+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 23:19:19 on 12-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh028 in P2(1)2(1)2(1) CELL 0.71073 5.1717 9.7527 17.8113 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0013 0.0024 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 36 32 4 4 12 V = 898.37 F(000) = 416.0 Mu = 0.14 mm-1 Cell Wt = 812.66 Rho = 1.502 MERG 2 OMIT -3.00 55.00 EADP F1A F1B EADP F2A F2B EADP F3A F3B EQIV $1 -x, y+1/2, -z+3/2 HTAB N1 O1_$1 FMAP 2 PLAN 5 SIZE 0.02 0.08 0.24 ACTA HTAB 2.00000 BOND $H L.S. 6 TWIN TEMP -153.00 WGHT 0.0198 1.3286 BASF 0.3 FVAR 0.87197 0.93630 C1 1 0.342137 0.210480 0.670123 11.00000 0.03967 0.03740 = 0.03866 0.00110 -0.00529 0.00116 C2 1 0.393329 0.085633 0.636209 11.00000 0.04211 0.03664 = 0.04773 -0.00229 -0.00007 -0.00035 AFIX 43 H2 2 0.291227 0.007273 0.647387 11.00000 -1.20000 AFIX 0 C3 1 0.597959 0.077139 0.585254 11.00000 0.04554 0.03942 = 0.04166 -0.00284 0.00305 0.00870 C4 1 0.744297 0.189516 0.567108 11.00000 0.03678 0.05848 = 0.04622 0.00431 0.00303 -0.00228 AFIX 43 H4 2 0.881879 0.181913 0.532013 11.00000 -1.20000 AFIX 0 C5 1 0.688942 0.314551 0.600650 11.00000 0.04566 0.04626 = 0.05395 0.00524 -0.00121 -0.00966 AFIX 43 H5 2 0.786096 0.393720 0.587619 11.00000 -1.20000 AFIX 0 C6 1 0.494122 0.323847 0.652579 11.00000 0.05257 0.03737 = 0.04840 0.00241 -0.00551 -0.00227 AFIX 43 H6 2 0.462371 0.408851 0.676940 11.00000 -1.20000 AFIX 0 C7 1 0.002715 0.133629 0.759573 11.00000 0.04317 0.04200 = 0.04173 0.00125 -0.01067 0.00496 C8 1 -0.188134 0.188643 0.816324 11.00000 0.05611 0.03913 = 0.04918 0.00257 -0.00031 0.00242 AFIX 137 H8A 2 -0.356651 0.144854 0.808693 11.00000 -1.50000 H8B 2 -0.205508 0.288022 0.809935 11.00000 -1.50000 H8C 2 -0.126005 0.168728 0.867147 11.00000 -1.50000 AFIX 0 C9 1 0.647912 -0.058758 0.550274 11.00000 0.05437 0.05505 = 0.05527 0.00504 0.00813 0.00540 N1 3 0.145757 0.229949 0.724053 11.00000 0.04482 0.03129 = 0.04772 -0.00273 0.00396 -0.00629 O1 4 0.028232 0.009181 0.749391 11.00000 0.06372 0.03007 = 0.06563 0.00322 0.01456 0.00259 PART 1 F1A 5 0.679893 -0.158759 0.600488 21.00000 0.10509 0.04929 = 0.06530 0.00581 0.00726 0.02271 F3A 5 0.457120 -0.103028 0.506376 21.00000 0.09139 0.06987 = 0.08822 -0.03416 -0.02886 0.01654 F2A 5 0.859680 -0.061666 0.507155 21.00000 0.09048 0.06289 = 0.13309 -0.01884 0.06513 -0.00314 PART 2 SAME F1A > F3A F2B 5 0.716897 -0.026015 0.486419 -21.00000 0.09048 0.06289 = 0.13309 -0.01884 0.06513 -0.00314 F3B 5 0.477974 -0.132704 0.558890 -21.00000 0.09139 0.06987 = 0.08822 -0.03416 -0.02886 0.01654 F1B 5 0.831075 -0.111299 0.585328 -21.00000 0.10509 0.04929 = 0.06530 0.00581 0.00726 0.02271 PART 0 H1N 2 0.103233 0.320721 0.740187 11.00000 0.04192 HKLF 4 Covalent radii and connectivity table for 2008lsh028 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C9 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - F3B_b F2B_b F1B_b F3A_a F1A_a F2A_a C3 N1 - C7 C1 O1 - C7 F1A_a - C9 F3A_a - C9 F2A_a - C9 F2B_b - C9 F3B_b - C9 F1B_b - C9 Operators for generating equivalent atoms: $1 -x, y+1/2, -z+3/2 9185 Reflections read, of which 77 rejected -6 =< h =< 5, -12 =< k =< 12, -23 =< l =< 23, 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) 4 8 1 35.42 5.34 2 47.33 -5 6 3 15.86 4.71 2 24.86 -4 9 3 8.08 5.34 2 63.11 3 10 4 4.42 6.96 2 42.07 3 8 5 -2.01 1.91 3 18.09 -3 8 6 21.07 3.97 3 20.09 3 9 7 48.81 11.11 2 57.96 -3 8 9 24.15 4.52 2 29.36 8 Inconsistent equivalents 2032 Unique reflections, of which 0 suppressed R(int) = 0.0972 R(sigma) = 0.0927 Friedel opposites not merged Maximum memory for data reduction = 1538 / 20163 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 = 1933 / 180745 wR2 = 0.1700 before cycle 1 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87194 0.00319 -0.008 OSF 2 0.93638 0.00716 0.012 FVAR 2 3 0.44752 2.54019 0.058 BASF 1 Mean shift/esd = 0.007 Maximum = 0.058 for BASF 1 Max. shift = 0.002 A for F2B_b Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1933 / 180745 wR2 = 0.1700 before cycle 2 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87193 0.00319 -0.005 OSF 2 0.93646 0.00716 0.010 FVAR 2 3 0.50009 2.54001 0.021 BASF 1 Mean shift/esd = 0.003 Maximum = 0.021 for BASF 1 Max. shift = 0.001 A for F2B_b Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1933 / 180745 wR2 = 0.1700 before cycle 3 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87193 0.00319 0.000 OSF 2 0.93646 0.00716 0.000 FVAR 2 3 0.50133 2.54001 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.005 for tors H8A Max. shift = 0.000 A for F3B_b Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1933 / 180745 wR2 = 0.1700 before cycle 4 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87193 0.00319 0.000 OSF 2 0.93646 0.00715 0.001 FVAR 2 3 0.50165 2.53993 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for F3B_b Max. dU = 0.000 for F3A_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 1933 / 180745 wR2 = 0.1700 before cycle 5 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87193 0.00319 0.000 OSF 2 0.93647 0.00715 0.001 FVAR 2 3 0.50202 2.53996 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for F3B_b Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1933 / 180745 wR2 = 0.1700 before cycle 6 for 2032 data and 143 / 143 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87193 0.00319 0.000 OSF 2 0.93647 0.00715 0.000 FVAR 2 3 0.50193 2.53995 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for F3B_b Max. dU = 0.000 for H1N Largest correlation matrix elements 0.609 U33 F3A_a / FVAR 2 0.538 z F3B_b / z F3A_a 0.502 x F1A_a / FVAR 2 0.568 U13 F2A_a / U33 F2A_a -0.537 x F2B_b / FVAR 2 -0.558 x F2A_a / FVAR 2 0.503 x F2B_b / x F2A_a Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2912 0.0073 0.6474 43 0.950 0.000 C2 C1 C3 H4 0.8819 0.1819 0.5320 43 0.950 0.000 C4 C3 C5 H5 0.7861 0.3937 0.5876 43 0.950 0.000 C5 C6 C4 H6 0.4624 0.4088 0.6769 43 0.950 0.000 C6 C5 C1 H8A -0.3567 0.1449 0.8087 137 0.980 0.000 C8 C7 H8A H8B -0.2054 0.2880 0.8100 137 0.980 0.000 C8 C7 H8A H8C -0.1261 0.1686 0.8672 137 0.980 0.000 C8 C7 H8A 2008lsh028 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.34214 0.21048 0.67012 1.00000 0.03966 0.03737 0.03861 0.00111 -0.00526 0.00118 0.03855 0.00781 0.00094 0.00045 0.00024 0.00000 0.00242 0.00277 0.00246 0.00209 0.00227 0.00234 0.00109 C2 0.39333 0.08563 0.63621 1.00000 0.04213 0.03661 0.04771 -0.00229 -0.00008 -0.00037 0.04215 0.00820 0.00093 0.00050 0.00026 0.00000 0.00269 0.00259 0.00275 0.00235 0.00225 0.00238 0.00115 H2 0.29123 0.00727 0.64739 1.00000 0.05058 0.00000 0.00000 C3 0.59793 0.07714 0.58525 1.00000 0.04552 0.03937 0.04167 -0.00285 0.00304 0.00867 0.04219 0.00862 0.00096 0.00051 0.00025 0.00000 0.00287 0.00256 0.00261 0.00240 0.00223 0.00240 0.00115 C4 0.74430 0.18951 0.56711 1.00000 0.03679 0.05851 0.04625 0.00432 0.00305 -0.00226 0.04718 0.00873 0.00095 0.00056 0.00027 0.00000 0.00259 0.00349 0.00288 0.00272 0.00213 0.00269 0.00130 H4 0.88189 0.18190 0.53202 1.00000 0.05662 0.00000 0.00000 C5 0.68894 0.31456 0.60065 1.00000 0.04567 0.04626 0.05388 0.00521 -0.00114 -0.00965 0.04860 0.00869 0.00100 0.00053 0.00028 0.00000 0.00298 0.00305 0.00307 0.00273 0.00259 0.00270 0.00128 H5 0.78609 0.39373 0.58762 1.00000 0.05832 0.00000 0.00000 C6 0.49413 0.32384 0.65258 1.00000 0.05259 0.03735 0.04839 0.00240 -0.00550 -0.00223 0.04611 0.00858 0.00102 0.00050 0.00026 0.00000 0.00306 0.00257 0.00278 0.00237 0.00252 0.00257 0.00121 H6 0.46237 0.40884 0.67694 1.00000 0.05533 0.00000 0.00000 C7 0.00271 0.13363 0.75958 1.00000 0.04312 0.04210 0.04172 0.00126 -0.01068 0.00494 0.04231 0.00840 0.00100 0.00049 0.00027 0.00000 0.00266 0.00277 0.00272 0.00220 0.00250 0.00246 0.00118 C8 -0.18814 0.18865 0.81633 1.00000 0.05611 0.03909 0.04920 0.00259 -0.00025 0.00241 0.04813 0.00865 0.00100 0.00051 0.00026 0.00000 0.00319 0.00277 0.00283 0.00238 0.00263 0.00263 0.00126 H8A -0.35671 0.14494 0.80867 1.00000 0.07220 0.00000 0.00000 H8B -0.20536 0.28804 0.80998 1.00000 0.07220 0.00000 0.00000 H8C -0.12609 0.16864 0.86715 1.00000 0.07220 0.00000 0.00000 C9 0.64792 -0.05875 0.55027 1.00000 0.05441 0.05505 0.05531 0.00501 0.00820 0.00538 0.05492 0.01080 0.00123 0.00059 0.00031 0.00000 0.00353 0.00356 0.00340 0.00291 0.00325 0.00310 0.00143 N1 0.14575 0.22994 0.72405 1.00000 0.04480 0.03123 0.04775 -0.00273 0.00397 -0.00628 0.04126 0.00682 0.00084 0.00040 0.00021 0.00000 0.00233 0.00222 0.00235 0.00185 0.00208 0.00205 0.00098 O1 0.02824 0.00917 0.74939 1.00000 0.06372 0.03001 0.06566 0.00322 0.01456 0.00258 0.05313 0.00654 0.00073 0.00032 0.00021 0.00000 0.00230 0.00175 0.00229 0.00171 0.00209 0.00183 0.00096 F1A_a 0.67990 -0.15877 0.60049 0.93647 0.10504 0.04933 0.06530 0.00581 0.00727 0.02272 0.07322 0.00844 0.00109 0.00040 0.00022 0.00715 0.00379 0.00227 0.00231 0.00195 0.00253 0.00244 0.00137 F3A_a 0.45712 -0.10303 0.50638 0.93647 0.09132 0.06989 0.08828 -0.03415 -0.02886 0.01651 0.08316 0.00642 0.00081 0.00039 0.00028 0.00715 0.00309 0.00257 0.00359 0.00251 0.00255 0.00220 0.00157 F2A_a 0.85967 -0.06166 0.50715 0.93647 0.09047 0.06289 0.13304 -0.01884 0.06512 -0.00314 0.09547 0.00935 0.00109 0.00044 0.00031 0.00715 0.00353 0.00271 0.00409 0.00258 0.00352 0.00256 0.00182 F2B_b 0.71661 -0.02604 0.48634 0.06353 0.09047 0.06289 0.13304 -0.01884 0.06512 -0.00314 0.09547 0.15149 0.01663 0.00698 0.00479 0.00715 0.00353 0.00271 0.00409 0.00258 0.00352 0.00256 0.00182 F3B_b 0.47821 -0.13280 0.55891 0.06353 0.09132 0.06989 0.08828 -0.03415 -0.02886 0.01651 0.08316 0.12059 0.01370 0.00631 0.00403 0.00715 0.00309 0.00257 0.00359 0.00251 0.00255 0.00220 0.00157 F1B_b 0.83097 -0.11138 0.58529 0.06353 0.10504 0.04933 0.06530 0.00581 0.00727 0.02272 0.07322 0.13026 0.01736 0.00614 0.00348 0.00715 0.00379 0.00227 0.00231 0.00195 0.00253 0.00244 0.00137 H1N 0.10337 0.32057 0.74022 1.00000 0.04197 0.07977 0.00887 0.00494 0.00239 0.00000 0.01301 Final Structure Factor Calculation for 2008lsh028 in P2(1)2(1)2(1) Total number of l.s. parameters = 143 Maximum vector length = 511 Memory required = 1792 / 26068 wR2 = 0.1700 before cycle 7 for 2032 data and 2 / 143 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 1. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.128; Restrained GooF = 1.128 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0198 * P )^2 + 1.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0823 for 1224 Fo > 4sig(Fo) and 0.1571 for all 2032 data wR2 = 0.1700, GooF = S = 1.128, Restrained GooF = 1.128 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0444 0.0380 0.0332 C1 0.0482 0.0422 0.0361 C2 0.0517 0.0433 0.0316 C3 0.0599 0.0462 0.0354 C4 0.0595 0.0505 0.0358 C5 0.0569 0.0447 0.0368 C6 0.0538 0.0430 0.0301 C7 0.0564 0.0498 0.0381 C8 0.0674 0.0507 0.0466 C9 0.0522 0.0428 0.0287 N1 0.0796 0.0501 0.0297 O1 0.1147 0.0641 0.0408 F1A_a 0.1379 0.0685 0.0431 F3A_a 0.1827 0.0639 0.0398 F2A_a 0.1827 0.0639 0.0398 F2B_b 0.1379 0.0685 0.0431 F3B_b 0.1147 0.0641 0.0408 F1B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.018 0.023 0.030 0.038 0.048 0.063 0.086 0.133 1.000 Number in group 214. 216. 195. 207. 210. 192. 187. 204. 210. 197. GooF 1.138 1.321 1.179 1.130 1.161 1.179 1.092 0.980 0.953 1.093 K 5.174 2.653 1.710 1.298 1.114 1.006 0.956 0.994 1.000 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 205. 205. 205. 197. 208. 205. 196. 208. 198. 205. GooF 1.171 1.297 1.312 1.247 1.080 1.103 0.982 0.914 0.914 1.166 K 1.521 1.535 1.351 1.260 1.016 1.018 0.986 0.999 0.995 1.003 R1 0.470 0.510 0.350 0.316 0.238 0.130 0.086 0.071 0.054 0.032 Recommended weighting scheme: WGHT 0.0192 1.3326 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 5 0 67.71 21.15 4.90 0.043 1.83 -2 1 21 44.68 1.66 4.12 0.012 0.80 -4 2 18 42.16 5.90 3.82 0.023 0.78 4 4 17 61.04 14.32 3.69 0.035 0.77 2 2 0 1225.59 1642.74 3.57 0.378 2.28 0 10 7 -6.43 25.61 3.40 0.047 0.91 6 4 7 26.29 1.87 3.38 0.013 0.77 -4 6 11 -0.53 34.81 3.25 0.055 0.86 -4 6 1 87.20 39.13 3.16 0.058 1.01 -5 1 9 39.13 0.68 3.10 0.008 0.91 -3 6 12 -5.93 13.36 3.09 0.034 0.92 0 0 6 256.53 333.76 3.05 0.171 2.97 -4 9 8 -8.25 20.42 3.05 0.042 0.78 -2 4 14 97.48 160.23 3.03 0.118 1.03 -5 6 2 38.30 3.07 2.97 0.016 0.87 6 2 7 25.26 1.44 2.97 0.011 0.81 1 8 0 178.58 122.00 2.96 0.103 1.19 3 2 17 27.58 5.92 2.93 0.023 0.88 -3 5 16 21.79 0.43 2.90 0.006 0.84 2 0 16 17.84 1.88 2.87 0.013 1.02 6 0 1 15.97 1.62 2.83 0.012 0.86 6 1 0 16.58 0.36 2.80 0.006 0.86 5 0 4 9.36 33.24 2.79 0.054 1.01 6 3 1 -3.29 15.66 2.79 0.037 0.83 -4 2 14 69.57 38.46 2.78 0.058 0.89 5 1 14 44.05 2.74 2.72 0.015 0.80 0 1 4 2739.98 3046.02 2.70 0.515 4.05 -2 7 11 13.92 1.40 2.69 0.011 0.98 -5 1 14 42.49 2.74 2.67 0.015 0.80 -2 6 3 25.85 8.57 2.66 0.027 1.34 -2 3 20 23.65 1.09 2.64 0.010 0.82 3 10 7 57.23 9.86 2.63 0.029 0.81 0 10 0 93.09 56.91 2.62 0.070 0.98 3 2 18 30.59 2.34 2.60 0.014 0.85 -4 1 8 7.48 44.38 2.60 0.062 1.11 3 4 15 24.12 5.33 2.56 0.022 0.91 2 10 5 30.82 1.39 2.53 0.011 0.88 4 8 7 59.74 9.44 2.53 0.029 0.84 -4 1 16 36.90 7.27 2.51 0.025 0.84 0 1 16 6.70 25.89 2.51 0.048 1.11 -4 5 14 30.54 3.04 2.51 0.016 0.82 6 1 2 37.89 17.09 2.51 0.039 0.85 -3 7 15 27.85 1.05 2.49 0.010 0.80 4 3 15 -6.15 14.56 2.46 0.036 0.84 -4 4 10 13.11 0.25 2.46 0.005 0.96 4 6 11 71.44 34.81 2.43 0.055 0.86 3 10 2 27.72 3.79 2.42 0.018 0.85 4 1 7 8.25 25.05 2.41 0.047 1.14 -2 4 18 25.56 5.90 2.40 0.023 0.86 3 8 14 40.05 7.21 2.37 0.025 0.78 Bond lengths and angles C1 - Distance Angles C2 1.3847 (0.0063) C6 1.3921 (0.0067) 119.50 (0.45) N1 1.4107 (0.0058) 123.57 (0.42) 116.90 (0.40) C1 - C2 C6 C2 - Distance Angles C1 1.3847 (0.0063) C3 1.3965 (0.0065) 118.72 (0.45) H2 0.9500 120.64 120.64 C2 - C1 C3 C3 - Distance Angles C4 1.3705 (0.0069) C2 1.3965 (0.0065) 121.62 (0.45) C9 1.4871 (0.0071) 121.19 (0.47) 117.18 (0.47) C3 - C4 C2 C4 - Distance Angles C3 1.3705 (0.0069) C5 1.3879 (0.0069) 119.16 (0.46) H4 0.9500 120.42 120.42 C4 - C3 C5 C5 - Distance Angles C6 1.3706 (0.0067) C4 1.3879 (0.0069) 120.01 (0.47) H5 0.9500 120.00 120.00 C5 - C6 C4 C6 - Distance Angles C5 1.3706 (0.0067) C1 1.3921 (0.0067) 120.94 (0.46) H6 0.9500 119.53 119.53 C6 - C5 C1 C7 - Distance Angles O1 1.2343 (0.0054) N1 1.3528 (0.0064) 123.75 (0.48) C8 1.5113 (0.0065) 121.15 (0.45) 115.06 (0.42) C7 - O1 N1 C8 - Distance Angles C7 1.5113 (0.0065) 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 C9 - Distance Angles F3B_b 1.1469 (0.0636) F2B_b 1.2347 (0.0732) 120.44 (4.85) F1B_b 1.2445 (0.0716) 104.79 (4.66) 110.48 (4.78) F3A_a 1.3309 (0.0069) 46.15 (3.78) 75.84 (4.18) 136.44 (3.15) F1A_a 1.3338 (0.0068) 62.90 (3.92) 140.52 (3.73) 42.94 (3.79) 104.40 (0.52) F2A_a 1.3379 (0.0071) 133.63 (2.99) 40.59 (4.24) 69.90 (3.48) 105.23 (0.51) 105.55 (0.52) C3 1.4871 (0.0071) 111.83 (2.99) 101.89 (3.31) 106.84 (2.78) 113.98 (0.49) 113.10 (0.44) 113.68 (0.51) C9 - F3B_b F2B_b F1B_b F3A_a F1A_a F2A_a N1 - Distance Angles C7 1.3528 (0.0065) C1 1.4107 (0.0058) 128.23 (0.42) H1N 0.9551 (0.0466) 112.09 (2.73) 119.67 (2.77) N1 - C7 C1 O1 - Distance Angles C7 1.2343 (0.0055) O1 - F1A_a - Distance Angles C9 1.3338 (0.0068) F1A_a - F3A_a - Distance Angles C9 1.3309 (0.0070) F3A_a - F2A_a - Distance Angles C9 1.3379 (0.0071) F2A_a - F2B_b - Distance Angles C9 1.2347 (0.0731) F2B_b - F3B_b - Distance Angles C9 1.1469 (0.0630) F3B_b - F1B_b - Distance Angles C9 1.2445 (0.0714) F1B_b - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.96(5) 1.97(5) 2.907(5) 166(4) 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)