Download citation
Download citation
link to html
A new approach is proposed for assessment of the quality of restrained Rietveld refinement. As the first step, we require the consistency of the restraints and diffraction data: namely, the absence of outliers in the distribution of the bond length deviations from the target values. This condition is tested using a simple and robust outlier detection criterion and can be reached for any correct structure. Then, the range of restraint variation where the model remains consistent (uncertainty window) is calculated. This metric is indicative of the combined model and data quality. The average half uncertainty window (HUW) can serve as an estimate of the effective bond precision; HUW < 0.04 Å is reachable for highly crystalline powders, and HUW exceeds 0.3 Å for unacceptable models. A round-robin involving the most popular laboratory diffractometer geometries and an analysis of literature examples show that HUW, unlike `classic' R values, is instrument independent and versatile.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600576715018233/ks5484sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715018233/ks5484Isup2.hkl
Contains datablock I

zip

Zip compressed file https://doi.org/10.1107/S1600576715018233/ks5484sup3.zip
TOPAS OUT files for instrument round robin

zip

Zip compressed file https://doi.org/10.1107/S1600576715018233/ks5484sup4.zip
Rietveld fits for instrument round robin

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S1600576715018233/ks5484sup5.pdf
Statistical analysis, experimental details.

CCDC reference: 1428622

Computing details top

Cell refinement: SAINT v8.27A (Bruker, 2012); data reduction: SAINT v8.27A (Bruker, 2012); program(s) used to solve structure: olex2.solve (Bourhis et al., 2015); program(s) used to refine structure: SHELXL (Sheldrick, 2008); molecular graphics: Olex2 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 (Dolomanov et al., 2009).

sucrose top
Crystal data top
C12H22O11F(000) = 364
Mr = 342.29Dx = 1.587 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
a = 7.7630 (1) ÅCell parameters from 9946 reflections
b = 8.7109 (1) Åθ = 2.7–37.7°
c = 10.8701 (1) ŵ = 0.14 mm1
β = 102.937 (1)°T = 298 K
V = 716.41 (1) Å3Prism, colourless
Z = 20.2 × 0.2 × 0.1 mm
Data collection top
Bruker APEX-II CCD
diffractometer
16720 independent reflections
Graphite monochromator10732 reflections with I > 2σ(I)
Detector resolution: 7.9 pixels mm-1Rint = 0.053
ω and φ scansθmax = 52.9°, θmin = 1.9°
Absorption correction: multi-scan
SADABS2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0783 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.9421. The λ/2 correction factor is 0.0015.
h = 1717
Tmin = 0.814, Tmax = 0.864k = 1919
85318 measured reflectionsl = 2424
Refinement top
Refinement on F2Hydrogen site location: mixed
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.041 w = 1/[σ2(Fo2) + (0.0554P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.110(Δ/σ)max = 0.001
S = 0.97Δρmax = 0.42 e Å3
16720 reflectionsΔρmin = 0.27 e Å3
240 parametersAbsolute structure: Flack x determined using 3930 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
1 restraintAbsolute structure parameter: 0.10 (17)
Primary atom site location: iterative
Crystal data top
C12H22O11V = 716.41 (1) Å3
Mr = 342.29Z = 2
Monoclinic, P21Mo Kα radiation
a = 7.7630 (1) ŵ = 0.14 mm1
b = 8.7109 (1) ÅT = 298 K
c = 10.8701 (1) Å0.2 × 0.2 × 0.1 mm
β = 102.937 (1)°
Data collection top
Bruker APEX-II CCD
diffractometer
16720 independent reflections
Absorption correction: multi-scan
SADABS2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0783 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.9421. The λ/2 correction factor is 0.0015.
10732 reflections with I > 2σ(I)
Tmin = 0.814, Tmax = 0.864Rint = 0.053
85318 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.110Δρmax = 0.42 e Å3
S = 0.97Δρmin = 0.27 e Å3
16720 reflectionsAbsolute structure: Flack x determined using 3930 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
240 parametersAbsolute structure parameter: 0.10 (17)
1 restraint
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O50.36841 (9)0.35614 (8)0.87745 (6)0.01993 (10)
O10.39132 (8)0.40800 (7)0.67129 (5)0.01663 (8)
O2'0.31604 (8)0.66041 (8)0.71222 (6)0.02006 (10)
O20.74756 (10)0.31907 (10)0.72915 (7)0.02551 (13)
O3'0.20423 (10)0.43686 (9)0.42597 (6)0.02336 (12)
C10.48497 (10)0.39692 (9)0.79987 (7)0.01652 (10)
H10.53610.49760.82690.020*
C2'0.36918 (9)0.56218 (9)0.62442 (7)0.01536 (10)
O4'0.08937 (9)0.65786 (11)0.47835 (7)0.02704 (14)
O1'0.62086 (10)0.51904 (11)0.52977 (7)0.02675 (13)
O6'0.03985 (11)0.51644 (12)0.82653 (8)0.03054 (15)
C3'0.21469 (10)0.56404 (9)0.50718 (7)0.01667 (10)
H3'A0.22770.65610.45820.020*
O60.28608 (13)0.20923 (12)1.08175 (8)0.03221 (16)
C20.63601 (11)0.28017 (10)0.81255 (7)0.01893 (12)
H2A0.70660.28370.89940.023*
C5'0.12857 (10)0.69352 (10)0.67634 (8)0.01922 (12)
H5'0.11270.80040.64790.023*
C50.29554 (12)0.20323 (10)0.85919 (8)0.02092 (13)
H50.21910.19510.77450.025*
O30.70323 (14)0.00683 (11)0.80871 (9)0.03492 (19)
C30.56427 (13)0.11799 (10)0.78547 (8)0.02144 (13)
H3A0.49800.11060.69760.026*
C4'0.05477 (10)0.58827 (10)0.56467 (7)0.01792 (11)
H4'A0.01760.49030.59470.022*
C1'0.54373 (11)0.62374 (11)0.60298 (9)0.02158 (13)
H1'A0.52370.72170.55960.026*
H1'B0.62470.64040.68380.026*
C40.44218 (13)0.08372 (10)0.87418 (8)0.02258 (14)
H40.51110.08490.96150.027*
C60.18429 (14)0.18419 (13)0.95757 (10)0.02785 (17)
H6A0.08680.25650.94000.033*
H6B0.13510.08140.95180.033*
C6'0.04663 (13)0.67307 (13)0.78920 (9)0.02666 (17)
H6'A0.11450.73150.85960.032*
H6'B0.07240.71440.76900.032*
O40.35558 (16)0.05938 (11)0.84910 (13)0.0415 (2)
H20.837 (3)0.375 (3)0.768 (2)0.050 (6)*
H30.735 (3)0.022 (3)0.746 (2)0.051 (6)*
H6'0.151 (3)0.483 (3)0.850 (2)0.053 (7)*
H60.283 (3)0.305 (3)1.099 (2)0.046 (6)*
H1'0.654 (3)0.448 (3)0.572 (2)0.040 (5)*
H4'0.179 (3)0.607 (3)0.487 (2)0.047 (6)*
H3'0.185 (3)0.361 (3)0.4618 (18)0.030 (4)*
H4A0.421 (5)0.119 (4)0.842 (3)0.080 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O50.0246 (3)0.0178 (2)0.0197 (2)0.00012 (19)0.00992 (19)0.00016 (18)
O10.0190 (2)0.01404 (19)0.01625 (18)0.00084 (17)0.00274 (15)0.00062 (16)
O2'0.0166 (2)0.0196 (2)0.0233 (2)0.00146 (18)0.00322 (17)0.0064 (2)
O20.0201 (3)0.0300 (3)0.0282 (3)0.0008 (2)0.0093 (2)0.0025 (3)
O3'0.0270 (3)0.0235 (3)0.0199 (2)0.0030 (2)0.0058 (2)0.0046 (2)
C10.0181 (3)0.0159 (2)0.0157 (2)0.0002 (2)0.00409 (19)0.0002 (2)
C2'0.0141 (2)0.0146 (2)0.0180 (2)0.00066 (19)0.00474 (18)0.0003 (2)
O4'0.0161 (2)0.0332 (4)0.0300 (3)0.0030 (2)0.0013 (2)0.0076 (3)
O1'0.0215 (3)0.0338 (4)0.0283 (3)0.0016 (3)0.0127 (2)0.0040 (3)
O6'0.0260 (3)0.0352 (4)0.0329 (3)0.0002 (3)0.0117 (3)0.0068 (3)
C3'0.0160 (2)0.0172 (3)0.0172 (2)0.0007 (2)0.00456 (19)0.0014 (2)
O60.0428 (4)0.0337 (4)0.0238 (3)0.0067 (3)0.0152 (3)0.0049 (3)
C20.0191 (3)0.0200 (3)0.0174 (2)0.0018 (2)0.0036 (2)0.0013 (2)
C5'0.0171 (3)0.0181 (3)0.0232 (3)0.0021 (2)0.0062 (2)0.0006 (2)
C50.0236 (3)0.0203 (3)0.0194 (3)0.0024 (3)0.0061 (2)0.0011 (2)
O30.0498 (5)0.0266 (3)0.0342 (4)0.0186 (3)0.0218 (4)0.0099 (3)
C30.0287 (4)0.0179 (3)0.0192 (3)0.0034 (3)0.0085 (3)0.0009 (2)
C4'0.0149 (2)0.0193 (3)0.0197 (3)0.0002 (2)0.0041 (2)0.0017 (2)
C1'0.0162 (3)0.0220 (3)0.0272 (3)0.0038 (2)0.0064 (2)0.0023 (3)
C40.0299 (4)0.0161 (3)0.0237 (3)0.0008 (3)0.0101 (3)0.0006 (2)
C60.0257 (4)0.0308 (4)0.0301 (4)0.0001 (3)0.0126 (3)0.0064 (3)
C6'0.0253 (4)0.0302 (4)0.0276 (4)0.0024 (3)0.0126 (3)0.0032 (3)
O40.0482 (5)0.0186 (3)0.0637 (6)0.0088 (3)0.0256 (5)0.0069 (4)
Geometric parameters (Å, º) top
O5—C11.4134 (9)O6—H60.86 (3)
O5—C51.4433 (11)C2—H2A0.9800
O1—C11.4271 (9)C2—C31.5229 (13)
O1—C2'1.4330 (9)C5'—H5'0.9800
O2'—C2'1.4105 (9)C5'—C4'1.5267 (12)
O2'—C5'1.4489 (10)C5'—C6'1.5135 (12)
O2—C21.4276 (11)C5—H50.9800
O2—H20.87 (3)C5—C41.5242 (13)
O3'—C3'1.4075 (10)C5—C61.5265 (12)
O3'—H3'0.79 (2)O3—C31.4293 (12)
C1—H10.9800O3—H30.82 (3)
C1—C21.5348 (11)C3—H3A0.9800
C2'—C3'1.5423 (10)C3—C41.5253 (12)
C2'—C1'1.5230 (10)C4'—H4'A0.9800
O4'—C4'1.4247 (10)C1'—H1'A0.9700
O4'—H4'0.85 (2)C1'—H1'B0.9700
O1'—C1'1.4272 (12)C4—H40.9800
O1'—H1'0.78 (3)C4—O41.4135 (13)
O6'—C6'1.4278 (15)C6—H6A0.9700
O6'—H6'0.89 (3)C6—H6B0.9700
C3'—H3'A0.9800C6'—H6'A0.9700
C3'—C4'1.5244 (10)C6'—H6'B0.9700
O6—C61.4200 (14)O4—H4A0.74 (4)
C1—O5—C5115.69 (6)C4—C5—H5109.4
C1—O1—C2'113.94 (6)C4—C5—C6112.15 (7)
C2'—O2'—C5'111.53 (6)C6—C5—H5109.4
C2—O2—H2110.7 (16)C3—O3—H3114.6 (19)
C3'—O3'—H3'109.6 (14)C2—C3—H3A109.8
O5—C1—O1110.34 (6)C2—C3—C4108.15 (7)
O5—C1—H1108.4O3—C3—C2111.43 (9)
O5—C1—C2110.98 (6)O3—C3—H3A109.8
O1—C1—H1108.4O3—C3—C4107.88 (7)
O1—C1—C2110.13 (6)C4—C3—H3A109.8
C2—C1—H1108.4O4'—C4'—C3'112.37 (7)
O1—C2'—C3'108.23 (6)O4'—C4'—C5'111.58 (7)
O1—C2'—C1'110.15 (6)O4'—C4'—H4'A110.1
O2'—C2'—O1110.98 (6)C3'—C4'—C5'102.36 (6)
O2'—C2'—C3'105.16 (6)C3'—C4'—H4'A110.1
O2'—C2'—C1'107.16 (6)C5'—C4'—H4'A110.1
C1'—C2'—C3'115.07 (6)C2'—C1'—H1'A109.4
C4'—O4'—H4'104.5 (17)C2'—C1'—H1'B109.4
C1'—O1'—H1'107.4 (16)O1'—C1'—C2'111.04 (7)
C6'—O6'—H6'107.3 (19)O1'—C1'—H1'A109.4
O3'—C3'—C2'115.78 (7)O1'—C1'—H1'B109.4
O3'—C3'—H3'A107.6H1'A—C1'—H1'B108.0
O3'—C3'—C4'115.35 (7)C5—C4—C3110.71 (7)
C2'—C3'—H3'A107.6C5—C4—H4109.2
C4'—C3'—C2'102.52 (6)C3—C4—H4109.2
C4'—C3'—H3'A107.6O4—C4—C5105.68 (9)
C6—O6—H6108.5 (16)O4—C4—C3112.75 (8)
O2—C2—C1110.21 (7)O4—C4—H4109.2
O2—C2—H2A108.5O6—C6—C5111.56 (8)
O2—C2—C3110.18 (7)O6—C6—H6A109.3
C1—C2—H2A108.5O6—C6—H6B109.3
C3—C2—C1111.00 (7)C5—C6—H6A109.3
C3—C2—H2A108.5C5—C6—H6B109.3
O2'—C5'—H5'108.8H6A—C6—H6B108.0
O2'—C5'—C4'105.66 (6)O6'—C6'—C5'113.07 (8)
O2'—C5'—C6'109.72 (7)O6'—C6'—H6'A109.0
C4'—C5'—H5'108.8O6'—C6'—H6'B109.0
C6'—C5'—H5'108.8C5'—C6'—H6'A109.0
C6'—C5'—C4'115.01 (7)C5'—C6'—H6'B109.0
O5—C5—H5109.4H6'A—C6'—H6'B107.8
O5—C5—C4110.81 (7)C4—O4—H4A109 (3)
O5—C5—C6105.65 (8)
O5—C1—C2—O2177.24 (7)C1—C2—C3—C456.04 (8)
O5—C1—C2—C354.88 (8)C2'—O1—C1—O5108.00 (7)
O5—C5—C4—C355.19 (9)C2'—O1—C1—C2129.14 (7)
O5—C5—C4—O4177.56 (8)C2'—O2'—C5'—C4'8.07 (9)
O5—C5—C6—O656.89 (10)C2'—O2'—C5'—C6'132.61 (8)
O1—C1—C2—O254.75 (9)C2'—C3'—C4'—O4'154.83 (7)
O1—C1—C2—C367.60 (8)C2'—C3'—C4'—C5'35.01 (8)
O1—C2'—C3'—O3'38.93 (8)C3'—C2'—C1'—O1'72.06 (9)
O1—C2'—C3'—C4'87.53 (7)C2—C3—C4—C556.46 (9)
O1—C2'—C1'—O1'50.60 (9)C2—C3—C4—O4174.61 (9)
O2'—C2'—C3'—O3'157.60 (6)C5'—O2'—C2'—O1102.24 (7)
O2'—C2'—C3'—C4'31.14 (8)C5'—O2'—C2'—C3'14.57 (8)
O2'—C2'—C1'—O1'171.41 (7)C5'—O2'—C2'—C1'137.47 (7)
O2'—C5'—C4'—O4'147.62 (7)C5—O5—C1—O167.67 (8)
O2'—C5'—C4'—C3'27.25 (8)C5—O5—C1—C254.69 (9)
O2'—C5'—C6'—O6'69.72 (10)O3—C3—C4—C5177.11 (8)
O2—C2—C3—O363.18 (9)O3—C3—C4—O464.74 (12)
O2—C2—C3—C4178.42 (7)C4'—C5'—C6'—O6'49.21 (11)
O3'—C3'—C4'—O4'78.43 (9)C1'—C2'—C3'—O3'84.74 (9)
O3'—C3'—C4'—C5'161.75 (7)C1'—C2'—C3'—C4'148.80 (7)
C1—O5—C5—C455.18 (9)C4—C5—C6—O663.92 (11)
C1—O5—C5—C6176.86 (7)C6—C5—C4—C3172.97 (8)
C1—O1—C2'—O2'44.86 (8)C6—C5—C4—O464.65 (10)
C1—O1—C2'—C3'159.77 (6)C6'—C5'—C4'—O4'91.21 (9)
C1—O1—C2'—C1'73.64 (8)C6'—C5'—C4'—C3'148.42 (7)
C1—C2—C3—O3174.45 (6)

Experimental details

Crystal data
Chemical formulaC12H22O11
Mr342.29
Crystal system, space groupMonoclinic, P21
Temperature (K)298
a, b, c (Å)7.7630 (1), 8.7109 (1), 10.8701 (1)
β (°) 102.937 (1)
V3)716.41 (1)
Z2
Radiation typeMo Kα
µ (mm1)0.14
Crystal size (mm)0.2 × 0.2 × 0.1
Data collection
DiffractometerBruker APEX-II CCD
Absorption correctionMulti-scan
SADABS2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0783 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.9421. The λ/2 correction factor is 0.0015.
Tmin, Tmax0.814, 0.864
No. of measured, independent and
observed [I > 2σ(I)] reflections
85318, 16720, 10732
Rint0.053
(sin θ/λ)max1)1.122
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.110, 0.97
No. of reflections16720
No. of parameters240
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.42, 0.27
Absolute structureFlack x determined using 3930 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
Absolute structure parameter0.10 (17)

Computer programs: SAINT v8.27A (Bruker, 2012), olex2.solve (Bourhis et al., 2015), SHELXL (Sheldrick, 2008), Olex2 (Dolomanov et al., 2009).

 

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