+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:29:36 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh119 in P2(1)/c CELL 0.71073 8.2778 7.0864 14.7146 90.000 97.230 90.000 ZERR 4.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 28 28 8 8 12 V = 856.29 F(000) = 424.0 Mu = 0.16 mm-1 Cell Wt = 832.58 Rho = 1.615 MERG 2 OMIT -3.00 55.00 OMIT -2 0 4 OMIT 1 1 1 OMIT -2 0 2 OMIT -1 1 4 OMIT 0 0 4 OMIT -1 1 3 OMIT 0 1 1 OMIT -1 1 5 DFIX 0.88 0.02 N1 H1N N2 H2AN N2 H2BN EQIV $1 x+1, y+1, z EQIV $2 -x+2, -y+1, -z+1 HTAB N2 O2_$1 HTAB N2 O2_$2 HTAB N1 O1 FMAP 2 PLAN 5 SIZE 0.26 0.26 0.34 ACTA HTAB 2.00000 BOND $H L.S. 6 TEMP -153.00 WGHT 0.0482 0.4828 EXTI 0.045350 FVAR 1.40156 C1 1 1.294295 0.498161 0.579916 11.00000 0.01666 0.02176 = 0.02318 -0.00020 0.00257 -0.00155 AFIX 43 H1 2 1.204199 0.565595 0.549342 11.00000 -1.20000 AFIX 0 C2 1 1.446185 0.587278 0.599116 11.00000 0.01910 0.02003 = 0.02083 -0.00205 0.00415 -0.00205 C3 1 1.574339 0.479538 0.644920 11.00000 0.01639 0.02554 = 0.02285 -0.00138 0.00240 -0.00355 AFIX 43 H3 2 1.679095 0.534544 0.659309 11.00000 -1.20000 AFIX 0 C4 1 1.549073 0.294880 0.669063 11.00000 0.02130 0.02509 = 0.02336 0.00076 0.00146 0.00170 AFIX 43 H4 2 1.636050 0.223363 0.700237 11.00000 -1.20000 AFIX 0 C5 1 1.396846 0.213765 0.647838 11.00000 0.02523 0.02023 = 0.02526 0.00057 0.00354 -0.00211 AFIX 43 H5 2 1.378455 0.086284 0.663674 11.00000 -1.20000 AFIX 0 C6 1 0.885725 0.046062 0.580389 11.00000 0.01743 0.02236 = 0.02446 -0.00191 0.00487 -0.00122 C7 1 0.963125 -0.092746 0.654300 11.00000 0.02111 0.03486 = 0.03267 0.00827 0.00018 -0.00844 N1 3 1.276095 0.318104 0.604628 11.00000 0.01728 0.02230 = 0.02474 -0.00204 0.00319 -0.00483 N2 3 1.465880 0.770104 0.575891 11.00000 0.02077 0.02161 = 0.03389 0.00395 0.00080 -0.00460 O1 4 0.966904 0.186727 0.563953 11.00000 0.02112 0.02390 = 0.03498 0.00220 0.00177 -0.00526 O2 4 0.745466 0.000814 0.547588 11.00000 0.01666 0.02755 = 0.03860 0.00375 -0.00002 -0.00464 F1 5 1.123944 -0.076550 0.673105 11.00000 0.02452 0.06767 = 0.08057 0.04371 -0.01760 -0.01521 F2 5 0.933969 -0.273100 0.631314 11.00000 0.04168 0.02879 = 0.06117 0.01542 0.00000 -0.00228 F3 5 0.900076 -0.064968 0.732620 11.00000 0.07948 0.07828 = 0.02792 0.01089 0.01427 -0.00222 H2AN 2 1.566945 0.813726 0.576594 11.00000 0.03432 H2BN 2 1.387705 0.829445 0.536716 11.00000 0.04148 H1N 2 1.175826 0.270284 0.592618 11.00000 0.03637 HKLF 4 Covalent radii and connectivity table for 2008lsh119 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - N1 C2 C2 - N2 C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - N1 C4 C6 - O2 O1 C7 C7 - F1 F2 F3 C6 N1 - C5 C1 N2 - C2 O1 - C6 O2 - C6 F1 - C7 F2 - C7 F3 - C7 Operators for generating equivalent atoms: $1 x+1, y+1, z $2 -x+2, -y+1, -z+1 h k l Fo^2 Sigma Why rejected -6 0 1 21.38 4.29 observed but should be systematically absent -10 0 7 19.02 4.72 observed but should be systematically absent 13178 Reflections read, of which 648 rejected -10 =< h =< 10, -9 =< k =< 9, -19 =< l =< 19, Max. 2-theta = 54.98 2 Systematic absence violations 0 Inconsistent equivalents 1954 Unique reflections, of which 0 suppressed R(int) = 0.0418 R(sigma) = 0.0274 Friedel opposites merged Maximum memory for data reduction = 1389 / 19485 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 = 1715 / 177247 wR2 = 0.1085 before cycle 1 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.066; Restrained GooF = 1.066 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40152 0.00506 -0.007 OSF 2 0.04527 0.00948 -0.009 EXTI Mean shift/esd = 0.032 Maximum = -0.120 for U33 F3 Max. shift = 0.002 A for H2BN Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1715 / 177247 wR2 = 0.1085 before cycle 2 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40130 0.00505 -0.043 OSF 2 0.04518 0.00948 -0.010 EXTI Mean shift/esd = 0.012 Maximum = -0.043 for OSF Max. shift = 0.001 A for H1N Max. dU = 0.000 for H2BN Least-squares cycle 3 Maximum vector length = 511 Memory required = 1715 / 177247 wR2 = 0.1085 before cycle 3 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.023 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40130 0.00505 -0.001 OSF 2 0.04515 0.00948 -0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.004 for U22 F1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2BN Least-squares cycle 4 Maximum vector length = 511 Memory required = 1715 / 177247 wR2 = 0.1085 before cycle 4 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.023 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40130 0.00505 0.000 OSF 2 0.04515 0.00948 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U23 C2 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2BN Least-squares cycle 5 Maximum vector length = 511 Memory required = 1715 / 177247 wR2 = 0.1085 before cycle 5 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.023 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40130 0.00505 0.000 OSF 2 0.04515 0.00948 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2BN Least-squares cycle 6 Maximum vector length = 511 Memory required = 1715 / 177247 wR2 = 0.1085 before cycle 6 for 1954 data and 140 / 140 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.023 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.40130 0.00505 0.000 OSF 2 0.04515 0.00948 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2AN Largest correlation matrix elements 0.657 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 1.2042 0.5656 0.5493 43 0.950 0.000 C1 N1 C2 H3 1.6791 0.5345 0.6593 43 0.950 0.000 C3 C4 C2 H4 1.6360 0.2234 0.7002 43 0.950 0.000 C4 C3 C5 H5 1.3785 0.0863 0.6637 43 0.950 0.000 C5 N1 C4 2008lsh119 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.29430 0.49816 0.57992 1.00000 0.01667 0.02169 0.02311 -0.00020 0.00259 -0.00153 0.02048 0.00243 0.00016 0.00020 0.00009 0.00000 0.00063 0.00067 0.00066 0.00051 0.00048 0.00050 0.00031 H1 1.20421 0.56559 0.54934 1.00000 0.02458 0.00000 0.00000 C2 1.44618 0.58728 0.59912 1.00000 0.01909 0.01997 0.02077 -0.00206 0.00415 -0.00204 0.01981 0.00241 0.00016 0.00019 0.00009 0.00000 0.00065 0.00066 0.00061 0.00049 0.00048 0.00051 0.00030 C3 1.57433 0.47953 0.64492 1.00000 0.01638 0.02549 0.02279 -0.00140 0.00239 -0.00355 0.02156 0.00246 0.00016 0.00021 0.00009 0.00000 0.00064 0.00071 0.00064 0.00053 0.00049 0.00052 0.00031 H3 1.67908 0.53453 0.65932 1.00000 0.02587 0.00000 0.00000 C4 1.54906 0.29488 0.66906 1.00000 0.02128 0.02505 0.02329 0.00077 0.00146 0.00169 0.02332 0.00256 0.00017 0.00021 0.00009 0.00000 0.00069 0.00072 0.00066 0.00053 0.00051 0.00054 0.00032 H4 1.63604 0.22337 0.70023 1.00000 0.02798 0.00000 0.00000 C5 1.39686 0.21376 0.64784 1.00000 0.02525 0.02016 0.02521 0.00058 0.00356 -0.00212 0.02350 0.00257 0.00018 0.00020 0.00010 0.00000 0.00072 0.00066 0.00067 0.00052 0.00053 0.00055 0.00032 H5 1.37847 0.08628 0.66368 1.00000 0.02820 0.00000 0.00000 C6 0.88572 0.04608 0.58039 1.00000 0.01740 0.02237 0.02443 -0.00191 0.00488 -0.00122 0.02121 0.00244 0.00016 0.00020 0.00009 0.00000 0.00063 0.00068 0.00069 0.00052 0.00050 0.00053 0.00031 C7 0.96311 -0.09273 0.65429 1.00000 0.02110 0.03486 0.03259 0.00823 0.00017 -0.00848 0.02979 0.00287 0.00018 0.00023 0.00011 0.00000 0.00071 0.00085 0.00079 0.00063 0.00057 0.00061 0.00037 N1 1.27610 0.31812 0.60463 1.00000 0.01727 0.02225 0.02466 -0.00205 0.00317 -0.00484 0.02135 0.00210 0.00014 0.00017 0.00008 0.00000 0.00056 0.00061 0.00059 0.00045 0.00043 0.00045 0.00029 N2 1.46587 0.77010 0.57589 1.00000 0.02073 0.02162 0.03384 0.00394 0.00080 -0.00459 0.02562 0.00229 0.00015 0.00018 0.00009 0.00000 0.00062 0.00062 0.00068 0.00049 0.00049 0.00049 0.00030 O1 0.96690 0.18673 0.56395 1.00000 0.02106 0.02389 0.03494 0.00220 0.00177 -0.00528 0.02678 0.00185 0.00012 0.00015 0.00007 0.00000 0.00052 0.00054 0.00057 0.00042 0.00040 0.00041 0.00028 O2 0.74546 0.00081 0.54759 1.00000 0.01665 0.02753 0.03852 0.00373 -0.00005 -0.00467 0.02787 0.00190 0.00012 0.00015 0.00008 0.00000 0.00050 0.00057 0.00061 0.00044 0.00041 0.00040 0.00028 F1 1.12394 -0.07653 0.67311 1.00000 0.02448 0.06770 0.08047 0.04375 -0.01759 -0.01522 0.05961 0.00234 0.00013 0.00019 0.00009 0.00000 0.00054 0.00086 0.00088 0.00069 0.00052 0.00051 0.00042 F2 0.93397 -0.27309 0.63132 1.00000 0.04164 0.02876 0.06113 0.01541 0.00000 -0.00227 0.04440 0.00201 0.00013 0.00015 0.00008 0.00000 0.00062 0.00053 0.00071 0.00047 0.00050 0.00044 0.00032 F3 0.90007 -0.06497 0.73262 1.00000 0.07945 0.07828 0.02783 0.01090 0.01428 -0.00213 0.06121 0.00257 0.00018 0.00021 0.00008 0.00000 0.00095 0.00094 0.00057 0.00056 0.00055 0.00073 0.00041 H2AN 1.56696 0.81369 0.57669 1.00000 0.03456 0.03185 0.00191 0.00276 0.00135 0.00000 0.00496 H2BN 1.38741 0.82934 0.53670 1.00000 0.04178 0.03662 0.00232 0.00282 0.00132 0.00000 0.00545 H1N 1.17570 0.27009 0.59257 1.00000 0.03663 0.03068 0.00194 0.00287 0.00134 0.00000 0.00516 Final Structure Factor Calculation for 2008lsh119 in P2(1)/c Total number of l.s. parameters = 140 Maximum vector length = 511 Memory required = 1575 / 24017 wR2 = 0.1085 before cycle 7 for 1954 data and 0 / 140 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 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 0.023 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.067 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0432 for 1755 Fo > 4sig(Fo) and 0.0479 for all 1954 data wR2 = 0.1085, GooF = S = 1.067, Restrained GooF = 1.067 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 7.00 for hydrogen atoms Principal mean square atomic displacements U 0.0231 0.0221 0.0162 C1 0.0236 0.0184 0.0174 C2 0.0270 0.0226 0.0152 C3 0.0257 0.0241 0.0201 C4 0.0260 0.0253 0.0192 C5 0.0260 0.0212 0.0164 C6 0.0461 0.0264 0.0168 C7 0.0267 0.0231 0.0143 N1 0.0366 0.0239 0.0164 N2 0.0364 0.0270 0.0169 O1 0.0414 0.0273 0.0149 O2 0.1304 0.0303 0.0181 F1 0.0702 0.0405 0.0225 F2 0.0815 0.0789 0.0232 F3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.032 0.049 0.066 0.086 0.114 0.144 0.191 0.289 1.000 Number in group 196. 195. 198. 193. 195. 205. 186. 194. 197. 195. GooF 1.202 1.008 1.237 0.981 1.000 1.039 0.985 1.016 0.972 1.179 K 2.524 1.110 1.007 0.975 0.970 0.995 0.998 1.005 1.019 1.013 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.62 inf Number in group 197. 199. 193. 193. 202. 190. 193. 196. 194. 197. GooF 0.927 0.940 0.993 1.024 1.000 1.043 1.120 1.007 1.165 1.377 K 1.032 1.029 1.002 0.988 1.002 1.034 1.016 1.025 1.017 1.002 R1 0.090 0.088 0.079 0.070 0.055 0.049 0.041 0.032 0.034 0.034 Recommended weighting scheme: WGHT 0.0474 0.4895 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) 5 5 0 18.67 0.13 5.97 0.005 1.07 3 5 0 27.91 6.67 5.93 0.038 1.26 1 1 0 229.82 466.17 5.49 0.314 5.37 2 1 1 378.87 489.79 3.92 0.322 3.37 4 3 0 19.15 8.74 3.86 0.043 1.55 5 2 2 9.97 3.22 3.75 0.026 1.43 -1 7 2 12.81 4.95 3.57 0.032 1.00 8 4 3 6.21 0.77 3.43 0.013 0.86 -2 2 5 5.16 1.13 3.39 0.015 2.06 -8 2 3 14.80 3.91 3.28 0.029 0.99 -2 1 2 531.14 637.49 2.98 0.367 3.34 4 3 7 25.85 39.38 2.88 0.091 1.19 -3 0 2 554.64 663.66 2.85 0.375 2.68 9 4 2 13.22 5.70 2.83 0.035 0.80 5 3 5 24.14 37.13 2.80 0.089 1.18 1 0 2 1403.36 1686.92 2.79 0.597 5.14 5 1 0 16.26 9.01 2.78 0.044 1.60 0 8 1 2.76 7.98 2.76 0.041 0.88 -6 0 16 0.80 11.51 2.74 0.049 0.81 -10 1 1 3.49 0.02 2.72 0.002 0.82 -3 6 6 30.21 44.18 2.72 0.097 1.01 3 2 5 6.59 2.59 2.71 0.023 1.66 3 5 2 56.90 40.72 2.67 0.093 1.23 6 4 1 179.19 143.39 2.66 0.174 1.07 -8 3 2 21.07 12.39 2.64 0.051 0.95 2 1 5 49.89 66.76 2.63 0.119 2.14 -1 1 9 21.36 13.44 2.60 0.053 1.59 1 7 6 0.18 3.36 2.58 0.027 0.92 7 6 2 18.07 9.56 2.57 0.045 0.82 -2 7 1 4.39 0.66 2.52 0.012 0.98 0 4 0 3285.31 2799.78 2.48 0.769 1.77 -3 1 1 40.17 28.97 2.48 0.078 2.57 -5 8 3 57.12 40.89 2.47 0.093 0.78 1 3 8 1.94 0.11 2.46 0.005 1.40 0 1 3 1.22 0.00 2.45 0.001 4.01 0 1 2 2.72 6.87 2.39 0.038 5.08 -2 3 4 21.71 31.44 2.38 0.082 1.84 1 1 8 90.46 72.58 2.36 0.124 1.69 6 4 5 2.37 6.48 2.35 0.037 0.98 6 3 3 205.75 243.87 2.33 0.227 1.12 -5 5 1 692.36 602.87 2.32 0.357 1.08 8 4 7 50.13 36.93 2.30 0.088 0.79 0 3 6 135.51 162.31 2.26 0.185 1.69 2 1 9 439.62 382.20 2.25 0.284 1.42 6 6 0 25.67 17.09 2.24 0.060 0.89 3 2 6 39.75 29.66 2.22 0.079 1.54 -6 4 2 8.28 4.13 2.22 0.030 1.09 -1 0 2 97.52 79.01 2.21 0.129 5.83 -4 3 4 415.45 477.52 2.20 0.318 1.48 -1 0 8 130.56 108.69 2.18 0.152 1.83 Bond lengths and angles C1 - Distance Angles N1 1.3403 (0.0018) C2 1.4035 (0.0019) 120.14 (0.13) H1 0.9500 119.93 119.93 C1 - N1 C2 C2 - Distance Angles N2 1.3549 (0.0018) C1 1.4035 (0.0019) 120.84 (0.13) C3 1.4080 (0.0019) 122.14 (0.13) 117.01 (0.13) C2 - N2 C1 C3 - Distance Angles C4 1.3787 (0.0020) C2 1.4080 (0.0019) 120.56 (0.13) H3 0.9500 119.72 119.72 C3 - C4 C2 C4 - Distance Angles C3 1.3787 (0.0020) C5 1.3843 (0.0020) 119.96 (0.13) H4 0.9500 120.02 120.02 C4 - C3 C5 C5 - Distance Angles N1 1.3380 (0.0019) C4 1.3843 (0.0020) 118.81 (0.13) H5 0.9500 120.59 120.59 C5 - N1 C4 C6 - Distance Angles O2 1.2421 (0.0017) O1 1.2427 (0.0017) 129.30 (0.14) C7 1.5444 (0.0021) 113.19 (0.12) 117.47 (0.12) C6 - O2 O1 C7 - Distance Angles F1 1.3302 (0.0018) F2 1.3362 (0.0020) 106.22 (0.14) F3 1.3383 (0.0020) 107.25 (0.14) 106.31 (0.13) C6 1.5444 (0.0021) 114.03 (0.12) 112.67 (0.13) 109.92 (0.14) C7 - F1 F2 F3 N1 - Distance Angles C5 1.3380 (0.0019) C1 1.3403 (0.0018) 123.52 (0.12) H1N 0.8949 (0.0150) 120.24 (1.36) 116.20 (1.35) N1 - C5 C1 N2 - Distance Angles C2 1.3549 (0.0018) H2AN 0.8906 (0.0149) 118.10 (1.31) H2BN 0.9145 (0.0155) 119.97 (1.36) 116.14 (1.88) N2 - C2 H2AN O1 - Distance Angles C6 1.2427 (0.0017) O1 - O2 - Distance Angles C6 1.2421 (0.0017) O2 - F1 - Distance Angles C7 1.3302 (0.0018) F1 - F2 - Distance Angles C7 1.3362 (0.0020) F2 - F3 - Distance Angles C7 1.3383 (0.0020) F3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.891(15) 2.070(16) 2.9061(16) 156.0(18) N2-H2AN...O2_$1 0.915(15) 1.963(16) 2.8631(17) 168(2) N2-H2BN...O2_$2 0.895(15) 1.825(15) 2.7186(15) 176(2) N1-H1N...O1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)