+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 23:39:06 on 12-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh029 in Pbca CELL 0.71073 12.1766 9.5024 12.9638 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O F UNIT 64 64 8 8 8 V = 1500.00 F(000) = 640.0 Mu = 0.11 mm-1 Cell Wt = 1225.23 Rho = 1.356 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 SIZE 0.2 0.2 0.08 EQIV $1 -x+3/2, y-1/2, z HTAB N1 O1_$1 HTAB ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0366 0.8701 FVAR 0.18454 C1 1 0.564279 -0.047785 0.629382 11.00000 0.01988 0.02310 = 0.02096 -0.00123 -0.00226 -0.00018 C2 1 0.507831 0.079256 0.620720 11.00000 0.02260 0.02419 = 0.02650 -0.00058 -0.00145 0.00050 AFIX 43 H2 2 0.544141 0.162552 0.598831 11.00000 -1.20000 AFIX 0 C3 1 0.397941 0.080122 0.644870 11.00000 0.02528 0.03214 = 0.02712 -0.00319 -0.00261 0.00720 C4 1 0.340473 -0.036133 0.677321 11.00000 0.02095 0.04778 = 0.02745 0.00021 0.00091 -0.00218 AFIX 43 H4 2 0.264284 -0.030964 0.692634 11.00000 -1.20000 AFIX 0 C5 1 0.397873 -0.160857 0.686801 11.00000 0.02865 0.03945 = 0.03383 0.00789 0.00007 -0.00947 AFIX 43 H5 2 0.360839 -0.243117 0.709703 11.00000 -1.20000 AFIX 0 C6 1 0.508730 -0.167525 0.663344 11.00000 0.02830 0.02578 = 0.03137 0.00508 -0.00299 -0.00312 AFIX 43 H6 2 0.547105 -0.254033 0.670417 11.00000 -1.20000 AFIX 0 C7 1 0.749596 0.037263 0.580448 11.00000 0.02242 0.02088 = 0.02655 0.00140 -0.00061 -0.00004 C8 1 0.858583 -0.013394 0.540456 11.00000 0.02543 0.02675 = 0.04036 0.00100 0.00521 0.00012 AFIX 137 H8A 2 0.886560 0.053375 0.489184 11.00000 -1.50000 H8B 2 0.849418 -0.106038 0.508376 11.00000 -1.50000 H8C 2 0.910793 -0.020530 0.597748 11.00000 -1.50000 AFIX 0 N1 3 0.674806 -0.064629 0.599248 11.00000 0.02052 0.01647 = 0.02941 0.00020 -0.00013 0.00041 O1 4 0.731241 0.162888 0.595558 11.00000 0.02700 0.01844 = 0.05052 -0.00124 0.00579 -0.00201 F1 5 0.343237 0.204353 0.633993 11.00000 0.02968 0.03914 = 0.05364 -0.00229 0.00023 0.01436 H1N 2 0.696851 -0.152336 0.591478 11.00000 0.02904 HKLF 4 Covalent radii and connectivity table for 2008lsh029 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - C2 C6 N1 C2 - C3 C1 C3 - F1 C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 F1 - C3 Operators for generating equivalent atoms: $1 -x+3/2, y-1/2, z 10311 Reflections read, of which 798 rejected -15 =< h =< 15, -9 =< k =< 12, -16 =< l =< 15, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 1704 Unique reflections, of which 0 suppressed R(int) = 0.0316 R(sigma) = 0.0293 Friedel opposites merged Maximum memory for data reduction = 1230 / 17012 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 1 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18458 0.00050 0.083 OSF Mean shift/esd = 0.055 Maximum = -0.172 for y C3 Max. shift = 0.003 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 2 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18455 0.00050 -0.060 OSF Mean shift/esd = 0.019 Maximum = 0.068 for tors H8A Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 3 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18455 0.00050 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.026 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 4 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18455 0.00050 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.010 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 5 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18455 0.00050 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.1068 before cycle 6 for 1704 data and 105 / 105 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18455 0.00050 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5441 0.1626 0.5988 43 0.950 0.000 C2 C3 C1 H4 0.2643 -0.0309 0.6926 43 0.950 0.000 C4 C3 C5 H5 0.3609 -0.2431 0.7097 43 0.950 0.000 C5 C4 C6 H6 0.5471 -0.2540 0.6704 43 0.950 0.000 C6 C5 C1 H8A 0.8867 0.0535 0.4893 137 0.980 0.000 C8 C7 H8A H8B 0.8494 -0.1059 0.5082 137 0.980 0.000 C8 C7 H8A H8C 0.9107 -0.0208 0.5978 137 0.980 0.000 C8 C7 H8A 2008lsh029 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.56427 -0.04779 0.62939 1.00000 0.01979 0.02305 0.02089 -0.00120 -0.00226 -0.00020 0.02124 0.00227 0.00011 0.00014 0.00010 0.00000 0.00066 0.00064 0.00067 0.00050 0.00052 0.00053 0.00030 C2 0.50783 0.07927 0.62073 1.00000 0.02256 0.02405 0.02648 -0.00059 -0.00139 0.00046 0.02436 0.00239 0.00012 0.00015 0.00011 0.00000 0.00071 0.00070 0.00073 0.00053 0.00055 0.00054 0.00032 H2 0.54413 0.16257 0.59885 1.00000 0.02924 0.00000 0.00000 C3 0.39795 0.08008 0.64488 1.00000 0.02521 0.03208 0.02709 -0.00322 -0.00264 0.00725 0.02813 0.00262 0.00012 0.00016 0.00012 0.00000 0.00075 0.00077 0.00073 0.00057 0.00057 0.00060 0.00034 C4 0.34048 -0.03610 0.67731 1.00000 0.02089 0.04778 0.02734 0.00018 0.00088 -0.00216 0.03200 0.00267 0.00012 0.00017 0.00012 0.00000 0.00071 0.00094 0.00077 0.00066 0.00058 0.00063 0.00036 H4 0.26429 -0.03091 0.69262 1.00000 0.03840 0.00000 0.00000 C5 0.39788 -0.16084 0.68681 1.00000 0.02859 0.03943 0.03374 0.00791 0.00004 -0.00951 0.03392 0.00277 0.00013 0.00017 0.00012 0.00000 0.00081 0.00086 0.00084 0.00066 0.00066 0.00065 0.00037 H5 0.36085 -0.24310 0.70971 1.00000 0.04070 0.00000 0.00000 C6 0.50871 -0.16750 0.66335 1.00000 0.02824 0.02572 0.03127 0.00504 -0.00297 -0.00308 0.02841 0.00254 0.00012 0.00015 0.00012 0.00000 0.00078 0.00072 0.00079 0.00058 0.00061 0.00059 0.00034 H6 0.54708 -0.25401 0.67042 1.00000 0.03409 0.00000 0.00000 C7 0.74959 0.03725 0.58044 1.00000 0.02244 0.02093 0.02641 0.00139 -0.00062 -0.00004 0.02326 0.00236 0.00011 0.00014 0.00010 0.00000 0.00068 0.00064 0.00070 0.00053 0.00056 0.00053 0.00030 C8 0.85859 -0.01341 0.54045 1.00000 0.02538 0.02681 0.04027 0.00101 0.00521 0.00014 0.03082 0.00272 0.00012 0.00016 0.00013 0.00000 0.00076 0.00072 0.00087 0.00062 0.00064 0.00058 0.00036 H8A 0.88666 0.05348 0.48931 1.00000 0.04623 0.00000 0.00000 H8B 0.84939 -0.10595 0.50821 1.00000 0.04623 0.00000 0.00000 H8C 0.91074 -0.02078 0.59777 1.00000 0.04623 0.00000 0.00000 N1 0.67480 -0.06461 0.59924 1.00000 0.02047 0.01641 0.02941 0.00021 -0.00016 0.00042 0.02210 0.00196 0.00009 0.00012 0.00009 0.00000 0.00060 0.00053 0.00063 0.00045 0.00047 0.00043 0.00027 O1 0.73124 0.16289 0.59555 1.00000 0.02696 0.01837 0.05039 -0.00122 0.00581 -0.00199 0.03191 0.00183 0.00009 0.00010 0.00009 0.00000 0.00057 0.00049 0.00068 0.00044 0.00048 0.00040 0.00028 F1 0.34324 0.20436 0.63401 1.00000 0.02966 0.03912 0.05363 -0.00230 0.00027 0.01439 0.04081 0.00175 0.00007 0.00010 0.00008 0.00000 0.00052 0.00055 0.00062 0.00044 0.00042 0.00040 0.00029 H1N 0.69698 -0.15226 0.59125 1.00000 0.02946 0.02823 0.00143 0.00149 0.00123 0.00000 0.00430 Final Structure Factor Calculation for 2008lsh029 in Pbca Total number of l.s. parameters = 105 Maximum vector length = 511 Memory required = 1410 / 24017 wR2 = 0.1068 before cycle 7 for 1704 data and 0 / 105 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.080; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0366 * P )^2 + 0.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0437 for 1437 Fo > 4sig(Fo) and 0.0555 for all 1704 data wR2 = 0.1068, GooF = S = 1.080, Restrained GooF = 1.079 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0238 0.0221 0.0179 C1 0.0271 0.0239 0.0221 C2 0.0382 0.0256 0.0206 C3 0.0479 0.0275 0.0206 C4 0.0483 0.0320 0.0215 C5 0.0364 0.0264 0.0224 C6 0.0268 0.0224 0.0206 C7 0.0420 0.0268 0.0237 C8 0.0294 0.0205 0.0164 N1 0.0518 0.0260 0.0179 O1 0.0543 0.0489 0.0192 F1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.015 0.023 0.031 0.040 0.051 0.067 0.089 0.130 1.000 Number in group 182. 169. 187. 158. 171. 175. 160. 165. 167. 170. GooF 1.190 1.181 1.026 0.962 1.158 1.078 1.100 0.944 1.053 1.061 K 2.814 1.309 1.017 0.979 0.962 0.974 0.991 1.003 1.013 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.32 1.66 inf Number in group 174. 167. 170. 176. 166. 169. 172. 168. 173. 169. GooF 1.198 1.125 1.093 1.037 0.923 0.876 0.987 0.858 1.125 1.442 K 1.047 1.047 1.032 0.987 0.995 0.996 1.008 1.014 1.023 0.987 R1 0.176 0.123 0.111 0.082 0.057 0.044 0.035 0.029 0.036 0.032 Recommended weighting scheme: WGHT 0.0361 0.8557 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 3 3 369.06 271.20 4.51 0.094 2.16 3 6 6 10.03 0.67 3.88 0.005 1.22 7 0 2 142.17 93.41 3.81 0.055 1.68 6 1 0 71.53 108.84 3.56 0.060 1.98 0 0 12 24.37 0.07 3.46 0.002 1.08 4 5 0 171.05 126.80 3.27 0.064 1.61 1 4 1 690.49 577.12 3.21 0.138 2.29 1 5 4 386.82 313.92 3.15 0.101 1.62 5 0 14 55.49 3.62 3.13 0.011 0.87 13 2 5 3.22 15.57 3.10 0.023 0.87 3 1 1 4.52 0.01 3.07 0.000 3.59 3 4 4 32.88 18.07 3.04 0.024 1.73 8 9 7 13.21 34.16 3.02 0.033 0.79 6 2 0 50.38 75.71 2.93 0.050 1.87 6 9 6 20.40 38.41 2.90 0.035 0.86 11 1 3 56.38 83.03 2.90 0.052 1.07 11 2 11 13.41 32.17 2.86 0.032 0.80 2 2 0 126.73 164.29 2.73 0.073 3.75 1 2 2 3997.40 4500.82 2.69 0.384 3.66 2 4 0 780.46 670.54 2.67 0.148 2.21 12 7 1 14.09 37.69 2.65 0.035 0.81 12 7 0 18.79 40.20 2.61 0.036 0.81 2 1 15 -1.32 10.82 2.59 0.019 0.85 7 8 6 21.76 38.13 2.59 0.035 0.89 9 8 2 9.63 1.63 2.59 0.007 0.88 2 6 1 47.28 68.18 2.58 0.047 1.52 1 5 14 -1.65 2.96 2.57 0.010 0.83 2 1 0 1534.45 1743.68 2.55 0.239 5.13 6 3 0 178.75 143.07 2.54 0.069 1.71 1 4 15 86.52 49.49 2.52 0.040 0.81 0 2 1 27.75 43.81 2.50 0.038 4.46 4 3 1 304.64 255.82 2.49 0.092 2.16 14 4 3 12.16 2.06 2.49 0.008 0.80 1 2 1 -0.12 4.16 2.47 0.012 4.19 5 8 2 301.86 358.40 2.44 0.108 1.05 9 7 10 9.18 0.24 2.44 0.003 0.77 2 12 1 15.45 5.89 2.42 0.014 0.78 2 5 0 2318.37 2070.70 2.39 0.261 1.81 13 6 4 56.13 34.32 2.36 0.034 0.78 3 3 9 248.66 206.08 2.35 0.082 1.25 10 9 2 10.60 0.84 2.34 0.005 0.79 0 0 8 370.69 436.16 2.34 0.120 1.62 11 4 8 15.53 6.20 2.31 0.014 0.85 6 1 5 246.77 207.59 2.29 0.083 1.58 12 2 2 0.23 5.11 2.26 0.013 0.98 6 7 0 116.99 147.93 2.26 0.070 1.13 6 7 4 12.10 22.21 2.24 0.027 1.07 8 9 0 64.19 45.59 2.23 0.039 0.87 6 7 3 5.45 12.73 2.22 0.020 1.09 4 11 3 8.23 2.39 2.22 0.009 0.82 Bond lengths and angles C1 - Distance Angles C2 1.3938 (0.0019) C6 1.3948 (0.0019) 119.52 (0.13) N1 1.4106 (0.0018) 123.11 (0.12) 117.25 (0.12) C1 - C2 C6 C2 - Distance Angles C3 1.3741 (0.0021) C1 1.3938 (0.0019) 117.82 (0.13) H2 0.9500 121.09 121.09 C2 - C3 C1 C3 - Distance Angles F1 1.3632 (0.0017) C4 1.3730 (0.0022) 118.63 (0.13) C2 1.3741 (0.0021) 117.21 (0.14) 124.16 (0.14) C3 - F1 C4 C4 - Distance Angles C3 1.3730 (0.0022) C5 1.3816 (0.0022) 117.34 (0.14) H4 0.9500 121.33 121.33 C4 - C3 C5 C5 - Distance Angles C4 1.3816 (0.0022) C6 1.3847 (0.0022) 120.84 (0.14) H5 0.9500 119.58 119.58 C5 - C4 C6 C6 - Distance Angles C5 1.3847 (0.0022) C1 1.3948 (0.0019) 120.32 (0.14) H6 0.9500 119.84 119.84 C6 - C5 C1 C7 - Distance Angles O1 1.2303 (0.0016) N1 1.3512 (0.0017) 122.96 (0.13) C8 1.5040 (0.0020) 121.72 (0.13) 115.32 (0.12) C7 - O1 N1 C8 - Distance Angles C7 1.5040 (0.0020) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B N1 - Distance Angles C7 1.3512 (0.0017) C1 1.4106 (0.0018) 127.72 (0.12) H1N 0.8816 (0.0136) 116.69 (1.16) 115.58 (1.16) N1 - C7 C1 O1 - Distance Angles C7 1.2303 (0.0016) O1 - F1 - Distance Angles C3 1.3632 (0.0017) F1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.882(14) 1.963(14) 2.8313(15) 168.1(16) N1-H1N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)