sucrose_40min_data_collection

Crystal Structure Report for sucrose_40min_data_collection


A specimen of C12H21O11, approximate dimensions 0.30 mm x 0.30 mm x 0.30 mm, was used for the X-ray crystallographic analysis. The X-ray intensity data were measured on a APEXII system equipped with a graphite monochromator and a MoKα sealed tube (λ = 0.71073 Å).

The total exposure time was 0.30 hours. 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 5821 reflections to a maximum θ angle of 28.12° (0.75 Å resolution), of which 3119 were independent (average redundancy 1.866, completeness = 93.6%, Rint = 3.61%, Rsig = 5.84%) and 2543 (81.53%) were greater than 2σ(F2). The final cell constants of a = 7.760(9) Å, b = 8.719(10) Å, c = 10.892(13) Å, β = 102.748(14)°, volume = 718.8(15) Å3, are based upon the refinement of the XYZ-centroids of 1976 reflections above 20 σ(I) with 5.382° < 2θ < 46.37°. Data were corrected for absorption effects using the multi-scan method (SADABS). The ratio of minimum to maximum apparent transmission was 0.666. The calculated minimum and maximum transmission coefficients (based on crystal size) are 0.9588 and 0.9588.

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, C12H21O11. The final anisotropic full-matrix least-squares refinement on F2 with 215 variables converged at R1 = 4.54%, for the observed data and wR2 = 10.21% for all data. The goodness-of-fit was 1.006. The largest peak in the final difference electron density synthesis was 0.194 e-3 and the largest hole was -0.237 e-3 with an RMS deviation of 0.051 e-3. On the basis of the final model, the calculated density was 1.577 g/cm3 and F(000), 362 e-.





Table 1. Sample and crystal data for sucrose_40min_data_collection.
Identification codesucrose_40min_data_collection
Chemical formulaC12H21O11
Formula weight341.29
Temperature110(2) K
Wavelength0.71073 Å
Crystal size0.30 x 0.30 x 0.30 mm
Crystal systemmonoclinic
Space groupP 1 21 1
Unit cell dimensionsa = 7.760(9) Åα = 90°
b = 8.719(10) Åβ = 102.748(14)°
c = 10.892(13) Åγ = 90°
Volume718.8(15) Å3
Z2
Density (calculated)1.577 Mg/cm3
Absorption coefficient0.142 mm-1
F(000)362


Table 2. Data collection and structure refinement for sucrose_40min_data_collection.
DiffractometerAPEXII
Radiation sourcesealed tube, MoKα
Theta range for data collection1.92 to 28.12°
Index ranges-10<=h<=10, -11<=k<=11, -13<=l<=14
Reflections collected5821
Independent reflections3119 [R(int) = 0.0361]
Coverage of independent reflections93.6%
Absorption correctionmulti-scan
Max. and min. transmission0.9588 and 0.9588
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 / parameters3119 / 1 / 215
Goodness-of-fit on F21.006
Final R indices2543 data; I>2σ(I)R1 = 0.0454, wR2 = 0.0975
all dataR1 = 0.0573, wR2 = 0.1021
Weighting schemew=1/[σ2(Fo2)+(0.0500P)2+0.0000P]
where P=(Fo2+2Fc2)/3
Absolute structure parameter0.1(11)
Largest diff. peak and hole0.194 and -0.237 eÅ-3
R.M.S. deviation from mean0.051 eÅ-3


Table 3. Atomic coordinates and equivalent isotropic atomic displacement parameters (Å2) for sucrose_40min_data_collection.
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
x/ay/bz/cU(eq)
O10.3551(3)0.6513(2)0.3483(2)0.0506(6)
O20.3687(2)0.23597(18)0.37764(16)0.0282(4)
O30.3917(2)0.18423(17)0.17178(14)0.0242(4)
O40.3159(2)0.9316(2)0.21219(15)0.0281(4)
O50.0393(3)0.0756(2)0.3269(2)0.0408(5)
O60.2860(3)0.3821(2)0.58151(17)0.0425(5)
O70.9107(2)0.9348(2)0.97818(17)0.0355(5)
O80.2048(2)0.1552(2)0.92566(15)0.0315(4)
O90.6204(3)0.0724(2)0.02978(17)0.0357(5)
O100.7473(3)0.2731(2)0.22891(18)0.0355(5)
O110.7030(3)0.5848(2)0.3094(2)0.0435(5)
C10.4432(4)0.5081(3)0.3742(3)0.0307(6)
C20.2951(4)0.3893(3)0.3592(2)0.0291(6)
C30.4852(4)0.1949(3)0.2998(2)0.0248(5)
C40.3696(3)0.0292(2)0.1239(2)0.0244(5)
C50.1279(3)0.8990(3)0.1760(2)0.0282(6)
C60.0477(4)0.9185(3)0.2890(3)0.0373(7)
C70.1849(4)0.4074(3)0.4571(2)0.0368(7)
C80.0552(3)0.0040(3)0.0647(2)0.0257(5)
C90.2149(3)0.0281(3)0.0073(2)0.0251(6)
C100.5431(3)0.9685(3)0.1033(2)0.0297(6)
C110.6354(4)0.3115(3)0.3134(2)0.0276(6)
C120.5637(4)0.4735(3)0.2862(2)0.0296(6)


Table 4. Bond lengths (Å) for sucrose_40min_data_collection.
O1-C11.421(3)O1-H10.84
O2-C31.415(3)O2-C21.450(3)
O3-C31.426(3)O3-C41.445(3)
O4-C41.413(3)O4-C51.453(3)
O5-C61.435(4)O5-H50.84
O6-C71.425(3)O7-C81.429(3)
O7-H70.84O8-C91.412(3)
O8-H80.84O9-C101.426(3)
O9-H90.84O10-C111.437(3)
O10-H100.84O11-C121.432(3)
O11-H110.84C1-C121.510(4)
C1-C21.529(4)C1-H1A1.0
C2-C71.516(4)C2-H21.0
C3-C111.529(4)C3-H31.0
C4-C101.509(4)C4-C91.543(4)
C5-C61.506(4)C5-C81.524(4)
C5-H5A1.0C6-H6A0.99
C6-H6B0.99C7-H7A0.99
C7-H7B0.99C8-C91.521(4)
C8-H8A1.0C9-H9A1.0
C10-H10A0.99C10-H10B0.99
C11-C121.523(4)C11-H11A1.0
C12-H121.0


Table 5. Bond angles (°) for sucrose_40min_data_collection.
C1-O1-H1109.5C3-O2-C2115.74(18)
C3-O3-C4114.08(17)C4-O4-C5111.23(19)
C6-O5-H5109.5C8-O7-H7109.5
C9-O8-H8109.5C10-O9-H9109.5
C11-O10-H10109.5C12-O11-H11109.5
O1-C1-C12112.8(2)O1-C1-C2104.9(2)
C12-C1-C2110.7(2)O1-C1-H1A109.4
C12-C1-H1A109.4C2-C1-H1A109.4
O2-C2-C7105.4(2)O2-C2-C1110.3(2)
C7-C2-C1112.5(2)O2-C2-H2109.6
C7-C2-H2109.6C1-C2-H2109.6
O2-C3-O3110.4(2)O2-C3-C11110.4(2)
O3-C3-C11110.55(19)O2-C3-H3108.5
O3-C3-H3108.5C11-C3-H3108.5
O4-C4-O3110.32(19)O4-C4-C10107.2(2)
O3-C4-C10110.1(2)O4-C4-C9105.3(2)
O3-C4-C9108.15(19)C10-C4-C9115.6(2)
O4-C5-C6109.1(2)O4-C5-C8105.76(19)
C6-C5-C8115.8(2)O4-C5-H5A108.7
C6-C5-H5A108.7C8-C5-H5A108.7
O5-C6-C5113.3(2)O5-C6-H6A108.9
C5-C6-H6A108.9O5-C6-H6B108.9
C5-C6-H6B108.9H6A-C6-H6B107.7
O6-C7-C2112.0(2)O6-C7-H7A109.2
C2-C7-H7A109.2O6-C7-H7B109.2
C2-C7-H7B109.2H7A-C7-H7B107.9
O7-C8-C9112.3(2)O7-C8-C5111.7(2)
C9-C8-C5102.6(2)O7-C8-H8A110.0
C9-C8-H8A110.0C5-C8-H8A110.0
O8-C9-C8115.5(2)O8-C9-C4116.0(2)
C8-C9-C4102.6(2)O8-C9-H9A107.4
C8-C9-H9A107.4C4-C9-H9A107.4
O9-C10-C4111.1(2)O9-C10-H10A109.4
C4-C10-H10A109.4O9-C10-H10B109.4
C4-C10-H10B109.4H10A-C10-H10B108.0
O10-C11-C12109.8(2)O10-C11-C3109.8(2)
C12-C11-C3111.1(2)O10-C11-H11A108.7
C12-C11-H11A108.7C3-C11-H11A108.7
O11-C12-C1107.6(2)O11-C12-C11111.4(2)
C1-C12-C11108.2(2)O11-C12-H12109.9
C1-C12-H12109.9C11-C12-H12109.9


Table 6. Torsion angles (°) for sucrose_40min_data_collection.
C3-O2-C2-C7-177.0(2)C3-O2-C2-C1-55.4(3)
O1-C1-C2-O2177.3(2)C12-C1-C2-O255.4(3)
O1-C1-C2-C7-65.4(3)C12-C1-C2-C7172.7(2)
C2-O2-C3-O3-67.3(2)C2-O2-C3-C1155.2(3)
C4-O3-C3-O2-108.4(2)C4-O3-C3-C11129.2(2)
C5-O4-C4-O3102.3(2)C5-O4-C4-C10-137.8(2)
C5-O4-C4-C9-14.1(2)C3-O3-C4-O445.1(3)
C3-O3-C4-C10-73.1(2)C3-O3-C4-C9159.76(19)
C4-O4-C5-C6-133.4(2)C4-O4-C5-C8-8.3(2)
O4-C5-C6-O570.7(3)C8-C5-C6-O5-48.5(3)
O2-C2-C7-O656.7(3)C1-C2-C7-O6-63.5(3)
O4-C5-C8-O7147.68(19)C6-C5-C8-O7-91.4(3)
O4-C5-C8-C927.2(2)C6-C5-C8-C9148.2(2)
O7-C8-C9-O878.0(3)C5-C8-C9-O8-161.90(19)
O7-C8-C9-C4-154.81(19)C5-C8-C9-C4-34.7(2)
O4-C4-C9-O8157.53(18)O3-C4-C9-O839.6(3)
C10-C4-C9-O8-84.3(3)O4-C4-C9-C830.7(2)
O3-C4-C9-C8-87.3(2)C10-C4-C9-C8148.9(2)
O4-C4-C10-O9-171.42(19)O3-C4-C10-O9-51.4(3)
C9-C4-C10-O971.5(3)O2-C3-C11-O10-176.91(18)
O3-C3-C11-O10-54.5(3)O2-C3-C11-C12-55.4(3)
O3-C3-C11-C1267.0(2)O1-C1-C12-O1165.4(3)
C2-C1-C12-O11-177.4(2)O1-C1-C12-C11-174.2(2)
C2-C1-C12-C11-57.0(3)O10-C11-C12-O11-63.5(3)
C3-C11-C12-O11174.9(2)O10-C11-C12-C1178.5(2)
C3-C11-C12-C156.9(3)


Table 7. Anisotropic atomic displacement parameters (Å2) for sucrose_40min_data_collection.
The anisotropic atomic displacement factor exponent takes the form: -2π2[ h2 a*2 U11 + ... + 2 h k a* b* U12 ]
U11U22U33U23U13U12
O10.0596(14)0.0203(9)0.0783(16)0.0074(10)0.0294(13)0.0085(10)
O20.0351(11)0.0201(8)0.0309(10)0.0012(7)0.0107(9)0.0012(8)
O30.0305(10)0.0144(8)0.0263(9)-0.0015(7)0.0033(8)0.0009(7)
O40.0272(10)0.0237(8)0.0320(9)0.0064(7)0.0034(8)-0.0012(8)
O50.0410(12)0.0365(10)0.0481(13)-0.0097(10)0.0167(11)-0.0029(9)
O60.0576(15)0.0399(11)0.0324(10)-0.0067(8)0.0152(10)-0.0059(10)
O70.0239(10)0.0374(10)0.0417(11)-0.0069(9)-0.0003(9)-0.0030(9)
O80.0391(11)0.0259(9)0.0295(10)0.0045(8)0.0075(9)0.0028(8)
O90.0354(11)0.0336(10)0.0414(11)-0.0034(9)0.0158(9)-0.0017(9)
O100.0337(11)0.0313(10)0.0425(12)-0.0008(9)0.0109(9)-0.0009(8)
O110.0598(14)0.0287(10)0.0481(13)-0.0090(9)0.0251(11)-0.0201(9)
C10.0421(17)0.0206(12)0.0300(14)0.0004(10)0.0092(12)0.0024(12)
C20.0321(16)0.0223(11)0.0326(14)-0.0003(11)0.0067(12)0.0054(11)
C30.0322(14)0.0176(11)0.0234(12)0.0015(10)0.0034(11)0.0016(10)
C40.0302(14)0.0137(10)0.0298(13)-0.0031(10)0.0080(12)-0.0007(10)
C50.0289(15)0.0176(12)0.0370(14)-0.0021(10)0.0052(12)-0.0039(10)
C60.0410(17)0.0321(16)0.0419(16)0.0013(12)0.0159(14)-0.0026(13)
C70.0417(18)0.0304(15)0.0391(16)-0.0063(12)0.0105(14)-0.0003(12)
C80.0237(13)0.0205(11)0.0315(14)-0.0036(10)0.0032(11)-0.0014(10)
C90.0293(14)0.0185(11)0.0286(14)-0.0016(10)0.0090(12)0.0017(10)
C100.0305(15)0.0243(13)0.0345(15)-0.0023(11)0.0071(12)0.0024(11)
C110.0307(15)0.0265(13)0.0245(13)-0.0020(10)0.0040(12)-0.0025(11)
C120.0379(16)0.0217(13)0.0289(14)-0.0007(10)0.0065(12)-0.0055(11)


Table 8. Hydrogen atomic coordinates and isotropic atomic displacement parameters (Å2) for sucrose_40min_data_collection.
x/ay/bz/cU(eq)
H10.42820.71900.33900.076
H50.14070.11450.33980.061
H7-0.1836-0.0200-0.01780.053
H80.16970.2324-0.04070.047
H90.66000.14920.07360.053
H100.83200.21900.26690.053
H110.73150.60670.24150.065
H1A0.51320.50720.46310.037
H20.21730.39760.27310.035
H30.53720.09220.32710.03
H5A0.1117-0.20990.14700.034
H6A-0.0732-0.12470.26950.045
H6B0.1183-0.14060.36020.045
H7A0.13450.51220.45150.044
H7B0.08550.33370.43910.044
H8A0.01740.10390.09530.031
H9A0.2279-0.0659-0.04260.03
H10A0.6253-0.04770.18570.036
H10B0.5233-0.13180.05980.036
H11A0.70720.30760.40170.033
H120.49630.48100.19690.036