sucrose fast- high-redundancy

Crystal Structure Report for sucrose fast- high-redundancy


A specimen of C12H22O11, approximate dimensions 0.05 mm x 0.05 mm x 0.10 mm, was used for the X-ray crystallographic analysis. The X-ray intensity data were measured on a Bruker-AXS Duo system equipped with a Quasar mirror monochromator and a Copper Micro-source (λ = 1.54178 Å).

The frames were integrated with the Bruker SAINT software package using a narrow-frame algorithm. The integration of the data using a monoclinic unit cell yielded a total of 21316 reflections to a maximum θ angle of 67.22° (0.84 Å resolution), of which 2395 were independent (average redundancy 8.900, completeness = 96.5%, Rint = 3.91%, Rsig = 2.11%) and 2364 (98.71%) were greater than 2σ(F2). The final cell constants of a = 7.7128(5) Å, b = 8.6620(5) Å, c = 10.8084(6) Å, β = 102.983(3)°, volume = 703.63(7) Å3, are based upon the refinement of the XYZ-centroids of reflections above 20 σ(I). Data were corrected for absorption effects using the multi-scan method (SADABS). The calculated minimum and maximum transmission coefficients (based on crystal size) are 0.8842 and 0.9396.

The structure was solved and refined using the Bruker SHELXTL Software Package, using the space group P 1 21 1, with Z = 2 for the formula unit, C12H22O11. The final anisotropic full-matrix least-squares refinement on F2 with 296 variables converged at R1 = 2.11%, for the observed data and wR2 = 5.25% for all data. The goodness-of-fit was 1.011. The largest peak in the final difference electron density synthesis was 0.143 e-3 and the largest hole was -0.166 e-3 with an RMS deviation of 0.036 e-3. On the basis of the final model, the calculated density was 1.616 g/cm3 and F(000), 364 e-.





Table 1. Sample and crystal data for sucrose fast- high-redundancy.
Identification codesucrose fast- high-redundancy
Chemical formulaC12H22O11
Formula weight342.30
Temperature100(2) K
Wavelength1.54178 Å
Crystal size0.05 x 0.05 x 0.10 mm
Crystal systemmonoclinic
Space groupP 1 21 1
Unit cell dimensionsa = 7.7128(5) Åα = 90°
b = 8.6620(5) Åβ = 102.983(3)°
c = 10.8084(6) Åγ = 90°
Volume703.63(7) Å3
Z2
Density (calculated)1.616 Mg/cm3
Absorption coefficient1.261 mm-1
F(000)364


Table 2. Data collection and structure refinement for sucrose fast- high-redundancy.
DiffractometerBruker-AXS Duo
Radiation sourceMicro-source, Copper
Theta range for data collection4.20 to 67.22°
Index ranges-9<=h<=9, -10<=k<=10, -10<=l<=12
Reflections collected21316
Independent reflections2395 [R(int) = 0.0391]
Absorption correctionmulti-scan
Max. and min. transmission0.9396 and 0.8842
Structure solution techniquedirect methods
Structure solution programSHELXS-97 (Sheldrick, 1990)
Refinement methodFull-matrix least-squares on F2
Refinement programSHELXL-97 (Sheldrick, 1997)
Function minimizedΣ w(Fo2 - Fc2)2
Data / restraints / parameters2395 / 1 / 296
Goodness-of-fit on F21.011
Final R indices2364 data; I>2σ(I)R1 = 0.0211, wR2 = 0.0522
all dataR1 = 0.0216, wR2 = 0.0525
Weighting schemew=1/[σ2(Fo2)+(0.0300P)2+0.1647P]
where P=(Fo2+2Fc2)/3
Absolute structure parameter0.1(1)
Largest diff. peak and hole0.143 and -0.166 eÅ-3
R.M.S. deviation from mean0.036 eÅ-3


Table 3. Atomic coordinates and equivalent isotropic atomic displacement parameters (Å2) for sucrose fast- high-redundancy.
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
x/ay/bz/cU(eq)
O10.71260(15)0.11337(14)0.91599(10)0.0197(2)
O20.63114(13)0.26022(11)0.12165(9)0.0154(2)
O30.60826(12)0.31069(11)0.32933(8)0.0137(2)
O40.68097(12)0.56518(12)0.28762(9)0.0152(2)
O50.95893(14)0.41964(13)0.17246(10)0.0190(2)
O60.64484(15)0.84286(13)0.15061(11)0.0226(2)
O70.09084(14)0.56486(13)0.52146(9)0.0177(2)
O80.79784(13)0.34120(13)0.57586(9)0.0164(2)
O90.37748(13)0.41950(13)0.47204(9)0.0175(2)
O100.24912(14)0.22320(13)0.27067(10)0.0175(2)
O110.29456(14)0.90866(13)0.19109(10)0.0208(2)
C10.8158(2)0.08705(18)0.04114(14)0.0183(3)
C20.70435(19)0.10629(17)0.13983(13)0.0162(3)
C30.51279(19)0.30072(17)0.19974(12)0.0140(3)
C40.62904(18)0.46624(16)0.37661(13)0.0142(3)
C50.86997(18)0.59894(17)0.32275(13)0.0151(3)
C60.9509(2)0.57798(17)0.20910(14)0.0181(3)
C70.5563(2)0.98689(18)0.12475(14)0.0168(3)
C80.94525(18)0.49395(17)0.43484(13)0.0148(3)
C90.78589(18)0.46933(16)0.49390(13)0.0141(3)
C100.45394(19)0.52663(17)0.39830(13)0.0154(3)
C110.3624(2)0.18363(18)0.18670(14)0.0156(3)
C120.4338(2)0.02074(17)0.21415(13)0.0160(3)


Table 4. Bond lengths (Å) for sucrose fast- high-redundancy.
O1-C11.4252(19)O1-H10.84(3)
O2-C31.4195(17)O2-C21.4441(18)
O3-C31.4311(16)O3-C41.4371(17)
O4-C41.4118(17)O4-C51.4512(17)
O5-C61.4327(19)O5-H50.86(3)
O6-C71.4194(19)O6-H60.80(3)
O7-C81.4290(17)O7-H70.85(2)
O8-C91.4102(17)O8-H80.87(3)
O9-C101.4336(17)O9-H90.88(3)
O10-C111.4355(18)O10-H100.87(3)
O11-C121.4277(18)O11-H110.83(2)
C1-C21.522(2)C1-H1A0.972(19)
C1-H1B0.984(18)C2-C71.522(2)
C2-H20.967(15)C3-C111.523(2)
C3-H30.937(17)C4-C101.515(2)
C4-C91.5435(19)C5-C61.509(2)
C5-C81.5218(19)C5-H5A0.948(19)
C6-H6A1.023(19)C6-H6B1.000(19)
C7-C121.524(2)C7-H7A0.961(15)
C8-C91.522(2)C8-H8A0.952(16)
C9-H9A1.010(17)C10-H10A0.991(18)
C10-H10B1.005(14)C11-C121.520(2)
C11-H11A0.981(15)C12-H120.983(17)


Table 5. Bond angles (°) for sucrose fast- high-redundancy.
C1-O1-H1109.9(16)C3-O2-C2115.55(11)
C3-O3-C4113.35(10)C4-O4-C5111.48(10)
C6-O5-H5108.2(17)C7-O6-H6110.8(19)
C8-O7-H7105.1(16)C9-O8-H8109.2(14)
C10-O9-H9105.5(14)C11-O10-H10107.8(15)
C12-O11-H11111.4(16)O1-C1-C2111.38(12)
O1-C1-H1A110.6(10)C2-C1-H1A110.1(10)
O1-C1-H1B110.1(9)C2-C1-H1B107.8(9)
H1A-C1-H1B106.7(13)O2-C2-C7110.61(11)
O2-C2-C1105.72(12)C7-C2-C1112.26(12)
O2-C2-H2111.0(10)C7-C2-H2108.5(9)
C1-C2-H2108.7(9)O2-C3-O3109.80(11)
O2-C3-C11111.01(11)O3-C3-C11110.14(11)
O2-C3-H3105.4(9)O3-C3-H3110.7(9)
C11-C3-H3109.7(9)O4-C4-O3110.67(10)
O4-C4-C10107.16(11)O3-C4-C10110.29(11)
O4-C4-C9105.01(11)O3-C4-C9108.21(11)
C10-C4-C9115.37(11)O4-C5-C6109.74(11)
O4-C5-C8105.61(11)C6-C5-C8115.00(12)
O4-C5-H5A106.4(10)C6-C5-H5A108.0(10)
C8-C5-H5A111.7(9)O5-C6-C5113.06(12)
O5-C6-H6A109.9(10)C5-C6-H6A110.2(10)
O5-C6-H6B105.4(11)C5-C6-H6B109.7(10)
H6A-C6-H6B108.4(14)O6-C7-C2105.09(12)
O6-C7-C12112.55(12)C2-C7-C12110.99(12)
O6-C7-H7A111.7(10)C2-C7-H7A110.7(9)
C12-C7-H7A105.9(8)O7-C8-C5111.58(12)
O7-C8-C9112.04(11)C5-C8-C9102.59(11)
O7-C8-H8A110.3(9)C5-C8-H8A110.6(9)
C9-C8-H8A109.5(9)O8-C9-C8115.39(12)
O8-C9-C4115.52(11)C8-C9-C4102.46(11)
O8-C9-H9A106.3(9)C8-C9-H9A110.0(9)
C4-C9-H9A106.9(9)O9-C10-C4110.78(12)
O9-C10-H10A108.8(10)C4-C10-H10A107.9(10)
O9-C10-H10B111.2(8)C4-C10-H10B109.0(8)
H10A-C10-H10B109.0(13)O10-C11-C12110.11(12)
O10-C11-C3109.96(11)C12-C11-C3111.40(12)
O10-C11-H11A108.8(9)C12-C11-H11A108.6(9)
C3-C11-H11A107.9(9)O11-C12-C11111.82(12)
O11-C12-C7107.92(12)C11-C12-C7107.71(12)
O11-C12-H12110.8(10)C11-C12-H12109.1(10)
C7-C12-H12109.4(9)


Table 6. Torsion angles (°) for sucrose fast- high-redundancy.
C3-O2-C2-C754.76(14)C3-O2-C2-C1176.51(11)
O1-C1-C2-O2-56.60(15)O1-C1-C2-C764.08(16)
C2-O2-C3-O367.63(14)C2-O2-C3-C11-54.39(15)
C4-O3-C3-O2108.47(12)C4-O3-C3-C11-128.99(12)
C5-O4-C4-O3-101.79(12)C5-O4-C4-C10137.92(11)
C5-O4-C4-C914.76(14)C3-O3-C4-O4-44.97(14)
C3-O3-C4-C1073.43(14)C3-O3-C4-C9-159.53(11)
C4-O4-C5-C6132.40(12)C4-O4-C5-C87.89(15)
O4-C5-C6-O5-70.14(15)C8-C5-C6-O548.73(17)
O2-C2-C7-O6-177.29(11)C1-C2-C7-O664.90(14)
O2-C2-C7-C12-55.37(15)C1-C2-C7-C12-173.18(12)
O4-C5-C8-O7-147.37(11)C6-C5-C8-O791.48(15)
O4-C5-C8-C9-27.26(14)C6-C5-C8-C9-148.40(12)
O7-C8-C9-O8-78.63(15)C5-C8-C9-O8161.56(11)
O7-C8-C9-C4154.97(11)C5-C8-C9-C435.17(14)
O4-C4-C9-O8-157.57(11)O3-C4-C9-O8-39.35(15)
C10-C4-C9-O884.70(15)O4-C4-C9-C8-31.26(13)
O3-C4-C9-C886.96(13)C10-C4-C9-C8-148.98(12)
O4-C4-C10-O9170.91(10)O3-C4-C10-O950.38(15)
C9-C4-C10-O9-72.57(15)O2-C3-C11-O10177.43(11)
O3-C3-C11-O1055.61(15)O2-C3-C11-C1255.07(15)
O3-C3-C11-C12-66.75(14)O10-C11-C12-O1162.99(14)
C3-C11-C12-O11-174.73(11)O10-C11-C12-C7-178.60(11)
C3-C11-C12-C7-56.32(14)O6-C7-C12-O11-64.98(15)
C2-C7-C12-O11177.55(11)O6-C7-C12-C11174.13(12)
C2-C7-C12-C1156.67(14)


Table 7. Anisotropic atomic displacement parameters (Å2) for sucrose fast- high-redundancy.
The anisotropic atomic displacement factor exponent takes the form: -2π2[ h2 a*2 U11 + ... + 2 h k a* b* U12 ]
U11U22U33U23U13U12
O10.0255(6)0.0181(6)0.0166(5)-0.0020(4)0.0073(4)-0.0036(4)
O20.0173(5)0.0140(5)0.0162(5)0.0006(4)0.0067(4)0.0016(4)
O30.0164(5)0.0108(5)0.0137(5)-0.0005(4)0.0029(4)0.0004(4)
O40.0136(5)0.0155(5)0.0166(5)0.0039(4)0.0039(4)-0.0009(4)
O50.0180(5)0.0187(5)0.0216(5)-0.0027(5)0.0070(4)-0.0003(5)
O60.0250(6)0.0127(5)0.0326(6)0.0026(5)0.0115(5)0.0026(5)
O70.0143(5)0.0191(5)0.0194(5)-0.0027(4)0.0030(4)-0.0011(4)
O80.0193(5)0.0148(5)0.0156(5)0.0027(4)0.0049(4)0.0016(4)
O90.0180(5)0.0179(5)0.0183(5)-0.0010(5)0.0076(4)-0.0012(4)
O100.0162(5)0.0184(5)0.0190(5)-0.0004(4)0.0063(4)0.0004(4)
O110.0274(6)0.0169(5)0.0209(6)-0.0032(5)0.0111(4)-0.0087(4)
C10.0185(8)0.0173(8)0.0198(7)-0.0023(6)0.0058(6)0.0003(6)
C20.0181(8)0.0133(7)0.0168(7)-0.0004(6)0.0032(6)0.0038(6)
C30.0153(7)0.0142(7)0.0126(7)-0.0006(5)0.0036(5)0.0009(6)
C40.0179(7)0.0095(7)0.0158(7)-0.0006(5)0.0051(5)-0.0014(6)
C50.0134(7)0.0127(8)0.0196(7)0.0004(6)0.0047(5)-0.0014(5)
C60.0190(8)0.0169(8)0.0196(7)0.0010(6)0.0071(6)-0.0006(6)
C70.0206(7)0.0129(7)0.0176(7)0.0013(5)0.0055(6)0.0019(6)
C80.0145(7)0.0133(7)0.0167(7)-0.0025(6)0.0036(5)-0.0010(6)
C90.0165(7)0.0125(7)0.0140(7)-0.0008(5)0.0048(5)0.0004(6)
C100.0156(7)0.0137(7)0.0175(7)0.0001(6)0.0051(6)0.0005(6)
C110.0170(7)0.0167(7)0.0135(7)-0.0021(5)0.0040(5)0.0004(6)
C120.0197(7)0.0143(7)0.0144(7)-0.0015(5)0.0050(6)-0.0027(6)


Table 8. Hydrogen atomic coordinates and isotropic atomic displacement parameters (Å2) for sucrose fast- high-redundancy.
x/ay/bz/cU(eq)
H10.717(3)0.207(3)-0.103(2)0.051(7)
H50.853(3)0.383(3)0.156(2)0.053(7)
H60.575(4)-0.225(3)0.154(2)0.056(8)
H71.183(3)0.516(3)0.511(2)0.046(6)
H80.820(3)0.259(3)0.536(2)0.037(6)
H90.344(3)0.340(3)0.422(2)0.041(6)
H100.162(3)0.279(3)0.228(2)0.048(7)
H110.260(3)-0.111(3)0.257(2)0.041(6)
H1A0.918(2)0.156(2)0.0599(16)0.016(4)
H1B0.863(2)-0.019(2)0.0484(15)0.010(4)
H20.781(2)0.0950(19)0.2234(14)0.008(4)
H30.4662(19)0.397(2)0.1702(13)0.004(3)
H5A0.880(2)0.705(2)0.3462(14)0.013(4)
H6A0.882(2)0.641(2)0.1340(17)0.021(4)
H6B1.077(3)0.614(2)0.2301(15)0.020(4)
H7A0.4823(19)-0.0098(18)0.0404(14)0.007(4)
H8A0.9811(19)0.398(2)0.4062(14)0.006(3)
H9A0.768(2)0.563(2)0.5456(13)0.008(3)
H10A0.478(2)0.625(2)0.4456(15)0.015(4)
H10B0.3712(19)0.5469(18)0.3138(13)0.004(3)
H11A0.292(2)0.1877(18)0.0990(15)0.005(3)
H120.502(2)0.015(2)0.3025(16)0.014(4)