suc_fast

Crystal Structure Report for suc_fast


A specimen of C12H19O11, approximate dimensions 0.05 mm x 0.05 mm x 0.05 mm, was used for the X-ray crystallographic analysis. The X-ray intensity data were measured on a Bruker GADDS system equipped with a Graphite monochromator and a Cu Sealed Tube (λ = 1.54178 Å).

The total exposure time was 1.16 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 5605 reflections to a maximum θ angle of 62.81° (0.87 Å resolution), of which 1997 were independent (average redundancy 2.807, completeness = 95.1%, Rint = 6.73%, Rsig = 11.79%) and 1731 (86.68%) were greater than 2σ(F2). The final cell constants of a = 7.7206(18) Å, b = 8.668(2) Å, c = 10.807(3) Å, β = 102.992(11)°, volume = 704.7(3) Å3, are based upon the refinement of the XYZ-centroids of 1181 reflections above 20 σ(I) with 8.396° < 2θ < 117.4°. Data were corrected for absorption effects using the multi-scan method (SADABS). The ratio of minimum to maximum apparent transmission was 0.850. The calculated minimum and maximum transmission coefficients (based on crystal size) are 0.9397 and 0.9397.

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, C12H19O11. The final anisotropic full-matrix least-squares refinement on F2 with 216 variables converged at R1 = 5.36%, for the observed data and wR2 = 16.56% for all data. The goodness-of-fit was 1.001. The largest peak in the final difference electron density synthesis was 0.336 e-3 and the largest hole was -0.370 e-3 with an RMS deviation of 0.081 e-3. On the basis of the final model, the calculated density was 1.599 g/cm3 and F(000), 358 e-.





Table 1. Sample and crystal data for suc_fast.
Identification codesuc_fast
Chemical formulaC12H19O11
Formula weight339.27
Temperature110(2) K
Wavelength1.54178 Å
Crystal size0.05 x 0.05 x 0.05 mm
Crystal systemmonoclinic
Space groupP 1 21 1
Unit cell dimensionsa = 7.7206(18) Åα = 90°
b = 8.668(2) Åβ = 102.992(11)°
c = 10.807(3) Åγ = 90°
Volume704.7(3) Å3
Z2
Density (calculated)1.599 Mg/cm3
Absorption coefficient1.259 mm-1
F(000)358


Table 2. Data collection and structure refinement for suc_fast.
DiffractometerBruker GADDS
Radiation sourceSealed Tube, Cu
Theta range for data collection4.20 to 62.81°
Index ranges-8<=h<=8, -9<=k<=9, -10<=l<=12
Reflections collected5605
Independent reflections1997 [R(int) = 0.0673]
Coverage of independent reflections95.1%
Absorption correctionmulti-scan
Max. and min. transmission0.9397 and 0.9397
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 / parameters1997 / 1 / 216
Goodness-of-fit on F21.001
Final R indices1731 data; I>2σ(I)R1 = 0.0536, wR2 = 0.1484
all dataR1 = 0.0634, wR2 = 0.1656
Weighting schemew=1/[σ2(Fo2)+(0.1000P)2+0.0000P]
where P=(Fo2+2Fc2)/3
Largest diff. peak and hole0.336 and -0.370 eÅ-3
R.M.S. deviation from mean0.081 eÅ-3


Table 3. Atomic coordinates and equivalent isotropic atomic displacement parameters (Å2) for suc_fast.
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
x/ay/bz/cU(eq)
O10.9593(4)0.1250(4)0.6725(3)0.0233(8)
O20.6818(4)0.2710(4)0.7879(3)0.0188(8)
O30.6086(4)0.0171(4)0.8298(3)0.0176(8)
O40.6444(5)0.5487(4)0.6498(4)0.0267(9)
O50.6315(4)0.9665(4)0.6216(3)0.0206(8)
O60.7128(5)0.8188(4)0.4155(3)0.0249(9)
O70.2934(5)0.6156(4)0.6917(4)0.0258(9)
O80.2498(5)0.9303(4)0.7710(3)0.0229(8)
O90.3771(4)0.1255(4)0.9720(3)0.0217(8)
O100.7982(4)0.0467(4)0.0755(3)0.0219(8)
O110.0900(4)0.2712(4)0.0219(3)0.0227(8)
C10.9516(7)0.2844(6)0.7077(5)0.0221(11)
C20.8696(6)0.3053(6)0.8225(4)0.0182(11)
C30.6291(7)0.1724(5)0.8772(4)0.0180(11)
C40.5126(7)0.0065(6)0.6990(4)0.0184(11)
C50.3628(7)0.8887(6)0.6876(5)0.0204(11)
C60.4339(7)0.7269(6)0.7145(5)0.0200(11)
C70.5573(7)0.6930(7)0.6250(5)0.0229(11)
C80.7040(7)0.8127(6)0.6407(5)0.0195(11)
C90.8164(6)0.7938(7)0.5407(5)0.0240(12)
C100.4548(7)0.2313(6)0.8984(5)0.0185(11)
C110.7860(7)0.1757(6)0.9947(4)0.0178(11)
C120.9450(6)0.1995(6)0.9344(4)0.0186(11)


Table 4. Bond lengths (Å) for suc_fast.
O1-C11.439(6)O1-H10.84
O2-C31.416(6)O2-C21.444(6)
O3-C31.436(6)O3-C41.444(6)
O4-C71.417(7)O4-H4A0.84
O5-C41.417(6)O5-C81.443(6)
O6-C91.426(6)O6-H60.84
O7-C61.431(6)O7-H7A0.84
O8-C51.434(6)O8-H80.84
O9-C101.432(6)O9-H90.84
O10-C111.408(6)O10-H100.84
O11-C121.435(6)O11-H11A0.84
C1-C21.525(6)C1-H1A0.99
C1-H1B0.99C2-C121.525(7)
C2-H21.0C3-C101.504(7)
C3-C111.546(7)C4-C51.527(7)
C4-H41.0C5-C61.510(7)
C5-H51.0C6-C71.530(7)
C6-H6A1.0C7-C81.517(7)
C7-H71.0C8-C91.539(6)
C8-H8A1.0C9-H9A0.99
C9-H9B0.99C10-H10A0.99
C10-H10B0.99C11-C121.528(7)
C11-H111.0C12-H121.0


Table 5. Bond angles (°) for suc_fast.
C1-O1-H1109.5C3-O2-C2111.9(3)
C3-O3-C4113.6(4)C7-O4-H4A109.5
C4-O5-C8115.0(4)C9-O6-H6109.5
C6-O7-H7A109.5C5-O8-H8109.5
C10-O9-H9109.5C11-O10-H10109.5
C12-O11-H11A109.5O1-C1-C2112.3(4)
O1-C1-H1A109.2C2-C1-H1A109.2
O1-C1-H1B109.2C2-C1-H1B109.2
H1A-C1-H1B107.9O2-C2-C12105.3(4)
O2-C2-C1109.9(4)C12-C2-C1114.8(4)
O2-C2-H2108.9C12-C2-H2108.9
C1-C2-H2108.9O2-C3-O3110.4(3)
O2-C3-C10107.6(4)O3-C3-C10110.0(4)
O2-C3-C11104.9(4)O3-C3-C11108.3(4)
C10-C3-C11115.6(4)O5-C4-O3109.6(4)
O5-C4-C5111.6(4)O3-C4-C5109.5(4)
O5-C4-H4108.7O3-C4-H4108.7
C5-C4-H4108.7O8-C5-C6111.0(4)
O8-C5-C4109.7(4)C6-C5-C4111.7(4)
O8-C5-H5108.1C6-C5-H5108.1
C4-C5-H5108.1O7-C6-C5111.4(4)
O7-C6-C7108.5(4)C5-C6-C7107.9(4)
O7-C6-H6A109.7C5-C6-H6A109.7
C7-C6-H6A109.7O4-C7-C8105.8(4)
O4-C7-C6112.7(4)C8-C7-C6110.7(4)
O4-C7-H7109.2C8-C7-H7109.2
C6-C7-H7109.2O5-C8-C7111.1(4)
O5-C8-C9105.1(4)C7-C8-C9111.9(4)
O5-C8-H8A109.6C7-C8-H8A109.6
C9-C8-H8A109.6O6-C9-C8111.5(4)
O6-C9-H9A109.3C8-C9-H9A109.3
O6-C9-H9B109.3C8-C9-H9B109.3
H9A-C9-H9B108.0O9-C10-C3111.6(4)
O9-C10-H10A109.3C3-C10-H10A109.3
O9-C10-H10B109.3C3-C10-H10B109.3
H10A-C10-H10B108.0O10-C11-C12115.1(4)
O10-C11-C3115.2(4)C12-C11-C3102.0(4)
O10-C11-H11108.1C12-C11-H11108.1
C3-C11-H11108.1O11-C12-C2111.4(4)
O11-C12-C11111.1(4)C2-C12-C11102.7(4)
O11-C12-H12110.5C2-C12-H12110.5
C11-C12-H12110.5


Table 6. Torsion angles (°) for suc_fast.
C3-O2-C2-C128.5(5)C3-O2-C2-C1132.7(4)
O1-C1-C2-O2-70.1(5)O1-C1-C2-C1248.4(6)
C2-O2-C3-O3-101.9(4)C2-O2-C3-C10138.1(4)
C2-O2-C3-C1114.6(5)C4-O3-C3-O2-45.2(5)
C4-O3-C3-C1073.4(4)C4-O3-C3-C11-159.5(3)
C8-O5-C4-O368.0(5)C8-O5-C4-C5-53.6(5)
C3-O3-C4-O5108.3(4)C3-O3-C4-C5-128.9(4)
O5-C4-C5-O8177.8(4)O3-C4-C5-O856.2(5)
O5-C4-C5-C654.2(5)O3-C4-C5-C6-67.4(5)
O8-C5-C6-O762.8(5)C4-C5-C6-O7-174.4(4)
O8-C5-C6-C7-178.3(4)C4-C5-C6-C7-55.4(5)
O7-C6-C7-O4-64.6(6)C5-C6-C7-O4174.7(4)
O7-C6-C7-C8177.2(4)C5-C6-C7-C856.4(5)
C4-O5-C8-C754.9(5)C4-O5-C8-C9176.1(4)
O4-C7-C8-O5-178.2(4)C6-C7-C8-O5-55.8(5)
O4-C7-C8-C964.7(5)C6-C7-C8-C9-172.9(4)
O5-C8-C9-O6-57.1(5)C7-C8-C9-O663.6(6)
O2-C3-C10-O9170.9(4)O3-C3-C10-O950.6(5)
C11-C3-C10-O9-72.3(5)O2-C3-C11-O10-156.7(4)
O3-C3-C11-O10-38.8(5)C10-C3-C11-O1085.0(5)
O2-C3-C11-C12-31.3(5)O3-C3-C11-C1286.5(4)
C10-C3-C11-C12-149.6(4)O2-C2-C12-O11-146.9(4)
C1-C2-C12-O1192.0(5)O2-C2-C12-C11-28.0(5)
C1-C2-C12-C11-149.0(4)O10-C11-C12-O11-79.8(5)
C3-C11-C12-O11154.8(4)O10-C11-C12-C2161.1(4)
C3-C11-C12-C235.7(5)


Table 7. Anisotropic atomic displacement parameters (Å2) for suc_fast.
The anisotropic atomic displacement factor exponent takes the form: -2π2[ h2 a*2 U11 + ... + 2 h k a* b* U12 ]
U11U22U33U23U13U12
O10.017(2)0.0210(19)0.033(2)-0.0051(16)0.0081(15)-0.0017(15)
O20.0186(19)0.0162(19)0.0216(18)0.0056(13)0.0046(14)-0.0006(14)
O30.0178(19)0.013(2)0.0214(19)-0.0019(13)0.0035(14)-0.0012(13)
O40.026(2)0.0129(19)0.042(2)0.0005(17)0.0101(17)0.0029(15)
O50.019(2)0.017(2)0.027(2)0.0006(14)0.0074(16)0.0046(14)
O60.030(2)0.022(2)0.0245(19)-0.0027(14)0.0104(16)-0.0032(16)
O70.027(2)0.0151(19)0.039(2)-0.0079(16)0.0137(16)-0.0093(15)
O80.021(2)0.025(2)0.024(2)0.0007(15)0.0086(15)0.0005(15)
O90.020(2)0.0196(19)0.027(2)-0.0005(16)0.0093(15)-0.0009(15)
O100.024(2)0.0178(19)0.024(2)0.0025(15)0.0065(15)-0.0018(15)
O110.018(2)0.023(2)0.026(2)-0.0020(15)0.0021(15)-0.0001(16)
C10.019(3)0.019(3)0.028(3)0.004(2)0.005(2)0.002(2)
C20.016(3)0.016(3)0.024(3)-0.002(2)0.007(2)-0.0018(19)
C30.024(3)0.009(3)0.021(3)-0.002(2)0.005(2)-0.002(2)
C40.020(3)0.025(3)0.009(3)-0.0049(19)0.0005(19)0.0036(19)
C50.015(3)0.023(3)0.023(3)-0.011(2)0.004(2)-0.002(2)
C60.020(3)0.013(3)0.029(3)-0.002(2)0.008(2)-0.0024(19)
C70.021(3)0.022(3)0.029(3)0.003(2)0.012(2)-0.001(2)
C80.020(3)0.013(3)0.025(3)0.002(2)0.007(2)0.005(2)
C90.018(3)0.031(3)0.023(3)-0.003(2)0.005(2)0.001(2)
C100.014(3)0.017(3)0.026(3)-0.001(2)0.007(2)-0.0021(19)
C110.029(3)0.015(3)0.010(3)-0.0018(18)0.005(2)-0.004(2)
C120.011(3)0.023(3)0.021(3)-0.001(2)0.0020(19)-0.003(2)


Table 8. Hydrogen atomic coordinates and isotropic atomic displacement parameters (Å2) for suc_fast.
x/ay/bz/cU(eq)
H10.85640.09350.63940.035
H4A0.5704-0.52270.62740.04
H60.7125-0.08670.39810.037
H7A0.3277-0.46470.66080.039
H80.1615-0.02070.73000.034
H90.35220.04260.93160.033
H100.8100-0.03361.03470.033
H11A1.18360.22081.02440.034
H1A0.88050.34260.63500.026
H1B1.07330.32780.72740.026
H20.88570.41490.85160.022
H40.45930.10950.67150.022
H50.2902-0.10830.59850.024
H6A0.5022-0.28060.80460.024
H70.4867-0.30530.53530.027
H8A0.7824-0.19560.72770.023
H9A0.9162-0.13180.55850.029
H9B0.8672-0.31150.54660.029
H10A0.47410.33180.94280.022
H10B0.37180.24780.81520.022
H110.77330.26991.04540.021
H120.98340.09900.90370.022