+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 15:46:46 on 15-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh168 in P2(1)/c CELL 0.71073 19.8550 5.0020 18.3360 90.000 108.655 90.000 ZERR 8.00 0.0015 0.0005 0.0016 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR UNIT 64 64 8 8 8 V = 1725.36 F(000) = 848.0 Mu = 4.71 mm-1 Cell Wt = 1712.51 Rho = 1.648 MERG 2 OMIT -3.00 55.00 OMIT -12 0 22 OMIT -1 1 1 DFIX 0.88 N1 H1N N11 H11N FMAP 2 PLAN 5 ACTA BOND $H SIZE 0.44 0.08 0.06 EQIV $1 x, -y+5/2, z-1/2 HTAB N1 O11_$1 HTAB N11 O1 HTAB L.S. 6 TEMP -153.00 WGHT 0.105700 1.547000 FVAR 0.12079 MOLE 1 C1 1 0.338430 0.929170 0.192826 11.00000 0.03257 0.02939 = 0.02804 0.00062 0.00699 -0.00932 C2 1 0.365352 0.937482 0.273209 11.00000 0.03652 0.02931 = 0.03394 0.00197 0.01032 -0.00149 AFIX 43 H2 2 0.348742 1.066040 0.301574 11.00000 -1.20000 AFIX 0 C3 1 0.417008 0.752577 0.310316 11.00000 0.03738 0.04272 = 0.03099 0.00304 0.00387 -0.00625 C4 1 0.442373 0.561802 0.271858 11.00000 0.03155 0.03095 = 0.04798 0.00267 0.00809 0.00026 AFIX 43 H4 2 0.477062 0.435815 0.299254 11.00000 -1.20000 AFIX 0 C5 1 0.416221 0.557629 0.192410 11.00000 0.03563 0.03535 = 0.04448 -0.00344 0.01060 0.00135 AFIX 43 H5 2 0.433993 0.430508 0.164664 11.00000 -1.20000 AFIX 0 C6 1 0.363931 0.738584 0.152619 11.00000 0.03169 0.03576 = 0.03365 -0.00864 0.00847 -0.00519 AFIX 43 H6 2 0.345632 0.732097 0.098023 11.00000 -1.20000 AFIX 0 C7 1 0.249131 1.296324 0.172467 11.00000 0.03092 0.03187 = 0.02733 0.00301 0.00822 -0.00528 C8 1 0.191941 1.433596 0.107647 11.00000 0.03987 0.03829 = 0.03221 0.00686 0.00610 0.00325 AFIX 137 H8A 2 0.154685 1.501537 0.127179 11.00000 -1.50000 H8B 2 0.171266 1.305102 0.066164 11.00000 -1.50000 H8C 2 0.212996 1.582659 0.087803 11.00000 -1.50000 AFIX 0 N1 3 0.283417 1.096023 0.148847 11.00000 0.03620 0.03576 = 0.02283 -0.00121 0.00629 0.00183 O1 4 0.261920 1.361523 0.240310 11.00000 0.03633 0.03860 = 0.02917 -0.00541 0.01399 -0.00031 H1N 2 0.265781 1.063617 0.098662 11.00000 0.04485 MOLE 2 C11 1 0.166594 1.784897 0.342131 11.00000 0.03324 0.03809 = 0.02901 -0.00577 0.00694 -0.00573 C12 1 0.127378 1.873026 0.388597 11.00000 0.03194 0.04701 = 0.02603 0.00005 0.00826 -0.00119 AFIX 43 H12 2 0.133730 1.794574 0.437529 11.00000 -1.20000 AFIX 0 C13 1 0.079155 2.077250 0.361411 11.00000 0.03114 0.04671 = 0.03441 -0.00212 0.00954 -0.00154 C14 1 0.066986 2.196391 0.290519 11.00000 0.03318 0.04296 = 0.04066 0.00594 0.00895 -0.00129 AFIX 43 H14 2 0.033484 2.337209 0.273693 11.00000 -1.20000 AFIX 0 C15 1 0.105307 2.103173 0.245113 11.00000 0.04355 0.04774 = 0.03363 0.00587 0.00885 -0.00872 AFIX 43 H15 2 0.097244 2.178254 0.195454 11.00000 -1.20000 AFIX 0 C16 1 0.155536 1.901561 0.270388 11.00000 0.03961 0.04489 = 0.02769 0.00068 0.01118 -0.00828 AFIX 43 H16 2 0.182306 1.843446 0.238688 11.00000 -1.20000 AFIX 0 C17 1 0.248936 1.475609 0.434940 11.00000 0.03918 0.04290 = 0.02640 -0.00195 0.00674 -0.00645 C18 1 0.302095 1.257330 0.440990 11.00000 0.04653 0.04485 = 0.02862 -0.00112 0.00609 0.00669 AFIX 137 H18A 2 0.350038 1.325682 0.467057 11.00000 -1.50000 H18B 2 0.298953 1.195431 0.389295 11.00000 -1.50000 H18C 2 0.292074 1.108062 0.470576 11.00000 -1.50000 AFIX 0 N11 3 0.218151 1.580205 0.364056 11.00000 0.04038 0.03623 = 0.02781 -0.00159 0.01093 -0.00136 O11 4 0.234820 1.554743 0.492298 11.00000 0.05245 0.04895 = 0.02424 0.00194 0.01055 0.00759 BR1 5 0.454105 0.768416 0.419839 11.00000 0.04799 0.06557 = 0.03222 0.00998 0.00264 0.00624 BR11 5 0.025060 2.195335 0.424835 11.00000 0.04366 0.08612 = 0.04271 0.00371 0.01554 0.01820 H11N 2 0.233794 1.510977 0.328618 11.00000 0.05123 HKLF 4 Covalent radii and connectivity table for 2008lsh168 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 C1 - C6 C2 N1 C2 - C3 C1 C3 - C4 C2 Br1 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 C11 - C16 C12 N11 C12 - C13 C11 C13 - C14 C12 Br11 C14 - C15 C13 C15 - C14 C16 C16 - C15 C11 C17 - O11 N11 C18 C18 - C17 N11 - C17 C11 O11 - C17 Br1 - C3 Br11 - C13 Operators for generating equivalent atoms: $1 x, -y+5/2, z-1/2 20190 Reflections read, of which 1493 rejected -25 =< h =< 25, -6 =< k =< 6, -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) -3 4 16 0.15 0.34 3 1.76 1 Inconsistent equivalents 3912 Unique reflections, of which 0 suppressed R(int) = 0.0934 R(sigma) = 0.0775 Friedel opposites merged Maximum memory for data reduction = 2060 / 39419 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 = 2623 / 259978 wR2 = 0.1914 before cycle 1 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.007 OSF Mean shift/esd = 0.001 Maximum = -0.013 for U23 Br1 Max. shift = 0.000 A for H18A Max. dU = 0.000 for H11N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2623 / 259978 wR2 = 0.1914 before cycle 2 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for U13 Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2623 / 259978 wR2 = 0.1914 before cycle 3 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Br11 Max. shift = 0.000 A for H11N Max. dU = 0.000 for H11N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2623 / 259978 wR2 = 0.1914 before cycle 4 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Br11 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2623 / 259978 wR2 = 0.1914 before cycle 5 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Br11 Max. shift = 0.000 A for H11N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 2623 / 259978 wR2 = 0.1914 before cycle 6 for 3912 data and 209 / 209 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12079 0.00042 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Br11 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H11N Largest correlation matrix elements 0.730 z H11N / x H11N 0.505 U33 Br1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3487 1.0660 0.3016 43 0.950 0.000 C2 C3 C1 H4 0.4771 0.4358 0.2993 43 0.950 0.000 C4 C3 C5 H5 0.4340 0.4305 0.1647 43 0.950 0.000 C5 C4 C6 H6 0.3456 0.7321 0.0980 43 0.950 0.000 C6 C5 C1 H8A 0.1547 1.5015 0.1272 137 0.980 0.000 C8 C7 H8A H8B 0.1713 1.3051 0.0662 137 0.980 0.000 C8 C7 H8A H8C 0.2130 1.5827 0.0878 137 0.980 0.000 C8 C7 H8A H12 0.1337 1.7946 0.4375 43 0.950 0.000 C12 C13 C11 H14 0.0335 2.3372 0.2737 43 0.950 0.000 C14 C15 C13 H15 0.0972 2.1783 0.1955 43 0.950 0.000 C15 C14 C16 H16 0.1823 1.8434 0.2387 43 0.950 0.000 C16 C15 C11 H18A 0.3500 1.3257 0.4671 137 0.980 0.000 C18 C17 H18A H18B 0.2990 1.1954 0.3893 137 0.980 0.000 C18 C17 H18A H18C 0.2921 1.1081 0.4706 137 0.980 0.000 C18 C17 H18A 2008lsh168 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.33843 0.92917 0.19283 1.00000 0.03257 0.02939 0.02804 0.00062 0.00699 -0.00932 0.03064 0.00850 0.00024 0.00090 0.00026 0.00000 0.00231 0.00229 0.00233 0.00185 0.00189 0.00192 0.00100 C2 0.36535 0.93748 0.27321 1.00000 0.03652 0.02931 0.03394 0.00197 0.01032 -0.00149 0.03348 0.00928 0.00025 0.00093 0.00028 0.00000 0.00248 0.00235 0.00254 0.00193 0.00203 0.00199 0.00104 H2 0.34874 1.06604 0.30157 1.00000 0.04018 0.00000 0.00000 C3 0.41701 0.75258 0.31032 1.00000 0.03738 0.04272 0.03099 0.00304 0.00387 -0.00625 0.03871 0.01013 0.00029 0.00101 0.00031 0.00000 0.00269 0.00280 0.00268 0.00209 0.00212 0.00216 0.00119 C4 0.44237 0.56180 0.27186 1.00000 0.03155 0.03095 0.04798 0.00267 0.00809 0.00026 0.03793 0.00982 0.00026 0.00099 0.00031 0.00000 0.00240 0.00245 0.00306 0.00218 0.00219 0.00199 0.00114 H4 0.47706 0.43581 0.29925 1.00000 0.04552 0.00000 0.00000 C5 0.41622 0.55763 0.19241 1.00000 0.03563 0.03535 0.04448 -0.00344 0.01060 0.00135 0.03901 0.00998 0.00026 0.00104 0.00031 0.00000 0.00255 0.00261 0.00298 0.00219 0.00223 0.00209 0.00115 H5 0.43399 0.43051 0.16466 1.00000 0.04681 0.00000 0.00000 C6 0.36393 0.73858 0.15262 1.00000 0.03169 0.03576 0.03365 -0.00864 0.00847 -0.00519 0.03417 0.00945 0.00026 0.00093 0.00031 0.00000 0.00245 0.00251 0.00270 0.00199 0.00205 0.00195 0.00109 H6 0.34563 0.73210 0.09802 1.00000 0.04101 0.00000 0.00000 C7 0.24913 1.29632 0.17247 1.00000 0.03092 0.03187 0.02733 0.00301 0.00822 -0.00528 0.03030 0.00908 0.00025 0.00091 0.00027 0.00000 0.00235 0.00238 0.00251 0.00188 0.00191 0.00187 0.00102 C8 0.19194 1.43360 0.10765 1.00000 0.03987 0.03829 0.03221 0.00686 0.00610 0.00325 0.03808 0.01005 0.00027 0.00102 0.00028 0.00000 0.00263 0.00262 0.00258 0.00209 0.00211 0.00221 0.00113 H8A 0.15469 1.50154 0.12718 1.00000 0.05712 0.00000 0.00000 H8B 0.17127 1.30510 0.06616 1.00000 0.05712 0.00000 0.00000 H8C 0.21300 1.58266 0.08780 1.00000 0.05712 0.00000 0.00000 N1 0.28342 1.09602 0.14885 1.00000 0.03620 0.03576 0.02283 -0.00121 0.00629 0.00183 0.03234 0.00774 0.00021 0.00082 0.00022 0.00000 0.00210 0.00214 0.00201 0.00165 0.00167 0.00170 0.00088 O1 0.26192 1.36152 0.24031 1.00000 0.03633 0.03860 0.02917 -0.00541 0.01399 -0.00031 0.03387 0.00649 0.00018 0.00069 0.00019 0.00000 0.00175 0.00176 0.00178 0.00146 0.00140 0.00150 0.00074 H1N 0.26578 1.06362 0.09866 1.00000 0.04485 0.07253 0.00274 0.01125 0.00130 0.00000 0.01541 C11 0.16659 1.78490 0.34213 1.00000 0.03324 0.03809 0.02901 -0.00577 0.00694 -0.00573 0.03416 0.00929 0.00026 0.00097 0.00029 0.00000 0.00249 0.00259 0.00252 0.00198 0.00204 0.00199 0.00109 C12 0.12738 1.87303 0.38860 1.00000 0.03194 0.04702 0.02603 0.00005 0.00826 -0.00119 0.03524 0.00960 0.00025 0.00107 0.00028 0.00000 0.00238 0.00280 0.00235 0.00215 0.00190 0.00215 0.00107 H12 0.13373 1.79457 0.43753 1.00000 0.04228 0.00000 0.00000 C13 0.07916 2.07725 0.36141 1.00000 0.03114 0.04671 0.03441 -0.00212 0.00954 -0.00154 0.03765 0.00970 0.00025 0.00109 0.00029 0.00000 0.00244 0.00292 0.00267 0.00225 0.00204 0.00217 0.00113 C14 0.06699 2.19639 0.29052 1.00000 0.03318 0.04296 0.04066 0.00594 0.00895 -0.00129 0.03961 0.01065 0.00028 0.00107 0.00032 0.00000 0.00254 0.00285 0.00299 0.00228 0.00222 0.00213 0.00120 H14 0.03348 2.33721 0.27369 1.00000 0.04754 0.00000 0.00000 C15 0.10531 2.10317 0.24511 1.00000 0.04355 0.04774 0.03363 0.00587 0.00885 -0.00872 0.04247 0.01029 0.00028 0.00112 0.00031 0.00000 0.00291 0.00309 0.00273 0.00233 0.00227 0.00245 0.00126 H15 0.09724 2.17825 0.19545 1.00000 0.05096 0.00000 0.00000 C16 0.15554 1.90156 0.27039 1.00000 0.03961 0.04489 0.02769 0.00068 0.01118 -0.00828 0.03730 0.00950 0.00026 0.00107 0.00028 0.00000 0.00265 0.00282 0.00247 0.00212 0.00207 0.00223 0.00112 H16 0.18231 1.84345 0.23869 1.00000 0.04476 0.00000 0.00000 C17 0.24894 1.47561 0.43494 1.00000 0.03918 0.04290 0.02640 -0.00195 0.00674 -0.00645 0.03705 0.00924 0.00026 0.00102 0.00027 0.00000 0.00262 0.00279 0.00248 0.00216 0.00205 0.00223 0.00113 C18 0.30209 1.25733 0.44099 1.00000 0.04653 0.04485 0.02862 -0.00112 0.00609 0.00669 0.04141 0.01097 0.00031 0.00105 0.00031 0.00000 0.00305 0.00294 0.00271 0.00207 0.00231 0.00229 0.00126 H18A 0.35004 1.32568 0.46706 1.00000 0.06211 0.00000 0.00000 H18B 0.29895 1.19543 0.38930 1.00000 0.06211 0.00000 0.00000 H18C 0.29207 1.10806 0.47058 1.00000 0.06211 0.00000 0.00000 N11 0.21815 1.58020 0.36406 1.00000 0.04038 0.03622 0.02781 -0.00159 0.01093 -0.00136 0.03480 0.00790 0.00022 0.00084 0.00023 0.00000 0.00226 0.00223 0.00220 0.00177 0.00181 0.00179 0.00093 O11 0.23482 1.55474 0.49230 1.00000 0.05245 0.04895 0.02424 0.00194 0.01055 0.00759 0.04229 0.00719 0.00020 0.00077 0.00019 0.00000 0.00208 0.00218 0.00178 0.00152 0.00155 0.00177 0.00087 Br1 0.45410 0.76842 0.41984 1.00000 0.04799 0.06557 0.03222 0.00998 0.00264 0.00624 0.05102 0.00119 0.00003 0.00013 0.00003 0.00000 0.00038 0.00043 0.00036 0.00024 0.00026 0.00026 0.00024 Br11 0.02506 2.19534 0.42483 1.00000 0.04366 0.08612 0.04271 0.00371 0.01554 0.01820 0.05708 0.00139 0.00003 0.00016 0.00004 0.00000 0.00036 0.00051 0.00039 0.00029 0.00027 0.00029 0.00026 H11N 0.23379 1.51098 0.32862 1.00000 0.05123 0.11025 0.00299 0.01134 0.00254 0.00000 0.01740 Final Structure Factor Calculation for 2008lsh168 in P2(1)/c Total number of l.s. parameters = 209 Maximum vector length = 511 Memory required = 2414 / 24017 wR2 = 0.1914 before cycle 7 for 3912 data and 0 / 209 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.025 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1057 * P )^2 + 1.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0648 for 2647 Fo > 4sig(Fo) and 0.0987 for all 3912 data wR2 = 0.1914, GooF = S = 1.025, Restrained GooF = 1.025 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0426 0.0279 0.0215 C1 0.0381 0.0342 0.0282 C2 0.0523 0.0357 0.0281 C3 0.0519 0.0316 0.0303 C4 0.0476 0.0360 0.0335 C5 0.0434 0.0345 0.0246 C6 0.0389 0.0278 0.0241 C7 0.0456 0.0420 0.0266 C8 0.0399 0.0344 0.0227 N1 0.0411 0.0364 0.0241 O1 0.0421 0.0357 0.0247 C11 0.0471 0.0325 0.0260 C12 0.0471 0.0349 0.0309 C13 0.0498 0.0362 0.0329 C14 0.0594 0.0370 0.0311 C15 0.0515 0.0336 0.0267 C16 0.0486 0.0369 0.0257 C17 0.0562 0.0399 0.0282 C18 0.0410 0.0362 0.0272 N11 0.0594 0.0436 0.0239 O11 0.0684 0.0578 0.0268 Br1 0.0929 0.0424 0.0359 Br11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.018 0.027 0.038 0.050 0.065 0.085 0.119 0.190 1.000 Number in group 434. 364. 375. 423. 372. 389. 392. 387. 382. 394. GooF 0.963 0.952 0.985 1.026 1.064 1.116 1.116 1.033 0.981 1.006 K 3.588 1.582 1.106 1.003 0.989 1.022 0.999 1.017 1.035 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.64 inf Number in group 404. 382. 395. 385. 397. 385. 393. 386. 398. 387. GooF 1.036 1.123 1.106 1.097 1.018 0.938 0.967 0.906 0.944 1.093 K 1.199 1.121 1.050 1.046 1.024 1.025 1.017 1.012 1.028 0.979 R1 0.312 0.275 0.202 0.147 0.113 0.082 0.070 0.056 0.053 0.046 Recommended weighting scheme: WGHT 0.1055 1.5468 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 1 1 1337.13 3347.37 6.53 0.220 3.99 -7 2 20 -21.93 150.08 5.72 0.047 0.86 4 1 7 656.50 1587.24 4.83 0.151 1.82 -9 3 5 1130.88 2126.49 4.55 0.175 1.31 -1 4 17 82.24 274.17 4.52 0.063 0.80 6 5 3 164.83 28.70 4.50 0.020 0.93 4 0 6 3898.77 7425.77 3.91 0.327 2.17 -8 4 15 1845.02 1078.15 3.91 0.125 0.87 6 1 4 5670.82 9146.24 3.89 0.363 2.03 -12 0 10 3127.97 6052.78 3.86 0.295 1.41 -7 3 15 146.50 380.78 3.80 0.074 0.98 -5 4 14 152.97 418.23 3.76 0.078 0.90 14 4 6 305.36 60.34 3.67 0.029 0.82 5 0 8 8986.06 14535.11 3.63 0.458 1.66 -5 3 18 304.98 594.50 3.61 0.093 0.87 4 0 10 143.38 365.14 3.56 0.073 1.48 7 0 8 10614.13 16455.79 3.45 0.487 1.47 13 4 6 439.98 189.17 3.36 0.052 0.85 5 4 11 318.14 706.07 3.23 0.101 0.91 -2 3 19 82.93 220.97 3.15 0.056 0.82 6 1 6 16976.59 25041.30 3.13 0.601 1.74 -16 1 18 57.35 181.83 3.12 0.051 0.89 4 1 5 1472.67 2200.49 3.10 0.178 2.20 -22 3 10 -92.52 155.93 3.07 0.047 0.78 4 5 12 438.21 198.49 2.98 0.053 0.79 4 2 14 -6.37 53.07 2.94 0.028 1.02 2 2 16 69.96 168.27 2.90 0.049 0.96 12 4 1 187.93 332.35 2.86 0.069 0.97 -13 1 18 914.70 1514.37 2.84 0.148 0.94 14 2 11 -18.56 76.00 2.84 0.033 0.84 -6 5 8 92.74 22.58 2.83 0.018 0.91 5 2 8 4855.80 7988.75 2.83 0.339 1.39 -20 4 8 350.90 0.43 2.82 0.002 0.77 -3 3 18 220.00 388.55 2.81 0.075 0.86 -10 3 15 199.51 73.51 2.80 0.033 0.96 -22 2 2 138.38 22.35 2.80 0.018 0.83 -8 0 6 691.19 450.31 2.79 0.081 2.20 -6 4 2 230.87 361.83 2.77 0.072 1.17 19 2 6 1257.61 831.82 2.76 0.109 0.81 -4 4 14 130.63 241.43 2.76 0.059 0.90 5 0 6 204.21 318.18 2.75 0.068 2.01 14 1 9 58.59 6.39 2.75 0.010 0.95 17 3 8 359.94 195.20 2.71 0.053 0.78 -2 3 18 -108.29 124.87 2.69 0.042 0.85 -1 4 8 131.17 219.48 2.68 0.056 1.09 -3 2 16 476.14 695.49 2.65 0.100 1.03 9 4 9 73.31 3.65 2.63 0.007 0.88 -10 1 23 18.39 132.83 2.62 0.044 0.78 5 4 14 -32.90 129.82 2.60 0.043 0.82 -20 1 1 19.13 89.06 2.57 0.036 0.94 Bond lengths and angles C1 - Distance Angles C6 1.3955 (0.0069) C2 1.3985 (0.0066) 119.74 (0.45) N1 1.4058 (0.0060) 116.69 (0.42) 123.49 (0.44) C1 - C6 C2 C2 - Distance Angles C3 1.3870 (0.0070) C1 1.3985 (0.0066) 118.07 (0.47) H2 0.9500 120.96 120.96 C2 - C3 C1 C3 - Distance Angles C4 1.3743 (0.0076) C2 1.3870 (0.0070) 123.10 (0.49) Br1 1.9067 (0.0054) 119.19 (0.39) 117.70 (0.40) C3 - C4 C2 C4 - Distance Angles C3 1.3743 (0.0076) C5 1.3814 (0.0075) 118.41 (0.47) H4 0.9500 120.80 120.80 C4 - C3 C5 C5 - Distance Angles C4 1.3814 (0.0075) C6 1.3946 (0.0071) 120.51 (0.49) H5 0.9500 119.74 119.74 C5 - C4 C6 C6 - Distance Angles C5 1.3946 (0.0071) C1 1.3955 (0.0069) 120.14 (0.49) H6 0.9500 119.93 119.93 C6 - C5 C1 C7 - Distance Angles O1 1.2314 (0.0057) N1 1.3577 (0.0064) 123.73 (0.43) C8 1.5199 (0.0064) 122.10 (0.44) 114.16 (0.41) C7 - O1 N1 C8 - Distance Angles C7 1.5199 (0.0064) 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 1.3577 (0.0064) C1 1.4058 (0.0060) 129.19 (0.40) H1N 0.8886 (0.0195) 113.16 (3.70) 117.53 (3.72) N1 - C7 C1 O1 - Distance Angles C7 1.2314 (0.0057) O1 - C11 - Distance Angles C16 1.3908 (0.0071) C12 1.3968 (0.0071) 119.63 (0.48) N11 1.4123 (0.0066) 117.01 (0.47) 123.36 (0.47) C11 - C16 C12 C12 - Distance Angles C13 1.3796 (0.0073) C11 1.3968 (0.0071) 118.11 (0.48) H12 0.9500 120.95 120.95 C12 - C13 C11 C13 - Distance Angles C14 1.3792 (0.0076) C12 1.3796 (0.0073) 123.54 (0.50) Br11 1.9115 (0.0051) 118.47 (0.40) 117.97 (0.39) C13 - C14 C12 C14 - Distance Angles C15 1.3765 (0.0078) C13 1.3792 (0.0076) 117.36 (0.51) H14 0.9500 121.32 121.32 C14 - C15 C13 C15 - Distance Angles C14 1.3765 (0.0078) C16 1.3895 (0.0077) 121.38 (0.50) H15 0.9500 119.31 119.31 C15 - C14 C16 C16 - Distance Angles C15 1.3895 (0.0077) C11 1.3908 (0.0071) 119.95 (0.50) H16 0.9500 120.02 120.02 C16 - C15 C11 C17 - Distance Angles O11 1.2369 (0.0058) N11 1.3522 (0.0061) 122.53 (0.48) C18 1.4978 (0.0074) 121.08 (0.45) 116.38 (0.44) C17 - O11 N11 C18 - Distance Angles C17 1.4978 (0.0073) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N11 - Distance Angles C17 1.3522 (0.0061) C11 1.4123 (0.0066) 128.15 (0.44) H11N 0.8762 (0.0196) 113.67 (3.99) 118.17 (3.98) N11 - C17 C11 O11 - Distance Angles C17 1.2369 (0.0058) O11 - Br1 - Distance Angles C3 1.9067 (0.0054) Br1 - Br11 - Distance Angles C13 1.9115 (0.0051) Br11 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.89(2) 1.94(2) 2.823(5) 172(5) N1-H1N...O11_$1 0.88(2) 2.02(2) 2.892(5) 175(6) N11-H11N...O1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)