lobo001

Crystal Structure Report for lobo001


A specimen of C12H10O6, approximate dimensions 0.162 mm x 0.203 mm x 0.381 mm, was used for the X-ray crystallographic analysis. The X-ray intensity data were measured.

The total exposure time was 17.33 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 15261 reflections to a maximum θ angle of 35.08° (0.62 Å resolution), of which 2396 were independent (average redundancy 6.369, completeness = 99.7%, Rint = 2.08%, Rsig = 1.35%) and 2143 (89.44%) were greater than 2σ(F2). The final cell constants of a = 3.7404(3) Å, b = 9.8818(9) Å, c = 14.8004(12) Å, β = 92.532(2)°, volume = 546.52(8) Å3, are based upon the refinement of the XYZ-centroids of 7616 reflections above 20 σ(I) with 4.958° < 2θ < 70.00°. Data were corrected for absorption effects using the Multi-Scan method (SADABS). The ratio of minimum to maximum apparent transmission was 0.946. The calculated minimum and maximum transmission coefficients (based on crystal size) are 0.9540 and 0.9800.

The structure was solved and refined using the Bruker SHELXTL Software Package, using the space group P 1 21/n 1, with Z = 2 for the formula unit, C12H10O6. The final anisotropic full-matrix least-squares refinement on F2 with 102 variables converged at R1 = 3.98%, for the observed data and wR2 = 11.86% for all data. The goodness-of-fit was 1.021. The largest peak in the final difference electron density synthesis was 0.617 e-/Å3 and the largest hole was -0.225 e-/Å3 with an RMS deviation of 0.070 e-/Å3. On the basis of the final model, the calculated density was 1.520 g/cm3 and F(000), 260 e-.





Table 1. Sample and crystal data for lobo001.
Identification codelobo001
Chemical formulaC12H10O6
Formula weight250.20 g/mol
Temperature106(2) K
Wavelength0.71073 Å
Crystal size0.162 x 0.203 x 0.381 mm
Crystal systemmonoclinic
Space groupP 1 21/n 1
Unit cell dimensionsa = 3.7404(3) Åα = 90°
b = 9.8818(9) Åβ = 92.532(2)°
c = 14.8004(12) Åγ = 90°
Volume546.52(8) Å3
Z2
Density (calculated)1.520 g/cm3
Absorption coefficient0.124 mm-1
F(000)260


Table 2. Data collection and structure refinement for lobo001.
Theta range for data collection2.48 to 35.08°
Index ranges-6<=h<=6, -15<=k<=15, -23<=l<=23
Reflections collected15261
Independent reflections2396 [R(int) = 0.0208]
Coverage of independent reflections99.7%
Absorption correctionMulti-Scan
Max. and min. transmission0.9800 and 0.9540
Structure solution techniquedirect methods
Structure solution programSHELXT 2014/5 (Sheldrick, 2014)
Refinement methodFull-matrix least-squares on F2
Refinement programSHELXL-2018/3 (Sheldrick, 2018)
Function minimizedΣ w(Fo2 - Fc2)2
Data / restraints / parameters2396 / 0 / 102
Goodness-of-fit on F21.021
Δ/σmax0.001
Final R indices2143 data; I>2σ(I)R1 = 0.0398, wR2 = 0.1150
all dataR1 = 0.0429, wR2 = 0.1186
Weighting schemew=1/[σ2(Fo2)+(0.0860P)2+0.0621P]
where P=(Fo2+2Fc2)/3
Largest diff. peak and hole0.617 and -0.225 eÅ-3
R.M.S. deviation from mean0.070 eÅ-3


Table 3. Atomic coordinates and equivalent isotropic atomic displacement parameters (Å2) for lobo001.
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
x/ay/bz/cU(eq)
O10.32054(13)0.52363(5)0.63410(3)0.01733(12)
O20.63360(14)0.67704(5)0.71910(3)0.01981(12)
O30.52917(13)0.86580(5)0.58247(3)0.01488(11)
C10.3636(2)0.42910(7)0.70863(5)0.02161(15)
C20.46851(17)0.64560(6)0.64977(4)0.01416(13)
C30.40697(16)0.73535(6)0.57197(4)0.01414(12)
C40.25278(17)0.71704(6)0.48728(4)0.01587(13)
C50.27999(18)0.84349(6)0.44166(4)0.01646(13)
C60.44860(16)0.92985(6)0.50232(4)0.01435(12)


Table 4. Bond lengths (Å) for lobo001.
O1-C21.3421(8)O1-C11.4490(8)
O2-C21.2144(8)O3-C61.3663(7)
O3-C31.3742(8)C1-H10.969(13)
C1-H20.939(14)C1-H30.930(13)
C2-C31.4635(9)C3-C41.3684(8)
C4-C51.4260(9)C4-H40.921(12)
C5-C61.3719(9)C5-H50.983(13)
C6-C61.4412(12)


Table 5. Bond angles (°) for lobo001.
C2-O1-C1114.60(5)C6-O3-C3106.08(5)
O1-C1-H1109.3(8)O1-C1-H2104.7(9)
H1-C1-H2109.6(12)O1-C1-H3109.0(8)
H1-C1-H3115.2(11)H2-C1-H3108.5(11)
O2-C2-O1124.48(6)O2-C2-C3124.48(6)
O1-C2-C3111.04(5)C4-C3-O3110.62(5)
C4-C3-C2133.30(6)O3-C3-C2116.08(5)
C3-C4-C5106.37(5)C3-C4-H4125.2(8)
C5-C4-H4128.4(8)C6-C5-C4106.00(5)
C6-C5-H5126.3(8)C4-C5-H5127.7(8)
O3-C6-C5110.94(5)O3-C6-C6115.98(7)
C5-C6-C6133.09(7)


Table 6. Torsion angles (°) for lobo001.
C1-O1-C2-O21.51(9)C1-O1-C2-C3-178.92(5)
C6-O3-C3-C40.01(7)C6-O3-C3-C2179.19(5)
O2-C2-C3-C4174.86(7)O1-C2-C3-C4-4.70(10)
O2-C2-C3-O3-4.08(9)O1-C2-C3-O3176.36(5)
O3-C3-C4-C50.09(7)C2-C3-C4-C5-178.89(7)
C3-C4-C5-C6-0.16(7)C3-O3-C6-C5-0.12(7)
C3-O3-C6-C6179.65(6)C4-C5-C6-O30.17(7)
C4-C5-C6-C6-179.54(9)


Table 7. Anisotropic atomic displacement parameters (Å2) for lobo001.
The anisotropic atomic displacement factor exponent takes the form: -2π2[ h2 a*2 U11 + ... + 2 h k a* b* U12 ]
U11U22U33U23U13U12
O10.0227(2)0.0130(2)0.0161(2)0.00132(14)-0.00120(16)-0.00152(16)
O20.0266(3)0.0182(2)0.0141(2)0.00021(15)-0.00475(17)-0.00099(17)
O30.0205(2)0.0125(2)0.01139(19)0.00042(13)-0.00162(15)-0.00021(14)
C10.0255(3)0.0177(3)0.0215(3)0.0071(2)-0.0007(2)-0.0019(2)
C20.0168(3)0.0128(2)0.0129(2)0.00027(17)0.00048(19)0.00120(17)
C30.0177(3)0.0124(2)0.0122(2)0.00000(17)-0.00049(18)0.00002(18)
C40.0194(3)0.0146(2)0.0134(2)-0.00063(18)-0.00133(19)-0.00053(19)
C50.0209(3)0.0161(3)0.0121(2)-0.00004(18)-0.00235(19)0.00012(19)
C60.0181(3)0.0138(2)0.0109(2)0.00096(17)-0.00083(18)0.00083(18)


Table 8. Hydrogen atomic coordinates and isotropic atomic displacement parameters (Å2) for lobo001.
x/ay/bz/cU(eq)
H10.234(3)0.4622(14)0.7594(9)0.027(3)
H20.258(4)0.3486(14)0.6868(10)0.036(3)
H30.606(4)0.4134(14)0.7205(9)0.030(3)
H40.152(3)0.6376(13)0.4659(8)0.023(3)
H50.201(3)0.8651(13)0.3791(8)0.026(3)