(21)—C(13)105.9 (9)O(8)—C(21)—H(11)109.1
O(6)—C(22)—C(20)111.0 (9)C(13)—C(21)—H(11)110.0
O(11)—C(23)—C(17)112.0 (9)O(6)—C(22)—H(12)109.7
O(11)—C(23)—C(20)103.3 (8)O(6)—C(22)—H(13)108.9
C(17)—C(23)—C(20)112.0 (9)C(20)—C(22)—H(12)109.5
C(13)—O(1)—H(17)109.2C(20)—C(22)—H(13)109.4
C(15)—O(2)—H(18)108.7H(12)—C(22)—H(13)108.1
C(19)—O(4)—H(19)107.3O(11)—C(23)—H(14)110.0
C(22)—O(6)—H(20)108.9C(17)—C(23)—H(14)109.6
C(18)—O(7)—H(15)109.2C(20)—C(23)—H(14)109.8
C(17)—O(9)—H(21)109.2
C(16)—O(3)—C(21)—O(8)109.5 (10)C(21)—C(13)—C(17)—O(9)177.5 (9)
C(16)—O(3)—C(21)—C(13)132.6 (9)C(21)—C(13)—C(17)—C(23)61.9 (11)
C(21)—O(3)—C(16)—O(5)43.8 (11)O(10)—C(14)—C(16)—O(3)38.4 (13)
C(21)—O(3)—C(16)—C(14)160.0 (9)O(10)—C(14)—C(16)—O(5)158.3 (8)
C(21)—O(3)—C(16)—C(15)71.4 (11)O(10)—C(14)—C(16)—C(15)87.3 (11)
C(11)—O(5)—C(16)—O(3)102.1 (9)O(10)—C(14)—C(19)—O(4)75.0 (11)
C(11)—O(5)—C(16)—C(14)15.6 (11)O(10)—C(14)—C(19)—C(11)160.5 (8)
C(11)—O(5)—C(16)—C(15)138.3 (8)C(16)—C(14)—C(19)—O(4)157.6 (8)
C(16)—O(5)—C(11)—C(18)132.6 (8)C(16)—C(14)—C(19)—C(11)33.0 (10)
C(16)—O(5)—C(11)—C(19)5.8 (11)C(19)—C(14)—C(16)—O(3)90.3 (9)
C(20)—O(8)—C(21)—O(3)65.1 (11)C(19)—C(14)—C(16)—O(5)29.5 (10)
C(20)—O(8)—C(21)—C(13)56.1 (10)C(19)—C(14)—C(16)—C(15)144.0 (9)
C(21)—O(8)—C(20)—C(22)179.8 (6)O(2)—C(15)—C(16)—O(3)51.5 (10)
C(21)—O(8)—C(20)—C(23)56.1 (11)O(2)—C(15)—C(16)—O(5)171.5 (7)
O(5)—C(11)—C(18)—O(7)68.6 (10)O(2)—C(15)—C(16)—C(14)72.9 (10)
O(5)—C(11)—C(19)—O(4)150.8 (9)O(9)—C(17)—C(23)—O(11)65.1 (10)
O(5)—C(11)—C(19)—C(14)25.0 (11)O(9)—C(17)—C(23)—C(20)179.4 (8)
C(18)—C(11)—C(19)—O(4)85.1 (11)C(13)—C(17)—C(23)—O(11)175.6 (8)
C(18)—C(11)—C(19)—C(14)149.1 (8)C(13)—C(17)—C(23)—C(20)60.1 (10)
C(19)—C(11)—C(18)—O(7)53.1 (11)O(8)—C(20)—C(22)—O(6)55.9 (10)
O(1)—C(13)—C(17)—O(9)65.6 (11)O(8)—C(20)—C(23)—O(11)177.0 (8)
O(1)—C(13)—C(17)—C(23)178.8 (7)O(8)—C(20)—C(23)—C(17)56.3 (11)
O(1)—C(13)—C(21)—O(3)55.2 (10)C(22)—C(20)—C(23)—O(11)63.6 (11)
O(1)—C(13)—C(21)—O(8)176.4 (7)C(22)—C(20)—C(23)—C(17)175.6 (9)
C(17)—C(13)—C(21)—O(3)61.7 (13)C(23)—C(20)—C(22)—O(6)64.0 (11)
C(17)—C(13)—C(21)—O(8)59.5 (11)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y1/2, z; (iii) x+1, y+1/2, z; (iv) x, y1/2, z; (v) x1, y, z; (vi) x, y+1/2, z; (vii) x+1, y+1/2, z+1; (viii) x, y+1, z; (ix) x+1, y1/2, z+1; (x) x, y1/2, z+1; (xi) x, y+1/2, z+1; (xii) x, y1, z; (xiii) x+1, y1, z; (xiv) x1, y+1, z.

Experimental details

Crystal data
Chemical formulaC12H22O11
Mr342.30
Crystal system, space groupMonoclinic, P21
Temperature (K)293
a, b, c (Å)7.7735 (12), 8.7169 (13), 10.8765 (17)
β (°) 102.936 (4)
V3)718.29 (19)
Z2
Radiation typeMo Kα
µ (mm1)0.14
Crystal size (mm)0.80 × 0.80 × 0.80
Data collection
DiffractometerRigaku RAXIS-RAPID
diffractometer
Absorption correctionMulti-scan
Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.
Tmin, Tmax0.054, 0.893
No. of measured, independent and
observed [F2 > 2.0σ(F2)] reflections
15524, 1730, 531
Rint0.166
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.079, 0.173, 1.01
No. of reflections1730
No. of parameters230
No. of restraints?
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.87, 0.78

Computer programs: PROCESS-AUTO, SIR92, CRYSTALS, CrystalStructure 3.8.

Selected geometric parameters (Å, º) top
O(1)—C(13)1.481 (15)O(10)—C(14)1.398 (12)
O(2)—C(15)1.466 (14)O(11)—C(23)1.481 (13)
O(3)—C(16)1.411 (12)C(11)—C(18)1.508 (17)
O(3)—C(21)1.412 (12)C(11)—C(19)1.467 (15)
O(4)—C(19)1.428 (12)C(13)—C(17)1.480 (16)
O(5)—C(11)1.439 (12)C(13)—C(21)1.562 (16)
O(5)—C(16)1.432 (14)C(14)—C(16)1.530 (13)
O(6)—C(22)1.428 (12)C(14)—C(19)1.522 (17)
O(7)—C(18)1.426 (12)C(15)—C(16)1.535 (16)
O(8)—C(20)1.440 (12)C(17)—C(23)1.524 (18)
O(8)—C(21)1.424 (14)C(20)—C(22)1.489 (18)
O(9)—C(17)1.382 (14)C(20)—C(23)1.535 (16)
C(16)—O(3)—C(21)114.2 (8)C(14)—C(16)—C(15)116.1 (9)
C(11)—O(5)—C(16)110.1 (7)O(9)—C(17)—C(13)112.5 (9)
C(20)—O(8)—C(21)117.7 (8)O(9)—C(17)—C(23)107.1 (9)
O(5)—C(11)—C(18)111.2 (8)C(13)—C(17)—C(23)104.2 (10)
O(5)—C(11)—C(19)106.6 (9)O(7)—C(18)—C(11)110.5 (8)
C(18)—C(11)—C(19)115.6 (9)O(4)—C(19)—C(11)112.7 (9)
O(1)—C(13)—C(17)106.7 (9)O(4)—C(19)—C(14)114.8 (9)
O(1)—C(13)—C(21)106.7 (8)C(11)—C(19)—C(14)105.3 (8)
C(17)—C(13)—C(21)112.9 (9)O(8)—C(20)—C(22)107.0 (9)
O(10)—C(14)—C(16)116.0 (8)O(8)—C(20)—C(23)108.0 (9)
O(10)—C(14)—C(19)117.9 (8)C(22)—C(20)—C(23)114.8 (9)
C(16)—C(14)—C(19)101.0 (8)O(3)—C(21)—O(8)111.4 (7)
O(2)—C(15)—C(16)107.4 (8)O(3)—C(21)—C(13)111.4 (9)
O(3)—C(16)—O(5)111.6 (8)O(8)—C(21)—C(13)105.9 (9)
O(3)—C(16)—C(14)108.5 (7)O(6)—C(22)—C(20)111.0 (9)
O(3)—C(16)—C(15)110.9 (8)O(11)—C(23)—C(17)112.0 (9)
O(5)—C(16)—C(14)105.8 (8)O(11)—C(23)—C(20)103.3 (8)
O(5)—C(16)—C(15)103.8 (8)C(17)—C(23)—C(20)112.0 (9)
 

Follow J. Appl. Cryst.
Sign up for e-alerts
Follow J. Appl. Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds