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ORNA-P-815
JAN
ATIES
. CONF-650202-/
REFINEMENT OF THE STRUCTURE OF g-D-GLUCOSE
FROM NEUTRON DIFFRACTION DATA*
MASTER
George M. Brown and Henri A. Levy
Chemistry Division, Oak Ridge National Laboratory
Oak Ridge, Tennessee
From a crystal weighing 31.7 mg., 1656 intensity data were
measured, corrected for absorption, and converted to Fol2
values for use in least-squares refinement. The starting param-
eters used (including those of the 12 hydrogen atoms) and the o
unit-cell data (P2,2,21, a = 10.36 $ 0.02 AO, b = 14.84 0.02 A,
c = 4.97 $ 0.02 Aº, Z = 4T were from the work of McDonald and
Beevers (Acta Cryst., 5, 654 (1952)). In the final refinement
the 37 data of highest intensity were omitted from the set of
observations because they appear to show extinction errors. The
discrepancy index Rx - F.*-|FC|1/8|F1* is 0.060 for x - 1
and 0.059 for x = 2: The standard deviation of an observation
of unit weight is 1.10. The atomic coordinates and their least-
squares errors (both fractional x 104) are as follows:
-772(3
Atom
(1) 3329(1 600701
C(2) 4184(1 6746(1
C(3) 5611(1 6514 (1
C(4) 5860(1 5569(1
C(5) 4956 (1 4886(1
C(6) 5141(1 3953(1
O(1) 3470(2 6007(1
0(2) 3880(1 7598(1
0(3) 6334(1 7154 (1
0(4) 7176(1 5348(1
0(5) 3654(1 5154(1
0(6) 4458(2 3311(1
154(3
1200(3
-123 (3
1026 (4
-3541(4
-657 (5
1634(5
688(4
369(4
-518(5
Atom
H(1)
H(2)
H(3)
H(4)
H(5)
H(6)
H(7)
H(8)
H(9)
H(10)
(11)
(12)
2327(2 6124(2.
395813 6776(2
5888(3 6543 (2
5677(3 5565(2
5136 (3 4865 (2
6172(3 3792(2
4804(5 3947 (3
2753(4 5674 (3
4485(3 7776(2
7247(2 7137(2
751703 5082(3
4127(3 2861(2
-154(9
259907
-1995 (7
3385 (6
-2312(7
1032(12
3116 (9
-4299 (9
-203109
1178(8.
2326(8
699(10.
.
.
.
All bond lengths and a selection of bond angles are shown
in Fig. 1. The six conformation angles about the pyranose ring
bonds (see Brown and Levy, Science, 141, 921 (1983), for defini-
tion) are: C(1)--C(2), 54.T; 0(2)-13), -51.3°; C(3)--C(4),
53.3°; C(4) -- C(5), -57.5°; C(5)-0(5), 62.2°; 0(5) --C(1), -60.9º.
The oxygen-oxygen separations and the angles at the hydrogen
atoms in the five different hydrogen bonds are as follows:
0(1) H(8)...015), 2.847 A°, 161.0°; 0(2) --H(9)...0(6), 2.776 A,
170.1°; 0(3)—H(10)...0(2), 2.707 A°, 164.8°; 0(4)—H(1l)...0(4),
2.773 A°, 167.7°; 0(6)-H(12)...0(3), 2.711 Aº, 169.7º. The
computed standard errors of these distances and angles, includ-
ing contributions from errors in the unit-cell parameters, are
as follows: C-C and C-O bonds, about 0.003 A0 (except 0.006 Aº
for c(1)-0(1)); C-H and 0-H bonds, 0.004 Aº to 0.006 Aº; bond
angles involving only carbon and oxygen atoms, 0.1° to 0.2°;
C-O-H angles, 0.2° to 0.4°; conformation angles, 0.2° to 0.3°;
0-0 distances and 0-H-Q angles in hydrogen bonds, 0.004 Aº to
0.009 Aº and 0.3° to 4°, respectively.
- LEGAL NOTICE

The report mo popare u L Account of cornment sponsored work. Molther the Vallad
main, nor the comboioa, hor my person sou on behalf of the Commission:
A. Maar my vorreoty or repremuu, .. Qxprend or lopund, nu respect to the acro-
racy, completo, 01' wefalms of the labor mauon contained la W, roport, or the wee
of my tutoratom, imenduo, anthod, or procw. dixcloudlu we report na Box Intriago
peintly mad righto; or
A. Aww way liabiliter mit nepect to the wes of, or for damages moeuling from the
m amy Internation, apparato, wobod, or moceur declined in ws report.
As westhe homewrno scono il of the Commission" wolne my .
close or canctor de Coaninou, or employee of weed contractor, to the ormt ut
med flere or contrector of Connials, or uplone ol must contractor propr.,
da
, of mortdw nocWw ho, w halorealio pirmat to Woorlopinat or contract
mu the Commission, or MI Omployant muni contractor.
Research sponsored by the U. S. Atomic Energy Commission under
contract with the Union Carbide Corporation.
Fig. 1. Bond lengths and bond angles in a-D-glucose.
No corrections for thermal motion have been made.
.
UNCLASSIFIED
ORNL. DWG. 64.5559A

112.40
107.0°
110.99108.3• 110.64-108.99
111.2• 109.80
108.7°
111.10 112.3°
12.1°
2,17
T
U
110.4. 108.10 >
7110.8°
113.8° 110.00 109.40

(14)
OH (1C)
H(11)
0 0.974
10.973
O014) 0(3)
1.425
1.415
LOH(3)
H(6) H(4) Quozy 1.51991.106
1.5281
1.525
C(5) H(5) H(2) C12)
H7, Q-1.510 P Page 14250
11.413 1.427
11.534
H(9)
11.095
0.98
1.096 in C/6)
O(2)
De
0.964016
1.426
MCCA
_1426
0(5)
1.095
1.389
Dom
0.969
014)
H(12)
Hlay
OH (8)

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- LEGAL NOTICE
This report was prepared as an account of Government sponsored work. Neither the United
States, nor the Commission, nor any person acting on behalf of the Commission:
A. Makes any warranty or representation, expregsed or implied, with respect to the accu-
racy, completeness, or usefulness of the information contained in this report, or that the use
of any information, apparatus, method, or process disclosed in this report may not infringe
privately owned rights; or
B. Assumos any liabilities with respect to the use of, or for damages resulting from the
use of any information, apparatus, mothod, or process disclosed in this report.
As used in the above, "person acting ou behalf of the Cummission” includes any em-
ployee or contractor of the Commission, or employee of such contractor, to the extent that
such employee or contractor of the Commission, or employee of such contractor prepares,
disseminates, or provides access to, any information pursuant to his employment or contract
with the Commission, or his employment with such contractor.
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