Buy article online - an online subscription or single-article purchase is required to access this article.
A high-resolution powder synchrotron X-ray diffraction pattern of the Γ form of
D-sorbitol has been recorded at 293 K on the BM1B beamline at the ESRF (Grenoble). The starting model of the structure was found by Monte Carlo simulated annealing. The final structure was obtained through Rietveld refinements performed with soft restraints on interatomic bond lengths and angles. The symmetry is orthorhombic, space group
P2
12
12, with 12 molecules within the cell [
a = 24.3012 (2),
b = 20.5726 (2),
c = 4.8672 (1) Å,
V = 2433.30 (3) Å
3,
Z′ = 3, 36 non-H independent atoms]. Crystalline cohesion between neighbouring molecules is achieved by three networks of O—H
O hydrogen bonds. The width of the Bragg peaks is interpreted through a microstructural approach in terms of anisotropic strain effects.
Supporting information
CCDC reference: 254343
Data collection: PEAKOC; program(s) used to solve structure: FOX; program(s) used to refine structure: FULLPROF; molecular graphics: ORTEP-3; software used to prepare material for publication: SHELX97 and PARST.
Crystal data top
C6H14O6 | V = 2433.30 (3) Å3 |
Mr = 182.17 | Z = 12 |
Orthorhombic, P21212 | BM01B, ESRF radiation, λ = 0.499570 Å |
Hall symbol: P 2 2ab | µ = 0.13 mm−1 |
a = 24.30122 (17) Å | T = 293 K |
b = 20.57261 (14) Å | white |
c = 4.86719 (3) Å | cylinder, diameter 1.5 mm, ? × ? × ? mm |
Data collection top
BM01B, ESRF diffractometer | Scan method: step |
Radiation source: Synchrotron | Absorption correction: for a cylinder mounted on the ϕ axis ? |
Si(1,1,1) monochromator | Tmin = ?, Tmax = ? |
Specimen mounting: Lindemann Glass Capillary | 2θmin = 1.500°, 2θmax = 28.000°, 2θstep = 0.005° |
Data collection mode: transmission | |
Refinement top
Rp = 1.837 | Profile function: pseudo-Voigt |
Rwp = 2.286 | 171 parameters |
Rexp = 1.650 | 63 restraints |
RBragg = 1.662 | |
χ2 = NOT FOUND | Background function: linear interpolation between 43 points |
6424 data points | Preferred orientation correction: March-Dollase function, axis [1,0,0], G1=0.994(1), G2=0 |
Excluded region(s): intensities too low | |
Crystal data top
C6H14O6 | V = 2433.30 (3) Å3 |
Mr = 182.17 | Z = 12 |
Orthorhombic, P21212 | BM01B, ESRF radiation, λ = 0.499570 Å |
a = 24.30122 (17) Å | µ = 0.13 mm−1 |
b = 20.57261 (14) Å | T = 293 K |
c = 4.86719 (3) Å | cylinder, diameter 1.5 mm, ? × ? × ? mm |
Data collection top
BM01B, ESRF diffractometer | Absorption correction: for a cylinder mounted on the ϕ axis ? |
Specimen mounting: Lindemann Glass Capillary | Tmin = ?, Tmax = ? |
Data collection mode: transmission | 2θmin = 1.500°, 2θmax = 28.000°, 2θstep = 0.005° |
Scan method: step | |
Refinement top
Rp = 1.837 | χ2 = NOT FOUND |
Rwp = 2.286 | 6424 data points |
Rexp = 1.650 | 171 parameters |
RBragg = 1.662 | 63 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C11 | 0.36472 (15) | 0.51245 (19) | 0.6125 (10) | 0.0326 (5)* | |
C12 | 0.41877 (13) | 0.50350 (11) | 0.4570 (7) | 0.0326 (5)* | |
C13 | 0.41601 (15) | 0.44029 (12) | 0.2907 (6) | 0.0326 (5)* | |
C14 | 0.42261 (14) | 0.38001 (11) | 0.4713 (7) | 0.0326 (5)* | |
C15 | 0.41697 (16) | 0.31586 (11) | 0.3152 (7) | 0.0326 (5)* | |
C16 | 0.42283 (19) | 0.2534 (2) | 0.4798 (10) | 0.0326 (5)* | |
O11 | 0.36953 (15) | 0.56981 (15) | 0.7773 (7) | 0.0326 (5)* | |
O12 | 0.42365 (16) | 0.55813 (15) | 0.2784 (7) | 0.0326 (5)* | |
O13 | 0.46221 (13) | 0.44282 (18) | 0.1099 (8) | 0.0326 (5)* | |
O14 | 0.47456 (11) | 0.37937 (18) | 0.6094 (8) | 0.0326 (5)* | |
O15 | 0.37078 (13) | 0.31704 (18) | 0.1344 (7) | 0.0326 (5)* | |
O16 | 0.37906 (13) | 0.25555 (19) | 0.6723 (7) | 0.0326 (5)* | |
H11A | 0.33360 | 0.51660 | 0.48090 | 0.0326 (5)* | |
H11B | 0.35800 | 0.47360 | 0.73380 | 0.0326 (5)* | |
H12 | 0.45050 | 0.50210 | 0.58810 | 0.0326 (5)* | |
H13 | 0.38090 | 0.43810 | 0.18380 | 0.0326 (5)* | |
H14 | 0.39310 | 0.38130 | 0.61450 | 0.0326 (5)* | |
H15 | 0.44940 | 0.31540 | 0.18870 | 0.0326 (5)* | |
H16A | 0.41950 | 0.21460 | 0.35830 | 0.0326 (5)* | |
H16B | 0.45920 | 0.25210 | 0.57630 | 0.0326 (5)* | |
HO11 | 0.33379 | 0.58747 | 0.75049 | 0.0326 (5)* | |
HO12 | 0.45349 | 0.56125 | 0.27003 | 0.0326 (5)* | |
HO13 | 0.45930 | 0.42230 | −0.03062 | 0.0326 (5)* | |
HO14 | 0.47024 | 0.36535 | 0.75735 | 0.0326 (5)* | |
HO15 | 0.33798 | 0.32362 | 0.20605 | 0.0326 (5)* | |
HO16 | 0.34860 | 0.26271 | 0.60495 | 0.0326 (5)* | |
C21 | 0.10186 (15) | 0.22078 (19) | 0.3416 (9) | 0.0339 (6)* | |
C22 | 0.07691 (11) | 0.27904 (15) | 0.1977 (7) | 0.0339 (6)* | |
C23 | 0.11906 (12) | 0.31472 (16) | 0.0233 (7) | 0.0339 (6)* | |
C24 | 0.16296 (11) | 0.34940 (16) | 0.1958 (7) | 0.0339 (6)* | |
C25 | 0.20804 (11) | 0.37951 (16) | 0.0202 (7) | 0.0339 (6)* | |
C26 | 0.25327 (19) | 0.41219 (17) | 0.1870 (10) | 0.0339 (6)* | |
O21 | 0.06459 (13) | 0.19346 (18) | 0.5354 (7) | 0.0339 (6)* | |
O22 | 0.03162 (13) | 0.25723 (19) | 0.0365 (7) | 0.0339 (6)* | |
O23 | 0.09113 (15) | 0.36106 (15) | −0.1473 (7) | 0.0339 (6)* | |
O24 | 0.13952 (14) | 0.40146 (15) | 0.3502 (7) | 0.0339 (6)* | |
O25 | 0.23291 (16) | 0.32992 (16) | −0.1452 (8) | 0.0339 (6)* | |
O26 | 0.27807 (15) | 0.36617 (14) | 0.3701 (8) | 0.0339 (6)* | |
H21A | 0.11220 | 0.18740 | 0.20330 | 0.0339 (6)* | |
H21B | 0.13600 | 0.23520 | 0.44210 | 0.0339 (6)* | |
H22 | 0.06270 | 0.30980 | 0.34040 | 0.0339 (6)* | |
H23 | 0.13780 | 0.28240 | −0.09810 | 0.0339 (6)* | |
H24 | 0.17990 | 0.31740 | 0.32540 | 0.0339 (6)* | |
H25 | 0.19110 | 0.41260 | −0.10430 | 0.0339 (6)* | |
H26A | 0.28180 | 0.43010 | 0.06020 | 0.0339 (6)* | |
H26B | 0.23710 | 0.44880 | 0.29640 | 0.0339 (6)* | |
HO21 | 0.06385 | 0.15432 | 0.55250 | 0.0339 (6)* | |
HO22 | 0.04755 | 0.23840 | −0.14054 | 0.0339 (6)* | |
HO23 | 0.10669 | 0.35595 | −0.28832 | 0.0339 (6)* | |
HO24 | 0.13148 | 0.41060 | 0.50022 | 0.0339 (6)* | |
HO25 | 0.21536 | 0.32980 | −0.26875 | 0.0339 (6)* | |
HO26 | 0.28423 | 0.38638 | 0.50852 | 0.0339 (6)* | |
C31 | 0.4478 (2) | 0.10689 (15) | 0.9420 (12) | 0.0521 (6)* | |
C32 | 0.41397 (10) | 0.05197 (16) | 0.8158 (7) | 0.0521 (6)* | |
C33 | 0.36336 (11) | 0.07649 (19) | 0.6578 (7) | 0.0521 (6)* | |
C34 | 0.31614 (11) | 0.10469 (16) | 0.8290 (7) | 0.0521 (6)* | |
C35 | 0.26915 (11) | 0.13216 (16) | 0.6570 (7) | 0.0521 (6)* | |
C36 | 0.22303 (14) | 0.1562 (2) | 0.8399 (9) | 0.0521 (6)* | |
O31 | 0.48932 (15) | 0.0791 (2) | 1.1122 (8) | 0.0521 (6)* | |
O32 | 0.45244 (14) | 0.0260 (2) | 0.6236 (7) | 0.0521 (6)* | |
O33 | 0.34700 (17) | 0.02917 (17) | 0.4592 (7) | 0.0521 (6)* | |
O34 | 0.29366 (15) | 0.05072 (15) | 0.9758 (9) | 0.0521 (6)* | |
O35 | 0.29054 (15) | 0.18453 (16) | 0.5000 (9) | 0.0521 (6)* | |
O36 | 0.24119 (16) | 0.20219 (16) | 1.0400 (8) | 0.0521 (6)* | |
H31A | 0.46510 | 0.13340 | 0.79340 | 0.0521 (6)* | |
H31B | 0.42330 | 0.13560 | 1.05490 | 0.0521 (6)* | |
H32 | 0.40350 | 0.01890 | 0.95710 | 0.0521 (6)* | |
H33 | 0.37720 | 0.11400 | 0.54720 | 0.0521 (6)* | |
H34 | 0.33020 | 0.13830 | 0.95990 | 0.0521 (6)* | |
H35 | 0.25490 | 0.09770 | 0.53100 | 0.0521 (6)* | |
H36A | 0.19430 | 0.17720 | 0.72210 | 0.0521 (6)* | |
H36B | 0.20640 | 0.11820 | 0.93680 | 0.0521 (6)* | |
HO31 | 0.52151 | 0.07209 | 1.03566 | 0.0521 (6)* | |
HO32 | 0.43449 | 0.00434 | 0.43925 | 0.0521 (6)* | |
HO33 | 0.32332 | 0.00529 | 0.52058 | 0.0521 (6)* | |
HO34 | 0.30225 | 0.05733 | 1.11887 | 0.0521 (6)* | |
HO35 | 0.31953 | 0.17597 | 0.44736 | 0.0521 (6)* | |
HO36 | 0.23909 | 0.23850 | 0.95956 | 0.0521 (6)* | |
Geometric parameters (Å, º) top
C11—O11 | 1.432 (5) | C25—O25 | 1.433 (5) |
C11—C12 | 1.527 (5) | C25—C26 | 1.523 (5) |
C11—H11A | 0.995 | C25—H25 | 1.000 |
C11—H11B | 1.007 | C26—O26 | 1.433 (5) |
C12—O12 | 1.426 (4) | C26—H26A | 0.999 |
C12—C13 | 1.533 (4) | C26—H26B | 1.002 |
C12—H12 | 1.001 | O21—HO21 | 0.810 |
C13—O13 | 1.427 (5) | O22—HO22 | 1.021 |
C13—C14 | 1.528 (4) | O23—HO23 | 0.791 |
C13—H13 | 1.000 | O24—HO24 | 0.779 |
C14—O14 | 1.430 (4) | O25—HO25 | 0.737 |
C14—C15 | 1.529 (4) | O26—HO26 | 0.806 |
C14—H14 | 1.001 | C31—O31 | 1.425 (6) |
C15—O15 | 1.426 (5) | C31—C32 | 1.526 (5) |
C15—C16 | 1.520 (5) | C31—H31A | 0.999 |
C15—H15 | 1.000 | C31—H31B | 1.002 |
C16—O16 | 1.418 (6) | C32—O32 | 1.426 (4) |
C16—H16A | 0.998 | C32—C33 | 1.536 (4) |
C16—H16B | 1.002 | C32—H32 | 1.000 |
O11—HO11 | 0.951 | C33—O33 | 1.428 (5) |
O12—HO12 | 0.729 | C33—C34 | 1.532 (4) |
O13—HO13 | 0.807 | C33—H33 | 0.999 |
O14—HO14 | 0.783 | C34—O34 | 1.429 (5) |
O15—HO15 | 0.880 | C34—C35 | 1.524 (4) |
O16—HO16 | 0.823 | C34—H34 | 1.000 |
C21—O21 | 1.424 (5) | C35—O35 | 1.420 (5) |
C21—C22 | 1.515 (5) | C35—C36 | 1.514 (5) |
C21—H21A | 0.994 | C35—H35 | 0.999 |
C21—H21B | 1.007 | C36—O36 | 1.428 (6) |
C22—O22 | 1.424 (4) | C36—H36A | 1.001 |
C22—C23 | 1.520 (4) | C36—H36B | 0.999 |
C22—H22 | 1.001 | O31—HO31 | 0.878 |
C23—O23 | 1.435 (5) | O32—HO32 | 1.093 |
C23—C24 | 1.534 (4) | O33—HO33 | 0.814 |
C23—H23 | 0.999 | O34—HO34 | 0.739 |
C24—O24 | 1.427 (4) | O35—HO35 | 0.770 |
C24—C25 | 1.521 (4) | O36—HO36 | 0.845 |
C24—H24 | 1.000 | | |
| | | |
O11—C11—C12 | 107.9 (3) | O24—C24—H24 | 109.0 |
O11—C11—H11A | 110.6 | C25—C24—H24 | 109.0 |
C12—C11—H11A | 110.2 | C23—C24—H24 | 109.0 |
O11—C11—H11B | 109.8 | O25—C25—C24 | 109.2 (3) |
C12—C11—H11B | 109.5 | O25—C25—C26 | 108.0 (3) |
H11A—C11—H11B | 108.8 | C24—C25—C26 | 113.6 (3) |
O12—C12—C11 | 106.2 (3) | O25—C25—H25 | 108.5 |
O12—C12—C13 | 110.5 (2) | C24—C25—H25 | 108.7 |
C11—C12—C13 | 109.0 (3) | C26—C25—H25 | 108.6 |
O12—C12—H12 | 110.3 | O26—C26—C25 | 110.1 (4) |
C11—C12—H12 | 110.5 | O26—C26—H26A | 109.6 |
C13—C12—H12 | 110.2 | C25—C26—H26A | 109.5 |
O13—C13—C14 | 107.5 (3) | O26—C26—H26B | 109.3 |
O13—C13—C12 | 105.1 (3) | C25—C26—H26B | 109.4 |
C14—C13—C12 | 112.3 (2) | H26A—C26—H26B | 108.9 |
O13—C13—H13 | 110.6 | C21—O21—HO21 | 118.4 |
C14—C13—H13 | 110.6 | C22—O22—HO22 | 107.0 |
C12—C13—H13 | 110.5 | C23—O23—HO23 | 100.8 |
O14—C14—C13 | 111.7 (3) | C24—O24—HO24 | 140.8 |
O14—C14—C15 | 107.7 (3) | C25—O25—HO25 | 102.5 |
C13—C14—C15 | 113.9 (2) | C26—O26—HO26 | 104.9 |
O14—C14—H14 | 107.8 | O31—C31—C32 | 108.6 (4) |
C13—C14—H14 | 107.7 | O31—C31—H31A | 110.0 |
C15—C14—H14 | 107.7 | C32—C31—H31A | 109.8 |
O15—C15—C16 | 114.4 (3) | O31—C31—H31B | 109.7 |
O15—C15—C14 | 111.2 (3) | C32—C31—H31B | 109.7 |
C16—C15—C14 | 117.3 (2) | H31A—C31—H31B | 109.0 |
O15—C15—H15 | 103.9 | O32—C32—C31 | 100.9 (3) |
C16—C15—H15 | 104.0 | O32—C32—C33 | 108.6 (2) |
C14—C15—H15 | 104.1 | C31—C32—C33 | 112.9 (3) |
O16—C16—C15 | 104.6 (3) | O32—C32—H32 | 111.3 |
O16—C16—H16A | 110.8 | C31—C32—H32 | 111.3 |
C15—C16—H16A | 110.9 | C33—C32—H32 | 111.3 |
O16—C16—H16B | 110.7 | O33—C33—C34 | 114.7 (3) |
C15—C16—H16B | 110.7 | O33—C33—C32 | 109.7 (3) |
H16A—C16—H16B | 109.1 | C34—C33—C32 | 116.9 (2) |
C11—O11—HO11 | 99.4 | O33—C33—H33 | 104.8 |
C12—O12—HO12 | 100.7 | C34—C33—H33 | 104.6 |
C13—O13—HO13 | 115.8 | C32—C33—H33 | 104.7 |
C14—O14—HO14 | 108.5 | O34—C34—C35 | 106.0 (3) |
C15—O15—HO15 | 118.1 | O34—C34—C33 | 105.3 (3) |
C16—O16—HO16 | 114.6 | C35—C34—C33 | 113.7 (2) |
O21—C21—C22 | 111.3 (4) | O34—C34—H34 | 110.4 |
O21—C21—H21A | 109.6 | C35—C34—H34 | 110.4 |
C22—C21—H21A | 109.5 | C33—C34—H34 | 110.6 |
O21—C21—H21B | 108.6 | O35—C35—C36 | 109.8 (3) |
C22—C21—H21B | 108.8 | O35—C35—C34 | 107.6 (3) |
H21A—C21—H21B | 108.9 | C36—C35—C34 | 110.7 (2) |
O22—C22—C21 | 108.4 (3) | O35—C35—H35 | 109.6 |
O22—C22—C23 | 111.4 (2) | C36—C35—H35 | 109.6 |
C21—C22—C23 | 111.8 (3) | C34—C35—H35 | 109.5 |
O22—C22—H22 | 108.3 | O36—C36—C35 | 112.9 (4) |
C21—C22—H22 | 108.5 | O36—C36—H36A | 108.7 |
C23—C22—H22 | 108.4 | C35—C36—H36A | 108.7 |
O23—C23—C22 | 109.0 (3) | O36—C36—H36B | 108.8 |
O23—C23—C24 | 109.7 (3) | C35—C36—H36B | 108.7 |
C22—C23—C24 | 112.8 (2) | H36A—C36—H36B | 109.0 |
O23—C23—H23 | 108.4 | C31—O31—HO31 | 116.8 |
C22—C23—H23 | 108.4 | C32—O32—HO32 | 115.4 |
C24—C23—H23 | 108.4 | C33—O33—HO33 | 111.1 |
O24—C24—C25 | 106.1 (3) | C34—O34—HO34 | 102.7 |
O24—C24—C23 | 111.1 (3) | C35—O35—HO35 | 109.9 |
C25—C24—C23 | 112.5 (2) | C36—O36—HO36 | 104.5 |
| | | |
O11—C11—C12—O12 | −64.0 (4) | O23—C23—C24—C25 | −63.8 (3) |
O11—C11—C12—C13 | 176.9 (3) | C22—C23—C24—C25 | 174.5 (2) |
O12—C12—C13—O13 | 51.7 (3) | O24—C24—C25—O25 | −179.0 (3) |
C11—C12—C13—O13 | 168.0 (3) | C23—C24—C25—O25 | −57.3 (3) |
O12—C12—C13—C14 | 168.3 (3) | O24—C24—C25—C26 | 60.4 (4) |
C11—C12—C13—C14 | −75.4 (3) | C23—C24—C25—C26 | −177.9 (3) |
O13—C13—C14—O14 | 54.4 (3) | O25—C25—C26—O26 | −63.1 (4) |
C12—C13—C14—O14 | −60.8 (3) | C24—C25—C26—O26 | 58.3 (4) |
O13—C13—C14—C15 | −68.0 (3) | O31—C31—C32—O32 | −71.7 (4) |
C12—C13—C14—C15 | 176.9 (3) | O31—C31—C32—C33 | 172.6 (3) |
O14—C14—C15—O15 | −170.0 (3) | O32—C32—C33—O33 | 45.5 (4) |
C13—C14—C15—O15 | −45.4 (4) | C31—C32—C33—O33 | 156.6 (3) |
O14—C14—C15—C16 | 55.6 (4) | O32—C32—C33—C34 | 178.4 (3) |
C13—C14—C15—C16 | −179.8 (3) | C31—C32—C33—C34 | −70.6 (4) |
O15—C15—C16—O16 | −71.0 (4) | O33—C33—C34—O34 | 62.3 (4) |
C14—C15—C16—O16 | 62.0 (4) | C32—C33—C34—O34 | −68.3 (3) |
O21—C21—C22—O22 | −65.5 (4) | O33—C33—C34—C35 | −53.4 (4) |
O21—C21—C22—C23 | 171.3 (3) | C32—C33—C34—C35 | 176.1 (3) |
O22—C22—C23—O23 | 47.6 (4) | O34—C34—C35—O35 | −177.9 (3) |
C21—C22—C23—O23 | 169.0 (3) | C33—C34—C35—O35 | −62.6 (3) |
O22—C22—C23—C24 | 169.7 (3) | O34—C34—C35—C36 | 62.1 (4) |
C21—C22—C23—C24 | −69.0 (3) | C33—C34—C35—C36 | 177.4 (3) |
O23—C23—C24—O24 | 55.0 (3) | O35—C35—C36—O36 | −63.9 (4) |
C22—C23—C24—O24 | −66.7 (3) | C34—C35—C36—O36 | 54.7 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O12—HO12···O13i | 0.729 (4) | 2.193 (3) | 2.892 (5) | 161.0 (3) |
O13—HO13···O14ii | 0.807 (4) | 1.997 (4) | 2.780 (5) | 163.5 (3) |
O15—HO15···O26 | 0.880 (3) | 1.877 (3) | 2.723 (5) | 160.4 (2) |
O21—HO21···O12iii | 0.810 (4) | 2.165 (3) | 2.942 (5) | 160.9 (3) |
O22—HO22···O21ii | 1.021 (3) | 1.875 (4) | 2.883 (5) | 168.8 (2) |
O24—HO24···O23iv | 0.779 (3) | 2.224 (3) | 2.838 (5) | 136.3 (3) |
O26—HO26···O25iv | 0.806 (3) | 2.397 (4) | 2.707 (5) | 104.0 (3) |
O33—HO33···O24iii | 0.814 (4) | 2.403 (3) | 2.805 (4) | 111.5 (2) |
O34—HO34···O33iv | 0.739 (4) | 2.065 (4) | 2.722 (5) | 148.5 (3) |
O35—HO35···O16 | 0.770 (4) | 2.444 (3) | 2.732 (5) | 103.8 (3) |
Symmetry codes: (i) −x+1, −y+1, z; (ii) x, y, z−1; (iii) −x+1/2, y−1/2, −z+1; (iv) x, y, z+1. |
Experimental details
Crystal data |
Chemical formula | C6H14O6 |
Mr | 182.17 |
Crystal system, space group | Orthorhombic, P21212 |
Temperature (K) | 293 |
a, b, c (Å) | 24.30122 (17), 20.57261 (14), 4.86719 (3) |
V (Å3) | 2433.30 (3) |
Z | 12 |
Radiation type | BM01B, ESRF, λ = 0.499570 Å |
µ (mm−1) | 0.13 |
Specimen shape, size (mm) | Cylinder, diameter 1.5 mm, ? × ? × ? |
|
Data collection |
Data collection method | BM01B, ESRF |
Specimen mounting | Lindemann Glass Capillary |
Data collection mode | Transmission |
Scan method | Step |
2θ values (°) | 2θmin = 1.500 2θmax = 28.000 2θstep = 0.005 |
|
Refinement |
R factors and goodness of fit | Rp = 1.837, Rwp = 2.286, Rexp = 1.650, RBragg = 1.662, χ2 = NOT FOUND |
No. of data points | 6424 |
No. of parameters | 171 |
No. of restraints | 63 |
Selected geometric parameters (Å, º) topC11—O11 | 1.432 (5) | C24—O24 | 1.427 (4) |
C11—C12 | 1.527 (5) | C24—C25 | 1.521 (4) |
C12—O12 | 1.426 (4) | C25—O25 | 1.433 (5) |
C12—C13 | 1.533 (4) | C25—C26 | 1.523 (5) |
C13—O13 | 1.427 (5) | C26—O26 | 1.433 (5) |
C13—C14 | 1.528 (4) | C31—O31 | 1.425 (6) |
C14—O14 | 1.430 (4) | C31—C32 | 1.526 (5) |
C14—C15 | 1.529 (4) | C32—O32 | 1.426 (4) |
C15—O15 | 1.426 (5) | C32—C33 | 1.536 (4) |
C15—C16 | 1.520 (5) | C33—O33 | 1.428 (5) |
C16—O16 | 1.418 (6) | C33—C34 | 1.532 (4) |
C21—O21 | 1.424 (5) | C34—O34 | 1.429 (5) |
C21—C22 | 1.515 (5) | C34—C35 | 1.524 (4) |
C22—O22 | 1.424 (4) | C35—O35 | 1.420 (5) |
C22—C23 | 1.520 (4) | C35—C36 | 1.514 (5) |
C23—O23 | 1.435 (5) | C36—O36 | 1.428 (6) |
C23—C24 | 1.534 (4) | | |
| | | |
O11—C11—C12 | 107.9 (3) | O24—C24—C25 | 106.1 (3) |
O12—C12—C11 | 106.2 (3) | O24—C24—C23 | 111.1 (3) |
O12—C12—C13 | 110.5 (2) | C25—C24—C23 | 112.5 (2) |
C11—C12—C13 | 109.0 (3) | O25—C25—C24 | 109.2 (3) |
O13—C13—C14 | 107.5 (3) | O25—C25—C26 | 108.0 (3) |
O13—C13—C12 | 105.1 (3) | C24—C25—C26 | 113.6 (3) |
C14—C13—C12 | 112.3 (2) | O26—C26—C25 | 110.1 (4) |
O14—C14—C13 | 111.7 (3) | O31—C31—C32 | 108.6 (4) |
O14—C14—C15 | 107.7 (3) | O32—C32—C31 | 100.9 (3) |
C13—C14—C15 | 113.9 (2) | O32—C32—C33 | 108.6 (2) |
O15—C15—C16 | 114.4 (3) | C31—C32—C33 | 112.9 (3) |
O15—C15—C14 | 111.2 (3) | O33—C33—C34 | 114.7 (3) |
C16—C15—C14 | 117.3 (2) | O33—C33—C32 | 109.7 (3) |
O16—C16—C15 | 104.6 (3) | C34—C33—C32 | 116.9 (2) |
O21—C21—C22 | 111.3 (4) | O34—C34—C35 | 106.0 (3) |
O22—C22—C21 | 108.4 (3) | O34—C34—C33 | 105.3 (3) |
O22—C22—C23 | 111.4 (2) | C35—C34—C33 | 113.7 (2) |
C21—C22—C23 | 111.8 (3) | O35—C35—C36 | 109.8 (3) |
O23—C23—C22 | 109.0 (3) | O35—C35—C34 | 107.6 (3) |
O23—C23—C24 | 109.7 (3) | C36—C35—C34 | 110.7 (2) |
C22—C23—C24 | 112.8 (2) | O36—C36—C35 | 112.9 (4) |
| | | |
O11—C11—C12—O12 | −64.0 (4) | O23—C23—C24—C25 | −63.8 (3) |
O11—C11—C12—C13 | 176.9 (3) | C22—C23—C24—C25 | 174.5 (2) |
O12—C12—C13—O13 | 51.7 (3) | O24—C24—C25—O25 | −179.0 (3) |
C11—C12—C13—O13 | 168.0 (3) | C23—C24—C25—O25 | −57.3 (3) |
O12—C12—C13—C14 | 168.3 (3) | O24—C24—C25—C26 | 60.4 (4) |
C11—C12—C13—C14 | −75.4 (3) | C23—C24—C25—C26 | −177.9 (3) |
O13—C13—C14—O14 | 54.4 (3) | O25—C25—C26—O26 | −63.1 (4) |
C12—C13—C14—O14 | −60.8 (3) | C24—C25—C26—O26 | 58.3 (4) |
O13—C13—C14—C15 | −68.0 (3) | O31—C31—C32—O32 | −71.7 (4) |
C12—C13—C14—C15 | 176.9 (3) | O31—C31—C32—C33 | 172.6 (3) |
O14—C14—C15—O15 | −170.0 (3) | O32—C32—C33—O33 | 45.5 (4) |
C13—C14—C15—O15 | −45.4 (4) | C31—C32—C33—O33 | 156.6 (3) |
O14—C14—C15—C16 | 55.6 (4) | O32—C32—C33—C34 | 178.4 (3) |
C13—C14—C15—C16 | −179.8 (3) | C31—C32—C33—C34 | −70.6 (4) |
O15—C15—C16—O16 | −71.0 (4) | O33—C33—C34—O34 | 62.3 (4) |
C14—C15—C16—O16 | 62.0 (4) | C32—C33—C34—O34 | −68.3 (3) |
O21—C21—C22—O22 | −65.5 (4) | O33—C33—C34—C35 | −53.4 (4) |
O21—C21—C22—C23 | 171.3 (3) | C32—C33—C34—C35 | 176.1 (3) |
O22—C22—C23—O23 | 47.6 (4) | O34—C34—C35—O35 | −177.9 (3) |
C21—C22—C23—O23 | 169.0 (3) | C33—C34—C35—O35 | −62.6 (3) |
O22—C22—C23—C24 | 169.7 (3) | O34—C34—C35—C36 | 62.1 (4) |
C21—C22—C23—C24 | −69.0 (3) | C33—C34—C35—C36 | 177.4 (3) |
O23—C23—C24—O24 | 55.0 (3) | O35—C35—C36—O36 | −63.9 (4) |
C22—C23—C24—O24 | −66.7 (3) | C34—C35—C36—O36 | 54.7 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O12—HO12···O13i | 0.729 (4) | 2.193 (3) | 2.892 (5) | 161.0 (3) |
O13—HO13···O14ii | 0.807 (4) | 1.997 (4) | 2.780 (5) | 163.5 (3) |
O15—HO15···O26 | 0.880 (3) | 1.877 (3) | 2.723 (5) | 160.4 (2) |
O21—HO21···O12iii | 0.810 (4) | 2.165 (3) | 2.942 (5) | 160.9 (3) |
O22—HO22···O21ii | 1.021 (3) | 1.875 (4) | 2.883 (5) | 168.8 (2) |
O24—HO24···O23iv | 0.779 (3) | 2.224 (3) | 2.838 (5) | 136.3 (3) |
O26—HO26···O25iv | 0.806 (3) | 2.397 (4) | 2.707 (5) | 104.0 (3) |
O33—HO33···O24iii | 0.814 (4) | 2.403 (3) | 2.805 (4) | 111.5 (2) |
O34—HO34···O33iv | 0.739 (4) | 2.065 (4) | 2.722 (5) | 148.5 (3) |
O35—HO35···O16 | 0.770 (4) | 2.444 (3) | 2.732 (5) | 103.8 (3) |
Symmetry codes: (i) −x+1, −y+1, z; (ii) x, y, z−1; (iii) −x+1/2, y−1/2, −z+1; (iv) x, y, z+1. |
Subscribe to Journal of Applied Crystallography
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.