sucrose very-fast

Crystal Structure Report for sucrose very-fast


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 4050 reflections to a maximum θ angle of 59.97° (0.89 Å resolution), of which 1851 were independent (average redundancy 2.188, completeness = 92.9%, Rint = 3.35%, Rsig = 4.17%) and 1798 (97.14%) were greater than 2σ(F2). The final cell constants of a = 7.7182(5) Å, b = 8.6588(5) Å, c = 10.7996(8) Å, β = 102.914(5)°, volume = 703.49(8) 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 274 variables converged at R1 = 2.68%, for the observed data and wR2 = 6.96% for all data. The goodness-of-fit was 1.128. The largest peak in the final difference electron density synthesis was 0.192 e-3 and the largest hole was -0.163 e-3 with an RMS deviation of 0.039 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 very-fast.
Identification codesucrose very-fast
Chemical formulaC12H22O11
Formula weight342.30
Temperature110(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 = 7.7182(5) Åα = 90°
b = 8.6588(5) Åβ = 102.914(5)°
c = 10.7996(8) Åγ = 90°
Volume703.49(8) 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 very-fast.
DiffractometerBruker-AXS Duo
Radiation sourceMicro-source, Copper
Theta range for data collection4.20 to 59.97°
Index ranges-8<=h<=8, -9<=k<=9, -10<=l<=11
Reflections collected4050
Independent reflections1851 [R(int) = 0.0335]
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 / parameters1851 / 1 / 274
Goodness-of-fit on F21.128
Final R indices1798 data; I>2σ(I)R1 = 0.0268, wR2 = 0.0687
all dataR1 = 0.0278, wR2 = 0.0696
Weighting schemew=1/[σ2(Fo2)+(0.0393P)2+0.0000P]
where P=(Fo2+2Fc2)/3
Absolute structure parameter0.2(2)
Largest diff. peak and hole0.192 and -0.163 eÅ-3
R.M.S. deviation from mean0.039 eÅ-3


Table 3. Atomic coordinates and equivalent isotropic atomic displacement parameters (Å2) for sucrose very-fast.
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
x/ay/bz/cU(eq)
O10.8546(2)0.8125(2)0.34934(19)0.0244(4)
O20.8688(2)0.22902(17)0.37809(15)0.0163(4)
O30.8920(2)0.27939(16)0.17113(14)0.0137(4)
O40.81941(19)0.53355(18)0.21233(15)0.0160(4)
O50.5415(2)0.38868(19)0.32773(17)0.0192(4)
O60.7874(2)0.0819(2)0.58368(17)0.0208(4)
O70.2049(2)0.8775(2)0.30899(18)0.0219(4)
O80.2508(2)0.1917(2)0.22918(18)0.0189(4)
O90.4094(2)0.53341(19)0.97866(16)0.0186(4)
O100.7026(2)0.30987(19)0.92422(16)0.0179(4)
O110.1223(2)0.38861(19)0.02753(17)0.0186(4)
C10.9436(4)0.9559(3)0.3752(3)0.0169(5)
C20.7955(3)0.0751(3)0.3601(2)0.0167(6)
C30.9866(3)0.2694(3)0.3001(2)0.0139(5)
C40.8696(3)0.4351(2)0.1231(2)0.0147(5)
C50.6300(3)0.5675(3)0.1773(2)0.0161(5)
C60.5497(3)0.5465(3)0.2908(3)0.0192(6)
C70.6847(3)0.0560(3)0.4590(2)0.0186(6)
C80.0654(3)0.9895(3)0.2855(2)0.0177(6)
C90.1380(3)0.1524(3)0.3139(3)0.0157(5)
C100.7147(3)0.4373(3)0.0064(2)0.0154(5)
C110.5544(3)0.4631(3)0.0650(2)0.0159(5)
C120.0454(3)0.4950(3)0.1013(3)0.0166(5)


Table 4. Bond lengths (Å) for sucrose very-fast.
O1-C11.416(3)O1-H10.72(3)
O2-C31.414(3)O2-C21.444(3)
O3-C31.423(3)O3-C41.441(3)
O4-C41.404(3)O4-C51.456(3)
O5-C61.429(3)O5-H50.89(3)
O6-C71.419(3)O6-H60.77(3)
O7-C81.429(3)O7-H70.76(3)
O8-C91.438(3)O8-H80.78(3)
O9-C111.424(3)O9-H90.85(3)
O10-C101.407(3)O10-H100.85(3)
O11-C121.430(3)O11-H110.75(3)
C1-C21.521(3)C1-C81.522(3)
C1-H1A0.94(3)C2-C71.519(3)
C2-H20.97(3)C3-C91.529(3)
C3-H30.91(3)C4-C121.519(3)
C4-C101.531(4)C5-C61.502(4)
C5-C111.521(3)C5-H5A0.94(3)
C6-H6A1.03(3)C6-H6B0.96(3)
C7-H7A1.04(3)C7-H7B1.03(3)
C8-C91.523(3)C8-H8A1.06(3)
C9-H9A0.98(3)C10-C111.527(3)
C10-H10A1.00(3)C11-H11A0.97(3)
C12-H12A1.04(3)C12-H12B1.00(3)


Table 5. Bond angles (°) for sucrose very-fast.
C1-O1-H1118.(3)C3-O2-C2115.65(17)
C3-O3-C4113.77(17)C4-O4-C5111.07(18)
C6-O5-H5108.8(18)C7-O6-H6107.(2)
C8-O7-H7111.(3)C9-O8-H8104.(2)
C11-O9-H9108.(2)C10-O10-H10110.(2)
C12-O11-H11101.(2)O1-C1-C2104.7(2)
O1-C1-C8112.5(2)C2-C1-C8111.0(2)
O1-C1-H1A113.3(18)C2-C1-H1A108.9(17)
C8-C1-H1A106.5(16)O2-C2-C7105.74(19)
O2-C2-C1110.44(19)C7-C2-C1112.2(2)
O2-C2-H2109.5(17)C7-C2-H2109.5(16)
C1-C2-H2109.3(17)O2-C3-O3109.90(19)
O2-C3-C9110.92(17)O3-C3-C9110.49(19)
O2-C3-H3105.4(17)O3-C3-H3110.0(18)
C9-C3-H3110.0(17)O4-C4-O3110.52(17)
O4-C4-C12106.98(18)O3-C4-C12109.63(18)
O4-C4-C10105.80(18)O3-C4-C10108.48(17)
C12-C4-C10115.3(2)O4-C5-C6109.7(2)
O4-C5-C11105.73(18)C6-C5-C11115.09(19)
O4-C5-H5A109.1(17)C6-C5-H5A108.2(16)
C11-C5-H5A108.9(17)O5-C6-C5113.29(19)
O5-C6-H6A109.4(17)C5-C6-H6A112.1(16)
O5-C6-H6B103.8(17)C5-C6-H6B111.6(17)
H6A-C6-H6B106.(2)O6-C7-C2111.53(19)
O6-C7-H7A112.6(17)C2-C7-H7A109.9(16)
O6-C7-H7B114.7(17)C2-C7-H7B107.0(15)
H7A-C7-H7B100.(2)O7-C8-C9111.4(2)
O7-C8-C1107.7(2)C9-C8-C1107.5(2)
O7-C8-H8A112.9(15)C9-C8-H8A108.3(15)
C1-C8-H8A108.9(14)O8-C9-C8109.8(2)
O8-C9-C3109.83(19)C8-C9-C3110.8(2)
O8-C9-H9A108.0(16)C8-C9-H9A108.6(16)
C3-C9-H9A109.8(16)O10-C10-C11115.5(2)
O10-C10-C4116.03(18)C11-C10-C4102.54(19)
O10-C10-H10A107.9(15)C11-C10-H10A109.0(15)
C4-C10-H10A105.3(16)O9-C11-C5111.91(19)
O9-C11-C10112.5(2)C5-C11-C10102.42(19)
O9-C11-H11A113.2(16)C5-C11-H11A106.9(17)
C10-C11-H11A109.1(16)O11-C12-C4111.26(19)
O11-C12-H12A109.7(15)C4-C12-H12A106.3(17)
O11-C12-H12B110.6(16)C4-C12-H12B109.3(16)
H12A-C12-H12B110.(2)


Table 6. Torsion angles (°) for sucrose very-fast.
C3-O2-C2-C7176.44(19)C3-O2-C2-C154.8(3)
O1-C1-C2-O2-177.19(19)C8-C1-C2-O2-55.5(3)
O1-C1-C2-C765.1(3)C8-C1-C2-C7-173.2(2)
C2-O2-C3-O367.6(2)C2-O2-C3-C9-54.9(3)
C4-O3-C3-O2108.09(19)C4-O3-C3-C9-129.18(19)
C5-O4-C4-O3-102.5(2)C5-O4-C4-C12138.22(19)
C5-O4-C4-C1014.7(2)C3-O3-C4-O4-44.1(2)
C3-O3-C4-C1273.6(2)C3-O3-C4-C10-159.66(17)
C4-O4-C5-C6132.38(19)C4-O4-C5-C117.7(2)
O4-C5-C6-O5-70.1(2)C11-C5-C6-O548.9(3)
O2-C2-C7-O6-56.7(2)C1-C2-C7-O663.8(3)
O1-C1-C8-O7-65.5(3)C2-C1-C8-O7177.5(2)
O1-C1-C8-C9174.3(2)C2-C1-C8-C957.4(3)
O7-C8-C9-O863.7(3)C1-C8-C9-O8-178.5(2)
O7-C8-C9-C3-174.82(19)C1-C8-C9-C3-57.0(3)
O2-C3-C9-O8177.18(19)O3-C3-C9-O855.1(3)
O2-C3-C9-C855.7(3)O3-C3-C9-C8-66.4(2)
O4-C4-C10-O10-157.79(17)O3-C4-C10-O10-39.2(3)
C12-C4-C10-O1084.2(2)O4-C4-C10-C11-31.0(2)
O3-C4-C10-C1187.6(2)C12-C4-C10-C11-149.00(19)
O4-C5-C11-O9-147.40(18)C6-C5-C11-O991.4(2)
O4-C5-C11-C10-26.7(2)C6-C5-C11-C10-147.9(2)
O10-C10-C11-O9-78.0(3)C4-C10-C11-O9154.87(17)
O10-C10-C11-C5161.71(19)C4-C10-C11-C534.5(2)
O4-C4-C12-O11170.66(19)O3-C4-C12-O1150.8(3)
C10-C4-C12-O11-72.0(2)


Table 7. Anisotropic atomic displacement parameters (Å2) for sucrose very-fast.
The anisotropic atomic displacement factor exponent takes the form: -2π2[ h2 a*2 U11 + ... + 2 h k a* b* U12 ]
U11U22U33U23U13U12
O10.0269(11)0.0138(8)0.0345(12)-0.0029(8)0.0113(9)-0.0024(7)
O20.0185(10)0.0152(8)0.0162(10)-0.0011(6)0.0062(8)-0.0004(6)
O30.0162(9)0.0116(7)0.0127(10)0.0005(6)0.0022(8)-0.0013(6)
O40.0138(9)0.0174(8)0.0172(9)-0.0037(6)0.0042(8)0.0017(6)
O50.0184(10)0.0201(8)0.0204(10)0.0038(7)0.0069(8)0.0015(7)
O60.0271(11)0.0184(8)0.0185(10)0.0019(7)0.0084(9)0.0049(7)
O70.0277(11)0.0186(8)0.0225(11)0.0025(8)0.0123(9)0.0083(7)
O80.0161(10)0.0212(9)0.0205(11)-0.0004(7)0.0063(8)-0.0024(7)
O90.0127(9)0.0224(8)0.0196(10)0.0019(7)0.0014(8)-0.0009(7)
O100.0205(9)0.0163(8)0.0170(10)-0.0015(7)0.0045(8)-0.0010(7)
O110.0177(10)0.0198(8)0.0200(11)0.0017(7)0.0077(8)0.0002(7)
C10.0210(15)0.0161(11)0.0132(14)-0.0011(9)0.0034(11)-0.0007(10)
C20.0173(15)0.0177(11)0.0142(15)-0.0003(10)0.0019(12)-0.0040(9)
C30.0164(13)0.0158(11)0.0096(14)-0.0001(9)0.0031(11)-0.0022(9)
C40.0180(13)0.0111(11)0.0161(15)0.0011(9)0.0058(11)0.0023(9)
C50.0121(13)0.0132(12)0.0227(15)0.0008(10)0.0031(11)0.0033(9)
C60.0162(14)0.0201(13)0.0214(15)-0.0019(10)0.0045(12)0.0001(10)
C70.0173(14)0.0188(13)0.0203(16)0.0040(10)0.0053(13)0.0016(10)
C80.0185(14)0.0202(13)0.0137(14)0.0035(9)0.0017(12)0.0038(9)
C90.0160(14)0.0187(11)0.0126(15)0.0011(9)0.0036(12)-0.0025(9)
C100.0200(14)0.0123(11)0.0137(15)0.0003(9)0.0035(11)-0.0017(9)
C110.0156(14)0.0154(11)0.0170(14)0.0023(9)0.0044(11)0.0009(9)
C120.0130(14)0.0173(12)0.0192(16)-0.0008(10)0.0031(12)0.0004(9)


Table 8. Hydrogen atomic coordinates and isotropic atomic displacement parameters (Å2) for sucrose very-fast.
x/ay/bz/cU(eq)
H10.905(5)-0.253(4)0.335(3)0.037
H50.649(4)0.347(3)0.339(3)0.029
H60.774(4)0.167(4)0.601(3)0.031
H71.237(4)-0.140(4)0.249(3)0.033
H81.326(4)0.242(4)0.271(3)0.028
H90.315(4)0.486(4)-0.016(3)0.028
H100.684(4)0.228(4)-0.038(3)0.027
H111.150(4)0.325(4)0.075(3)0.028
H1A1.014(4)-0.037(3)0.458(3)0.025
H20.719(4)0.066(3)0.276(3)0.025
H31.031(3)0.364(4)0.328(3)0.021
H5A0.614(4)0.671(4)0.151(3)0.024
H6A0.615(4)0.610(4)0.368(3)0.029
H6B0.428(4)0.580(3)0.273(3)0.029
H7A0.573(4)0.127(3)0.437(3)0.028
H7B0.626(4)-0.051(4)0.445(3)0.028
H8A0.990(4)-0.013(3)0.191(3)0.027
H9A1.210(4)0.155(3)0.401(3)0.024
H10A0.734(3)0.531(4)-0.042(2)0.023
H11A0.523(4)0.366(3)0.100(3)0.024
H12A1.017(4)0.599(3)0.052(3)0.025
H12B1.128(4)0.514(3)0.185(3)0.025