Small Molecule Crystallography Lab Department of Chemistry and Biochemistry University of Oklahoma 101 Stephenson Parkway Norman, OK

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Small Molecule Crystallography Lab Department of Chemistry and Biochemistry University of Oklahoma 101 Stephenson Parkway Norman, OK 73019-5251 Sample: KP-XI-furan-enzymatic alcohol Lab ID: 12042 User: Kaushik Panigrahi Formula: C 12 H 17 F 2 O 5 P Date: May 14, 2012 For Prof. David Berkowitz

Table of Contents Figure 1. Thermal Ellipsoid Plot of Structure.. 3 Figure 2. Packing Diagram 4 Comments.. 5 Experimental.. 5 Acknowledgements... 6 References. 6 Table 1. Crystal Data 7 Table 2. Atom Coordinates 8 Table 3. Bond Distances and Angles.. 9 Table 4. Anisotropic Displacement Parameters.. 11 Table 5. Hydrogen Atom Parameters 12 Table 6. Torsion Angles.. 13 Table 7. Hydrogen Bond Details 14 KP-XI-furan-enzymatic-alcohol 12042 Page 2

KP-XI-furan-enzymatic-alcohol 12042 Page 3

KP-XI-furan-enzymatic-alcohol 12042 Page 4

Comment The displacement ellipsoids were drawn at the 50% probability level. Experimental A colorless block-shaped crystal of dimensions 0.42 x 0.38 x 0.32 mm was selected for structural analysis. Intensity data for this compound were collected using a diffractometer with a Bruker APEX ccd area detector (1) and graphite-monochromated Mo K radiation ( = 0.71073 Å). The sample was cooled to 100(2) K. Cell parameters were determined from a non-linear least squares fit of 5538 peaks in the range 2.29 < < 25.91. A total of 12715 data were measured in the range 2.22 < < 25.91 using and oscillation frames. The data were corrected for absorption by the empirical method (2) giving minimum and maximum transmission factors of 0.9088 and 0.9294. The data were merged to form a set of 2622 independent data with R(int) = 0.0201 and a coverage of 99.7 %. The orthorhombic space group P2 1 2 1 2 1 was determined by systematic absences and statistical tests and verified by subsequent refinement. The structure was solved by direct methods and refined by full-matrix least-squares methods on F 2 (3). The positions of hydrogens bonded to carbons were initially determined by geometry and refined by a riding model. The hydrogen bonded to O4 was located on a difference map, and its position was refined independently. Non-hydrogen atoms were refined with anisotropic displacement parameters. Hydrogen atom displacement parameters were set to 1.2 (1.5 for methyl) times the isotropic equivalent displacement parameters of the bonded atoms. A total of 185 parameters were refined against 0 restraints and 2622 data to give wr(f 2 ) = 0.0688 and S = 0.991 for weights of w = 1/[ 2 (F 2 ) + (0.0480 P) 2 + 0.3200 P], where P = [F o 2 + 2F c 2 ] / 3. The final R(F) was 0.0254 for the 2579 observed, [F > 4 (F)], data. The largest shift/s.u. was 0.001 in the final refinement cycle. The final difference map had maxima and minima of 0.294 and -0.191 e/å 3, respectively. The absolute structure was determined by refinement of the Flack parameter(4). KP-XI-furan-enzymatic-alcohol 12042 Page 5

Acknowledgment The authors thank the National Science Foundation (grant CHE-0130835) and the University of Oklahoma for funds to purchase of the X-ray instrument and computers. This structure was determined by Douglas R. Powell. References (1) (a) Data Collection: SMART Software Reference Manual (2007). Bruker-AXS, 5465 E. Cheryl Parkway, Madison, WI 53711-5373 USA. (b) Data Reduction: SAINT Software Reference Manual (2007). Bruker-AXS, 5465 E. Cheryl Parkway, Madison, WI 53711-5373 USA. (2) G. M. Sheldrick (2001). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Göttingen, Germany. (3) G. M. Sheldrick (2008). Acta Cryst., A64, 112-122. (4) H. D. Flack (1983). Acta Cryst. A39, 876-881. KP-XI-furan-enzymatic-alcohol 12042 Page 6

Table 1. Crystal data and structure refinement for 12042. Empirical formula Formula weight 310.23 Crystal system C 12 H 17 F 2 O 5 P orthorhombic Space group P2 1 2 1 2 1 Unit cell dimensions a = 5.4421(7) Å = 90 Volume 1420.1(3) Å 3 Z, Z' 4, 1 Density (calculated) 1.451 Mg/m 3 Wavelength Temperature F(000) 648 b = 9.7834(13) Å = 90 c = 26.672(3) Å = 90 0.71073 Å 100(2) K Absorption coefficient 0.232 mm -1 Absorption correction Semi-empirical from equivalents Max. and min. transmission 0.9294 and 0.9088 Theta range for data collection 2.22 to 25.91 Reflections collected 12715 Independent reflections 2622 [R(int) = 0.0201] Data / restraints / parameters 2622 / 0 / 185 wr(f 2 all data) wr2 = 0.0688 R(F obsd data) R1 = 0.0254 Goodness-of-fit on F 2 0.991 Observed data [I > 2 (I)] 2579 Absolute structure parameter 0.00(8) Largest and mean shift / s.u. 0.001and 0.000 Largest diff. peak and hole 0.294 and -0.191 e/å 3 ---------- wr2 = { [w(f 2 o - F 2 c ) 2 ] / [w(f 2 o ) 2 ] } 1/2 R1 = F o - F c / F o KP-XI-furan-enzymatic-alcohol 12042 Page 7

Table 2. Atomic coordinates and equivalent isotropic displacement parameters for 12042. U(eq) is defined as one third of the trace of the orthogonalized U ij tensor. x y z U(eq) P(1) 0.61562(7) 0.40378(4) 0.660039(14) 0.01812(11) F(1) 0.60725(19) 0.67101(10) 0.65145(4) 0.0288(2) F(2) 0.25725(18) 0.58157(10) 0.67530(3) 0.0264(2) O(1) 0.7982(2) 0.36842(12) 0.62170(4) 0.0240(3) O(2) 0.7143(2) 0.44171(12) 0.71334(4) 0.0256(3) O(3) 0.4147(2) 0.29363(11) 0.67078(4) 0.0218(3) O(4) 0.2331(2) 0.44403(12) 0.57883(4) 0.0208(2) O(5) 0.1349(2) 1.13620(11) 0.50999(4) 0.0247(3) C(1) 0.8265(4) 0.3327(2) 0.74346(7) 0.0374(5) C(2) 1.0223(4) 0.3933(2) 0.77580(7) 0.0341(4) C(3) 0.3640(3) 0.17947(16) 0.63701(6) 0.0239(3) C(4) 0.5027(3) 0.05591(18) 0.65492(7) 0.0277(4) C(5) 0.4511(3) 0.56357(16) 0.64348(6) 0.0195(3) C(6) 0.3629(3) 0.56616(15) 0.58885(5) 0.0186(3) C(7) 0.2237(3) 0.69485(17) 0.57829(6) 0.0205(3) C(8) 0.3139(3) 0.79341(16) 0.54899(6) 0.0181(3) C(9) 0.1963(3) 0.92421(16) 0.53883(6) 0.0183(3) C(10) 0.2899(3) 1.02743(17) 0.51092(6) 0.0220(3) C(11) -0.0640(3) 1.10018(18) 0.53828(6) 0.0240(4) C(12) -0.0380(3) 0.97324(17) 0.55654(6) 0.0212(3) KP-XI-furan-enzymatic-alcohol 12042 Page 8

Table 3. Bond lengths [Å] and angles [ ] for 12042. P(1)-O(1) 1.4672(12) P(1)-O(3) 1.5619(12) P(1)-O(2) 1.5644(12) P(1)-C(5) 1.8549(16) F(1)-C(5) 1.3683(19) F(2)-C(5) 1.3653(18) O(2)-C(1) 1.468(2) O(3)-C(3) 1.461(2) O(4)-C(6) 1.414(2) O(4)-H(4O) 0.88(2) O(5)-C(10) 1.358(2) O(5)-C(11) 1.366(2) C(1)-C(2) 1.494(3) C(1)-H(1A) 0.9900 C(1)-H(1B) 0.9900 C(2)-H(2A) 0.9800 C(2)-H(2B) 0.9800 C(2)-H(2C) 0.9800 C(3)-C(4) 1.503(2) O(1)-P(1)-O(3) 116.07(7) O(1)-P(1)-O(2) 117.17(7) O(3)-P(1)-O(2) 103.74(6) O(1)-P(1)-C(5) 111.08(7) O(3)-P(1)-C(5) 106.69(7) O(2)-P(1)-C(5) 100.50(7) C(1)-O(2)-P(1) 117.88(11) C(3)-O(3)-P(1) 123.13(11) C(6)-O(4)-H(4O) 112.8(13) C(10)-O(5)-C(11) 106.26(13) O(2)-C(1)-C(2) 108.92(16) O(2)-C(1)-H(1A) 109.9 C(2)-C(1)-H(1A) 109.9 O(2)-C(1)-H(1B) 109.9 C(2)-C(1)-H(1B) 109.9 H(1A)-C(1)-H(1B) 108.3 C(1)-C(2)-H(2A) 109.5 C(1)-C(2)-H(2B) 109.5 H(2A)-C(2)-H(2B) 109.5 C(1)-C(2)-H(2C) 109.5 H(2A)-C(2)-H(2C) 109.5 H(2B)-C(2)-H(2C) 109.5 C(3)-H(3A) 0.9900 C(3)-H(3B) 0.9900 C(4)-H(4A) 0.9800 C(4)-H(4B) 0.9800 C(4)-H(4C) 0.9800 C(5)-C(6) 1.534(2) C(6)-C(7) 1.496(2) C(6)-H(6) 1.0000 C(7)-C(8) 1.335(2) C(7)-H(7) 0.9500 C(8)-C(9) 1.456(2) C(8)-H(8) 0.9500 C(9)-C(10) 1.354(2) C(9)-C(12) 1.442(2) C(10)-H(10) 0.9500 C(11)-C(12) 1.341(2) C(11)-H(11) 0.9500 C(12)-H(12) 0.9500 O(3)-C(3)-C(4) 108.91(13) O(3)-C(3)-H(3A) 109.9 C(4)-C(3)-H(3A) 109.9 O(3)-C(3)-H(3B) 109.9 C(4)-C(3)-H(3B) 109.9 H(3A)-C(3)-H(3B) 108.3 C(3)-C(4)-H(4A) 109.5 C(3)-C(4)-H(4B) 109.5 H(4A)-C(4)-H(4B) 109.5 C(3)-C(4)-H(4C) 109.5 H(4A)-C(4)-H(4C) 109.5 H(4B)-C(4)-H(4C) 109.5 F(2)-C(5)-F(1) 106.51(12) F(2)-C(5)-C(6) 110.28(13) F(1)-C(5)-C(6) 109.21(13) F(2)-C(5)-P(1) 109.49(10) F(1)-C(5)-P(1) 108.10(10) C(6)-C(5)-P(1) 113.02(11) O(4)-C(6)-C(7) 115.00(13) O(4)-C(6)-C(5) 108.78(12) C(7)-C(6)-C(5) 110.56(12) O(4)-C(6)-H(6) 107.4 KP-XI-furan-enzymatic-alcohol 12042 Page 9

C(7)-C(6)-H(6) 107.4 C(12)-C(9)-C(8) 128.32(15) C(5)-C(6)-H(6) 107.4 C(9)-C(10)-O(5) 111.16(14) C(8)-C(7)-C(6) 122.15(15) C(9)-C(10)-H(10) 124.4 C(8)-C(7)-H(7) 118.9 O(5)-C(10)-H(10) 124.4 C(6)-C(7)-H(7) 118.9 C(12)-C(11)-O(5) 110.83(15) C(7)-C(8)-C(9) 125.61(15) C(12)-C(11)-H(11) 124.6 C(7)-C(8)-H(8) 117.2 O(5)-C(11)-H(11) 124.6 C(9)-C(8)-H(8) 117.2 C(11)-C(12)-C(9) 106.41(15) C(10)-C(9)-C(12) 105.34(15) C(11)-C(12)-H(12) 126.8 C(10)-C(9)-C(8) 126.33(15) C(9)-C(12)-H(12) 126.8 KP-XI-furan-enzymatic-alcohol 12042 Page 10

Table 4. Anisotropic displacement parameters (Å 2 x 10 3 ) for 12042. The anisotropic displacement factor exponent takes the form: -2 2 [ h 2 a* 2 U 11 +... + 2 h k a* b* U 12 ] U 11 U 22 U 33 U 23 U 13 U 12 P(1) 18(1) 18(1) 18(1) 0(1) -3(1) 1(1) F(1) 33(1) 18(1) 35(1) -1(1) -12(1) -5(1) F(2) 30(1) 29(1) 20(1) -2(1) 3(1) 7(1) O(1) 20(1) 25(1) 28(1) -1(1) -1(1) 0(1) O(2) 31(1) 23(1) 23(1) 0(1) -10(1) 1(1) O(3) 25(1) 20(1) 21(1) -1(1) 0(1) -1(1) O(4) 21(1) 21(1) 21(1) -1(1) 0(1) -3(1) O(5) 27(1) 20(1) 27(1) 5(1) -1(1) -3(1) C(1) 53(1) 26(1) 33(1) 6(1) -20(1) 5(1) C(2) 29(1) 46(1) 27(1) 3(1) -8(1) 5(1) C(3) 24(1) 21(1) 26(1) -3(1) -5(1) -4(1) C(4) 33(1) 23(1) 28(1) -2(1) -3(1) 1(1) C(5) 18(1) 17(1) 23(1) -2(1) -1(1) 1(1) C(6) 19(1) 18(1) 19(1) 1(1) 0(1) -1(1) C(7) 19(1) 23(1) 19(1) 0(1) 0(1) 2(1) C(8) 16(1) 21(1) 17(1) -3(1) 0(1) -1(1) C(9) 19(1) 19(1) 17(1) -1(1) -2(1) -2(1) C(10) 22(1) 23(1) 21(1) -2(1) -2(1) -2(1) C(11) 21(1) 23(1) 28(1) 0(1) -3(1) 2(1) C(12) 19(1) 21(1) 23(1) 1(1) 1(1) -2(1) KP-XI-furan-enzymatic-alcohol 12042 Page 11

Table 5. Hydrogen coordinates and isotropic displacement parameters for 12042. x y z U(eq) H(4O) 0.096(4) 0.438(2) 0.5959(7) 0.025 H(1A) 0.8984 0.2624 0.7212 0.045 H(1B) 0.7000 0.2885 0.7646 0.045 H(2A) 1.1489 0.4350 0.7546 0.051 H(2B) 1.0965 0.3214 0.7964 0.051 H(2C) 0.9501 0.4632 0.7976 0.051 H(3A) 0.4158 0.2031 0.6025 0.029 H(3B) 0.1855 0.1598 0.6366 0.029 H(4A) 0.6796 0.0719 0.6513 0.042 H(4B) 0.4550-0.0238 0.6349 0.042 H(4C) 0.4640 0.0390 0.6903 0.042 H(6) 0.5123 0.5665 0.5670 0.022 H(7) 0.0660 0.7068 0.5929 0.025 H(8) 0.4681 0.7768 0.5334 0.022 H(10) 0.4438 1.0242 0.4942 0.026 H(11) -0.2022 1.1573 0.5442 0.029 H(12) -0.1514 0.9252 0.5771 0.025 KP-XI-furan-enzymatic-alcohol 12042 Page 12

Table 6. Torsion angles [ ] for 12042. O(1)-P(1)-O(2)-C(1) -68.75(16) O(3)-P(1)-O(2)-C(1) 60.59(15) C(5)-P(1)-O(2)-C(1) 170.83(14) O(1)-P(1)-O(3)-C(3) -16.26(14) O(2)-P(1)-O(3)-C(3) -146.27(12) C(5)-P(1)-O(3)-C(3) 108.12(13) P(1)-O(2)-C(1)-C(2) 148.42(14) P(1)-O(3)-C(3)-C(4) 96.10(15) O(1)-P(1)-C(5)-F(2) 170.25(10) O(3)-P(1)-C(5)-F(2) 42.87(11) O(2)-P(1)-C(5)-F(2) -65.05(11) O(1)-P(1)-C(5)-F(1) -74.10(12) O(3)-P(1)-C(5)-F(1) 158.52(10) O(2)-P(1)-C(5)-F(1) 50.60(12) O(1)-P(1)-C(5)-C(6) 46.90(13) O(3)-P(1)-C(5)-C(6) -80.49(12) O(2)-P(1)-C(5)-C(6) 171.59(11) F(2)-C(5)-C(6)-O(4) -72.23(15) F(1)-C(5)-C(6)-O(4) 171.05(12) P(1)-C(5)-C(6)-O(4) 50.69(15) F(2)-C(5)-C(6)-C(7) 54.95(17) F(1)-C(5)-C(6)-C(7) -61.76(16) P(1)-C(5)-C(6)-C(7) 177.88(11) O(4)-C(6)-C(7)-C(8) -126.73(16) C(5)-C(6)-C(7)-C(8) 109.61(17) C(6)-C(7)-C(8)-C(9) -176.76(14) C(7)-C(8)-C(9)-C(10) 177.06(17) C(7)-C(8)-C(9)-C(12) -1.6(3) C(12)-C(9)-C(10)-O(5) 0.31(18) C(8)-C(9)-C(10)-O(5) -178.59(14) C(11)-O(5)-C(10)-C(9) -0.13(18) C(10)-O(5)-C(11)-C(12) -0.13(18) O(5)-C(11)-C(12)-C(9) 0.31(18) C(10)-C(9)-C(12)-C(11) -0.37(17) C(8)-C(9)-C(12)-C(11) 178.50(15) KP-XI-furan-enzymatic-alcohol 12042 Page 13

Table 7. Hydrogen bonds for 12042[Å and ]. D-H...A d(d-h) d(h...a) d(d...a) <(DHA) O(4)-H(4O)...O(1)#1 0.88(2) 1.88(2) 2.7305(17) 161.2(19) Symmetry transformations used to generate equivalent atoms: #1 x-1, y, z KP-XI-furan-enzymatic-alcohol 12042 Page 14

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