+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:47:51 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh093 in P2(1)/c CELL 0.71073 13.3567 7.6145 11.0805 90.000 110.890 90.000 ZERR 4.00 0.0004 0.0003 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 40 48 4 8 12 V = 1052.86 F(000) = 488.0 Mu = 0.14 mm-1 Cell Wt = 940.82 Rho = 1.484 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 SIZE 0.12 0.12 0.04 ACTA EQIV $1 x, -y+1/2, z+1/2 EQIV $2 -x, y-1/2, -z+1/2 HTAB N1 O2_$1 HTAB N1 O2_$2 HTAB N1 O1 HTAB N1 F3 HTAB BOND $H L.S. 6 TEMP -153.00 WGHT 0.0206 0.6302 EXTI 0.027150 FVAR 0.69724 C2 1 0.434843 0.133449 0.585619 11.00000 0.02158 0.02218 = 0.02560 0.00009 0.01184 0.00013 AFIX 43 H2 2 0.477503 0.161316 0.535576 11.00000 -1.20000 AFIX 0 C3 1 0.323899 0.142008 0.528477 11.00000 0.02180 0.02217 = 0.01914 0.00083 0.00726 0.00067 AFIX 43 H3 2 0.290948 0.174236 0.440265 11.00000 -1.20000 AFIX 0 C5 1 0.308527 0.056218 0.730807 11.00000 0.01986 0.02328 = 0.02173 0.00067 0.00880 -0.00128 AFIX 43 H5 2 0.265380 0.030623 0.780672 11.00000 -1.20000 AFIX 0 C4 1 0.262193 0.102774 0.602276 11.00000 0.01610 0.01967 = 0.02131 -0.00139 0.00437 0.00069 C1 1 0.485120 0.084944 0.714661 11.00000 0.01748 0.01959 = 0.02461 -0.00136 0.00645 0.00061 C7 1 0.606212 0.069422 0.772937 11.00000 0.01699 0.02766 = 0.02874 0.00121 0.00805 0.00262 AFIX 23 H7A 2 0.637612 0.140883 0.720701 11.00000 -1.20000 H7B 2 0.626226 -0.054501 0.766622 11.00000 -1.20000 AFIX 0 C6 1 0.419980 0.047589 0.785809 11.00000 0.02019 0.02654 = 0.01963 0.00266 0.00560 0.00093 AFIX 43 H6 2 0.452453 0.015414 0.874093 11.00000 -1.20000 AFIX 0 C8 1 0.655864 0.127343 0.913561 11.00000 0.01887 0.03079 = 0.03158 0.00090 0.00704 -0.00060 AFIX 137 H8A 2 0.635350 0.249112 0.921665 11.00000 -1.50000 H8B 2 0.734086 0.118969 0.941821 11.00000 -1.50000 H8C 2 0.630064 0.051171 0.967573 11.00000 -1.50000 AFIX 0 N1 3 0.145219 0.112843 0.541573 11.00000 0.01591 0.02831 = 0.01964 0.00001 0.00508 -0.00091 O1 4 0.104115 0.380285 0.369126 11.00000 0.01890 0.03583 = 0.02390 0.00538 0.00352 0.00040 F2 5 -0.127184 0.548741 0.315554 11.00000 0.03532 0.03208 = 0.04604 0.00341 0.02221 0.01078 O2 4 0.001773 0.443837 0.164951 11.00000 0.02240 0.04797 = 0.02184 0.00685 0.00841 0.00684 C11 1 -0.085970 0.389534 0.311354 11.00000 0.02041 0.02730 = 0.02435 0.00171 0.00735 0.00318 F1 5 -0.161684 0.298722 0.221008 11.00000 0.02411 0.05150 = 0.04619 -0.01190 0.01078 -0.01113 C10 1 0.017902 0.404457 0.280129 11.00000 0.02209 0.02226 = 0.02180 0.00016 0.00817 0.00126 F3 5 -0.070526 0.311923 0.424359 11.00000 0.03395 0.05090 = 0.03741 0.01787 0.02201 0.01078 H1N 2 0.110112 0.098710 0.600352 11.00000 0.02830 H2N 2 0.113913 0.028533 0.474296 11.00000 0.03804 H3N 2 0.126563 0.221823 0.496251 11.00000 0.03828 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008lsh093 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C2 - C3 C1 C3 - C4 C2 C5 - C4 C6 C4 - C5 C3 N1 C1 - C2 C6 C7 C7 - C1 C8 C6 - C5 C1 C8 - C7 N1 - C4 O1 - C10 F2 - C11 O2 - C10 C11 - F3 F1 F2 C10 F1 - C11 C10 - O1 O2 C11 F3 - C11 Operators for generating equivalent atoms: $1 x, -y+1/2, z+1/2 $2 -x, y-1/2, -z+1/2 14547 Reflections read, of which 719 rejected -17 =< h =< 17, -9 =< k =< 9, -14 =< l =< 14, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 2 8 5.34 0.79 9 5.39 1 Inconsistent equivalents 2407 Unique reflections, of which 0 suppressed R(int) = 0.0646 R(sigma) = 0.0624 Friedel opposites merged Maximum memory for data reduction = 1677 / 24097 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 = 2100 / 199553 wR2 = 0.1101 before cycle 1 for 2407 data and 159 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69677 0.00198 -0.237 OSF 2 0.02696 0.00345 -0.056 EXTI Mean shift/esd = 0.062 Maximum = -0.237 for OSF Max. shift = 0.004 A for H3N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2100 / 199553 wR2 = 0.1101 before cycle 2 for 2407 data and 159 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69657 0.00198 -0.101 OSF 2 0.02685 0.00344 -0.032 EXTI Mean shift/esd = 0.022 Maximum = -0.101 for OSF Max. shift = 0.002 A for H3N Max. dU = 0.000 for H3N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2100 / 199553 wR2 = 0.1101 before cycle 3 for 2407 data and 159 / 159 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69657 0.00198 0.000 OSF 2 0.02683 0.00344 -0.005 EXTI Mean shift/esd = 0.001 Maximum = 0.018 for y H3N Max. shift = 0.001 A for H3N Max. dU = 0.000 for H3N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2100 / 199553 wR2 = 0.1101 before cycle 4 for 2407 data and 159 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69657 0.00198 0.002 OSF 2 0.02683 0.00344 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.006 for y H3N Max. shift = 0.000 A for H3N Max. dU = 0.000 for H3N Least-squares cycle 5 Maximum vector length = 511 Memory required = 2100 / 199553 wR2 = 0.1101 before cycle 5 for 2407 data and 159 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69657 0.00198 0.000 OSF 2 0.02683 0.00344 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for y H3N Max. shift = 0.000 A for H3N Max. dU = 0.000 for H3N Least-squares cycle 6 Maximum vector length = 511 Memory required = 2100 / 199553 wR2 = 0.1100 before cycle 6 for 2407 data and 159 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69657 0.00198 0.000 OSF 2 0.02683 0.00344 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y H3N Max. shift = 0.000 A for H3N Max. dU = 0.000 for H3N Largest correlation matrix elements 0.610 EXTI / OSF 0.532 U13 F2 / U11 F2 0.522 U13 F3 / U33 F3 0.546 U13 F3 / U11 F3 0.525 U13 F2 / U33 F2 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4775 0.1613 0.5356 43 0.950 0.000 C2 C3 C1 H3 0.2910 0.1742 0.4403 43 0.950 0.000 C3 C4 C2 H5 0.2654 0.0306 0.7806 43 0.950 0.000 C5 C4 C6 H7A 0.6376 0.1409 0.7207 23 0.990 0.000 C7 C1 C8 H7B 0.6262 -0.0545 0.7666 23 0.990 0.000 C7 C1 C8 H6 0.4525 0.0155 0.8741 43 0.950 0.000 C6 C5 C1 H8A 0.6353 0.2490 0.9217 137 0.980 0.000 C8 C7 H8A H8B 0.7341 0.1191 0.9418 137 0.980 0.000 C8 C7 H8A H8C 0.6301 0.0511 0.9676 137 0.980 0.000 C8 C7 H8A 2008lsh093 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.43484 0.13344 0.58563 1.00000 0.02152 0.02207 0.02541 0.00007 0.01180 0.00012 0.02207 0.00352 0.00014 0.00024 0.00016 0.00000 0.00089 0.00092 0.00086 0.00074 0.00069 0.00072 0.00039 H2 0.47750 0.16132 0.53559 1.00000 0.02648 0.00000 0.00000 C3 0.32390 0.14200 0.52850 1.00000 0.02174 0.02210 0.01896 0.00087 0.00722 0.00070 0.02094 0.00349 0.00014 0.00024 0.00016 0.00000 0.00088 0.00090 0.00080 0.00071 0.00066 0.00072 0.00038 H3 0.29095 0.17424 0.44029 1.00000 0.02513 0.00000 0.00000 C5 0.30854 0.05621 0.73078 1.00000 0.01979 0.02321 0.02157 0.00072 0.00882 -0.00127 0.02113 0.00347 0.00014 0.00024 0.00016 0.00000 0.00089 0.00095 0.00086 0.00071 0.00069 0.00070 0.00039 H5 0.26539 0.03058 0.78064 1.00000 0.02536 0.00000 0.00000 C4 0.26220 0.10276 0.60229 1.00000 0.01594 0.01953 0.02116 -0.00139 0.00428 0.00069 0.01951 0.00330 0.00013 0.00023 0.00016 0.00000 0.00082 0.00088 0.00082 0.00068 0.00064 0.00068 0.00037 C1 0.48511 0.08493 0.71464 1.00000 0.01745 0.01943 0.02450 -0.00132 0.00646 0.00063 0.02074 0.00342 0.00013 0.00023 0.00016 0.00000 0.00086 0.00089 0.00087 0.00071 0.00068 0.00069 0.00038 C7 0.60620 0.06942 0.77295 1.00000 0.01690 0.02759 0.02850 0.00114 0.00794 0.00265 0.02437 0.00358 0.00013 0.00026 0.00017 0.00000 0.00088 0.00100 0.00095 0.00077 0.00072 0.00072 0.00041 H7A 0.63760 0.14089 0.72072 1.00000 0.02925 0.00000 0.00000 H7B 0.62621 -0.05450 0.76663 1.00000 0.02925 0.00000 0.00000 C6 0.41998 0.04761 0.78580 1.00000 0.02012 0.02641 0.01952 0.00268 0.00556 0.00098 0.02243 0.00355 0.00014 0.00025 0.00016 0.00000 0.00089 0.00099 0.00085 0.00072 0.00068 0.00073 0.00040 H6 0.45245 0.01549 0.87410 1.00000 0.02691 0.00000 0.00000 C8 0.65586 0.12733 0.91356 1.00000 0.01889 0.03073 0.03137 0.00085 0.00703 -0.00067 0.02752 0.00366 0.00014 0.00027 0.00017 0.00000 0.00090 0.00108 0.00097 0.00084 0.00073 0.00077 0.00043 H8A 0.63526 0.24904 0.92169 1.00000 0.04128 0.00000 0.00000 H8B 0.73408 0.11910 0.94177 1.00000 0.04128 0.00000 0.00000 H8C 0.63014 0.05105 0.96759 1.00000 0.04128 0.00000 0.00000 N1 0.14522 0.11286 0.54157 1.00000 0.01578 0.02827 0.01955 -0.00003 0.00508 -0.00092 0.02153 0.00304 0.00011 0.00022 0.00015 0.00000 0.00075 0.00090 0.00074 0.00070 0.00059 0.00065 0.00035 O1 0.10412 0.38029 0.36912 1.00000 0.01879 0.03575 0.02381 0.00536 0.00345 0.00042 0.02725 0.00250 0.00010 0.00018 0.00011 0.00000 0.00065 0.00080 0.00065 0.00058 0.00051 0.00057 0.00033 F2 -0.12718 0.54876 0.31556 1.00000 0.03533 0.03191 0.04598 0.00339 0.02215 0.01081 0.03565 0.00247 0.00009 0.00016 0.00011 0.00000 0.00067 0.00069 0.00072 0.00053 0.00055 0.00051 0.00032 O2 0.00178 0.44383 0.16496 1.00000 0.02235 0.04782 0.02168 0.00687 0.00837 0.00686 0.03048 0.00274 0.00010 0.00020 0.00012 0.00000 0.00068 0.00092 0.00065 0.00060 0.00052 0.00061 0.00035 C11 -0.08593 0.38953 0.31134 1.00000 0.02042 0.02722 0.02418 0.00173 0.00734 0.00318 0.02410 0.00364 0.00014 0.00025 0.00017 0.00000 0.00090 0.00101 0.00087 0.00078 0.00070 0.00076 0.00040 F1 -0.16170 0.29876 0.22099 1.00000 0.02408 0.05139 0.04607 -0.01196 0.01071 -0.01119 0.04100 0.00228 0.00009 0.00018 0.00012 0.00000 0.00062 0.00084 0.00073 0.00061 0.00052 0.00056 0.00036 C10 0.01790 0.40445 0.28012 1.00000 0.02209 0.02205 0.02180 0.00013 0.00815 0.00125 0.02189 0.00349 0.00014 0.00024 0.00016 0.00000 0.00092 0.00093 0.00087 0.00072 0.00071 0.00073 0.00039 F3 -0.07052 0.31192 0.42438 1.00000 0.03390 0.05077 0.03728 0.01791 0.02190 0.01073 0.03814 0.00260 0.00009 0.00017 0.00011 0.00000 0.00066 0.00084 0.00066 0.00057 0.00052 0.00056 0.00034 H1N 0.11014 0.09881 0.60038 1.00000 0.02889 0.04107 0.00165 0.00280 0.00201 0.00000 0.00540 H2N 0.11397 0.02824 0.47409 1.00000 0.03825 0.04866 0.00177 0.00327 0.00220 0.00000 0.00611 H3N 0.12642 0.22260 0.49603 1.00000 0.03893 0.04397 0.00171 0.00337 0.00212 0.00000 0.00621 Final Structure Factor Calculation for 2008lsh093 in P2(1)/c Total number of l.s. parameters = 159 Maximum vector length = 511 Memory required = 1941 / 24017 wR2 = 0.1100 before cycle 7 for 2407 data and 0 / 159 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0206 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0476 for 1834 Fo > 4sig(Fo) and 0.0686 for all 2407 data wR2 = 0.1100, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0265 0.0221 0.0176 C2 0.0227 0.0215 0.0187 C3 0.0238 0.0220 0.0176 C5 0.0241 0.0188 0.0156 C4 0.0258 0.0192 0.0172 C1 0.0293 0.0278 0.0160 C7 0.0274 0.0219 0.0180 C6 0.0334 0.0303 0.0188 C8 0.0284 0.0206 0.0156 N1 0.0386 0.0260 0.0172 O1 0.0506 0.0365 0.0199 F2 0.0503 0.0213 0.0198 O2 0.0286 0.0246 0.0192 C11 0.0611 0.0418 0.0201 F1 0.0233 0.0217 0.0206 C10 0.0653 0.0294 0.0197 F3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.022 0.031 0.040 0.051 0.064 0.088 0.132 1.000 Number in group 243. 259. 243. 225. 257. 236. 223. 238. 241. 242. GooF 1.080 1.035 1.051 1.073 1.066 1.035 1.045 0.995 0.960 1.114 K 4.329 1.629 1.062 1.087 0.981 1.006 1.004 0.997 1.014 1.023 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 241. 246. 238. 238. 245. 238. 238. 240. 241. 242. GooF 1.058 1.019 0.975 1.089 0.983 1.018 0.924 0.888 1.111 1.331 K 1.120 1.101 1.009 0.966 0.992 1.009 1.021 1.035 1.030 1.016 R1 0.203 0.167 0.150 0.099 0.084 0.059 0.044 0.038 0.039 0.031 Recommended weighting scheme: WGHT 0.0179 0.6448 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) 1 3 6 81.35 52.42 3.91 0.045 1.37 -8 0 4 59.60 29.11 3.90 0.033 1.61 -6 1 5 453.13 365.74 3.87 0.118 1.78 -12 2 12 290.89 24.82 3.73 0.031 0.81 -3 1 2 557.82 673.54 3.73 0.160 3.55 -6 0 14 5.25 37.03 3.73 0.037 0.79 -3 1 1 599.70 729.09 3.72 0.166 3.84 0 1 1 115.55 163.28 3.63 0.079 6.13 -5 7 3 11.98 26.46 3.43 0.032 1.00 -4 2 1 234.18 290.47 3.33 0.105 2.51 -15 1 4 116.28 76.48 3.28 0.054 0.88 -5 1 4 61.42 40.02 3.28 0.039 2.15 0 1 3 2005.40 2292.09 3.28 0.294 3.14 5 0 4 129.84 93.65 3.16 0.059 1.54 11 0 0 10.09 0.22 3.12 0.003 1.13 1 1 3 33.44 19.17 3.10 0.027 2.84 11 2 1 121.00 158.92 3.05 0.078 1.04 -2 3 7 15.41 6.28 2.91 0.015 1.34 -7 1 6 17.75 30.95 2.84 0.034 1.51 -9 2 7 167.28 133.37 2.82 0.071 1.20 -6 3 6 271.27 222.46 2.77 0.092 1.38 0 2 11 65.14 90.92 2.75 0.059 0.91 11 0 2 168.62 219.35 2.74 0.091 1.03 2 2 1 150.63 186.55 2.74 0.084 2.95 3 4 2 7.94 0.05 2.74 0.001 1.57 -6 1 7 200.43 240.51 2.74 0.095 1.45 -7 2 14 19.79 1.71 2.69 0.008 0.77 2 0 2 863.73 979.36 2.69 0.192 3.43 -5 0 4 746.41 854.97 2.68 0.180 2.24 -2 3 10 50.16 70.80 2.66 0.052 1.00 0 5 7 11.96 3.97 2.65 0.012 1.06 -13 2 5 35.88 19.99 2.65 0.027 0.99 -12 6 8 89.46 54.63 2.65 0.045 0.79 11 4 3 52.24 87.50 2.64 0.058 0.87 -13 2 9 31.85 17.42 2.63 0.026 0.89 3 0 2 92.67 118.23 2.61 0.067 2.79 0 2 4 81.88 62.20 2.61 0.048 2.14 -1 2 7 712.16 629.59 2.60 0.154 1.42 -2 1 7 2.81 10.62 2.60 0.020 1.54 0 0 10 75.38 107.86 2.60 0.064 1.04 -3 9 2 11.51 0.89 2.57 0.006 0.83 6 1 1 1741.94 1566.38 2.56 0.243 1.85 -7 8 3 21.24 0.01 2.56 0.001 0.85 -4 8 1 7.13 17.92 2.56 0.026 0.92 -1 7 3 -1.94 4.23 2.50 0.013 1.04 1 8 3 16.94 29.28 2.48 0.033 0.91 -9 8 3 -1.39 12.64 2.46 0.022 0.80 -11 1 11 54.44 78.94 2.44 0.055 0.89 -1 1 1 138.80 184.50 2.44 0.084 6.03 6 2 9 21.86 37.26 2.43 0.038 0.86 Bond lengths and angles C2 - Distance Angles C3 1.3898 (0.0024) C1 1.3951 (0.0024) 121.64 (0.15) H2 0.9500 119.18 119.18 C2 - C3 C1 C3 - Distance Angles C4 1.3847 (0.0024) C2 1.3898 (0.0024) 118.90 (0.15) H3 0.9500 120.55 120.55 C3 - C4 C2 C5 - Distance Angles C4 1.3811 (0.0023) C6 1.3944 (0.0024) 118.61 (0.16) H5 0.9500 120.69 120.69 C5 - C4 C6 C4 - Distance Angles C5 1.3811 (0.0023) C3 1.3847 (0.0024) 121.45 (0.16) N1 1.4664 (0.0022) 119.93 (0.15) 118.61 (0.15) C4 - C5 C3 C1 - Distance Angles C2 1.3951 (0.0024) C6 1.3958 (0.0024) 117.61 (0.15) C7 1.5172 (0.0023) 120.49 (0.15) 121.87 (0.15) C1 - C2 C6 C7 - Distance Angles C1 1.5172 (0.0023) C8 1.5248 (0.0025) 114.95 (0.15) H7A 0.9900 108.53 108.53 H7B 0.9900 108.53 108.53 107.53 C7 - C1 C8 H7A C6 - Distance Angles C5 1.3944 (0.0024) C1 1.3958 (0.0024) 121.77 (0.16) H6 0.9500 119.11 119.11 C6 - C5 C1 C8 - Distance Angles C7 1.5248 (0.0025) 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 C4 1.4664 (0.0022) H1N 0.9346 (0.0219) 113.03 (1.24) H2N 0.9622 (0.0244) 114.67 (1.33) 106.19 (1.86) H3N 0.9620 (0.0252) 108.80 (1.31) 111.29 (1.83) 102.38 (1.79) N1 - C4 H1N H2N O1 - Distance Angles C10 1.2340 (0.0020) O1 - F2 - Distance Angles C11 1.3395 (0.0022) F2 - O2 - Distance Angles C10 1.2525 (0.0020) O2 - C11 - Distance Angles F3 1.3329 (0.0021) F1 1.3349 (0.0021) 107.27 (0.15) F2 1.3395 (0.0022) 107.23 (0.14) 106.47 (0.14) C10 1.5485 (0.0025) 113.08 (0.14) 111.73 (0.15) 110.71 (0.15) C11 - F3 F1 F2 F1 - Distance Angles C11 1.3349 (0.0021) F1 - C10 - Distance Angles O1 1.2340 (0.0020) O2 1.2525 (0.0020) 128.48 (0.17) C11 1.5485 (0.0025) 117.74 (0.15) 113.76 (0.15) C10 - O1 O2 F3 - Distance Angles C11 1.3329 (0.0021) F3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.93(2) 1.86(2) 2.756(2) 160.4(18) N1-H1N...O2_$1 0.96(2) 1.87(2) 2.747(2) 151(2) N1-H2N...O2_$2 0.96(3) 1.79(2) 2.711(2) 159(2) N1-H3N...O1 0.96(3) 2.55(2) 3.1014(19) 116.2(16) N1-H3N...F3 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)