+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 16:33:13 on 30-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh086 in P2(1)2(1)2 CELL 0.71073 9.5368 14.7516 4.5621 90.000 90.000 90.000 ZERR 2.00 0.0002 0.0004 0.0001 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O BR UNIT 26 20 4 2 4 V = 641.81 F(000) = 360.0 Mu = 6.30 mm-1 Cell Wt = 740.10 Rho = 1.915 MERG 2 OMIT -3.00 55.00 OMIT 1 2 0 EQIV $1 x, y, z+1 HTAB N1 O1_$1 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA SIZE 0.34 0.06 0.04 BOND $H L.S. 6 TEMP -153.00 WGHT 0.016300 0.261300 EXTI 0.012616 FVAR 0.82965 C1 1 0.635504 0.359966 0.326087 11.00000 0.01569 0.01200 = 0.01168 -0.00118 -0.00191 0.00210 C2 1 0.610204 0.271676 0.425411 11.00000 0.01546 0.01337 = 0.01499 -0.00108 -0.00291 0.00148 AFIX 43 H2 2 0.540510 0.260361 0.569627 11.00000 -1.20000 AFIX 0 C3 1 0.688459 0.201083 0.309955 11.00000 0.01815 0.01252 = 0.02011 -0.00203 -0.00476 0.00202 C4 1 0.791708 0.215595 0.098868 11.00000 0.01809 0.02081 = 0.01960 -0.00494 -0.00287 0.00751 AFIX 43 H4 2 0.844149 0.166442 0.020860 11.00000 -1.20000 AFIX 0 C5 1 0.815816 0.303711 0.005803 11.00000 0.01844 0.02732 = 0.01507 -0.00109 0.00187 0.00338 AFIX 43 H5 2 0.886201 0.314958 -0.136996 11.00000 -1.20000 AFIX 0 C6 1 0.738999 0.375784 0.117456 11.00000 0.01732 0.01638 = 0.01688 -0.00014 0.00037 0.00012 AFIX 43 H6 2 0.757059 0.435748 0.051562 11.00000 -1.20000 AFIX 0 C7 1 0.500000 0.500000 0.289991 10.50000 0.01380 0.01073 = 0.01278 0.00000 0.00000 -0.00158 N1 3 0.556211 0.431195 0.451210 11.00000 0.01981 0.01060 = 0.01073 -0.00008 -0.00026 0.00338 O1 4 0.500000 0.500000 0.018382 10.50000 0.03164 0.02099 = 0.00998 0.00000 0.00000 0.01077 BR1 5 0.650100 0.081592 0.440579 11.00000 0.03120 0.01093 = 0.04110 0.00096 -0.00145 0.00281 H1N 2 0.544941 0.433578 0.633021 11.00000 -1.20000 HKLF 4 1 0 1 0 0 0 -1 -1 0 0 Covalent radii and connectivity table for 2008lsh086 in P2(1)2(1)2 C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 C1 - C6 C2 N1 C2 - C3 C1 C3 - C2 C4 Br1 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 N1_$2 N1 - C7 C1 O1 - C7 Br1 - C3 Operators for generating equivalent atoms: $1 x, y, z+1 $2 -x+1, -y+1, z 12892 Reflections read, of which 81 rejected -10 =< h =< 12, -19 =< k =< 18, -5 =< l =< 5, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 1462 Unique reflections, of which 0 suppressed R(int) = 0.0342 R(sigma) = 0.0268 Friedel opposites not merged Maximum memory for data reduction = 1090 / 14460 Special position constraints for C7 x = 0.5000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1 x = 0.5000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1324 / 116933 wR2 = 0.0468 before cycle 1 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 0.003 OSF 2 0.01262 0.00125 0.000 EXTI Mean shift/esd = 0.003 Maximum = -0.029 for U22 Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1324 / 116933 wR2 = 0.0468 before cycle 2 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 -0.004 OSF 2 0.01262 0.00126 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.009 for U22 Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1324 / 116933 wR2 = 0.0468 before cycle 3 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 0.000 OSF 2 0.01262 0.00126 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1324 / 116933 wR2 = 0.0468 before cycle 4 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 0.000 OSF 2 0.01262 0.00126 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1324 / 116933 wR2 = 0.0468 before cycle 5 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 0.000 OSF 2 0.01262 0.00126 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1324 / 116933 wR2 = 0.0468 before cycle 6 for 1462 data and 87 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82965 0.00149 0.000 OSF 2 0.01262 0.00126 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Br1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C2 Largest correlation matrix elements 0.684 EXTI / OSF 0.632 U33 Br1 / OSF 0.659 U22 Br1 / OSF 0.624 U11 Br1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5405 0.2604 0.5696 43 0.950 0.000 C2 C3 C1 H4 0.8441 0.1664 0.0209 43 0.950 0.000 C4 C5 C3 H5 0.8862 0.3150 -0.1370 43 0.950 0.000 C5 C4 C6 H6 0.7571 0.4357 0.0516 43 0.950 0.000 C6 C5 C1 2008lsh086 in P2(1)2(1)2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.63550 0.35997 0.32609 1.00000 0.01569 0.01200 0.01168 -0.00118 -0.00191 0.00210 0.01313 0.00332 0.00021 0.00012 0.00044 0.00000 0.00091 0.00090 0.00087 0.00070 0.00081 0.00076 0.00037 C2 0.61020 0.27168 0.42541 1.00000 0.01546 0.01337 0.01499 -0.00108 -0.00291 0.00148 0.01461 0.00347 0.00019 0.00013 0.00050 0.00000 0.00088 0.00090 0.00091 0.00079 0.00077 0.00066 0.00038 H2 0.54051 0.26036 0.56963 1.00000 0.01753 0.00000 0.00000 C3 0.68846 0.20108 0.30996 1.00000 0.01815 0.01252 0.02011 -0.00203 -0.00476 0.00202 0.01692 0.00356 0.00021 0.00013 0.00051 0.00000 0.00100 0.00095 0.00104 0.00085 0.00081 0.00071 0.00043 C4 0.79171 0.21559 0.09887 1.00000 0.01809 0.02081 0.01960 -0.00494 -0.00287 0.00751 0.01950 0.00374 0.00022 0.00015 0.00050 0.00000 0.00094 0.00102 0.00115 0.00088 0.00085 0.00079 0.00045 H4 0.84415 0.16644 0.02086 1.00000 0.02340 0.00000 0.00000 C5 0.81582 0.30371 0.00580 1.00000 0.01844 0.02732 0.01507 -0.00109 0.00187 0.00338 0.02027 0.00379 0.00023 0.00015 0.00046 0.00000 0.00100 0.00117 0.00122 0.00083 0.00073 0.00082 0.00049 H5 0.88620 0.31496 -0.13700 1.00000 0.02433 0.00000 0.00000 C6 0.73900 0.37578 0.11746 1.00000 0.01732 0.01638 0.01688 -0.00014 0.00037 0.00012 0.01686 0.00355 0.00022 0.00015 0.00044 0.00000 0.00094 0.00096 0.00110 0.00078 0.00081 0.00077 0.00042 H6 0.75706 0.43575 0.05156 1.00000 0.02023 0.00000 0.00000 C7 0.50000 0.50000 0.28999 0.50000 0.01380 0.01073 0.01278 0.00000 0.00000 -0.00158 0.01244 0.00294 0.00000 0.00000 0.00064 0.00000 0.00120 0.00129 0.00144 0.00000 0.00000 0.00100 0.00054 N1 0.55621 0.43119 0.45121 1.00000 0.01981 0.01060 0.01073 -0.00008 -0.00026 0.00338 0.01372 0.00317 0.00019 0.00011 0.00041 0.00000 0.00078 0.00076 0.00073 0.00075 0.00070 0.00064 0.00032 O1 0.50000 0.50000 0.01838 0.50000 0.03164 0.02099 0.00998 0.00000 0.00000 0.01077 0.02087 0.00210 0.00000 0.00000 0.00046 0.00000 0.00116 0.00109 0.00115 0.00000 0.00000 0.00088 0.00049 Br1 0.65010 0.08159 0.44058 1.00000 0.03120 0.01093 0.04110 0.00096 -0.00145 0.00281 0.02774 0.00042 0.00002 0.00001 0.00006 0.00000 0.00014 0.00012 0.00016 0.00009 0.00011 0.00009 0.00010 H1N 0.54494 0.43357 0.63303 1.00000 0.03329 0.04646 0.00310 0.00192 0.00395 0.00000 0.00000 Final Structure Factor Calculation for 2008lsh086 in P2(1)2(1)2 Total number of l.s. parameters = 87 Maximum vector length = 511 Memory required = 1239 / 26068 wR2 = 0.0468 before cycle 7 for 1462 data and 2 / 87 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 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.107 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0163 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0198 for 1418 Fo > 4sig(Fo) and 0.0209 for all 1462 data wR2 = 0.0468, GooF = S = 1.106, Restrained GooF = 1.107 for all data Flack x parameter = 0.0079 with esd 0.0110 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0175 0.0112 0.0106 C1 0.0188 0.0128 0.0122 C2 0.0247 0.0143 0.0118 C3 0.0301 0.0167 0.0117 C4 0.0285 0.0186 0.0138 C5 0.0175 0.0168 0.0163 C6 0.0145 0.0128 0.0101 C7 0.0209 0.0107 0.0095 N1 0.0383 0.0143 0.0100 O1 0.0413 0.0314 0.0105 Br1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.050 0.079 0.102 0.123 0.147 0.174 0.207 0.261 0.336 1.000 Number in group 148. 148. 146. 143. 151. 143. 145. 147. 144. 147. GooF 1.170 1.345 1.146 1.036 1.022 0.849 1.010 1.132 1.125 1.149 K 0.939 0.951 0.954 0.978 0.989 0.994 1.007 1.013 1.014 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 149. 144. 147. 145. 148. 145. 145. 147. 146. 146. GooF 1.168 1.139 1.012 0.981 0.941 1.006 1.063 1.052 0.985 1.576 K 0.960 0.993 0.998 1.007 1.017 1.022 1.030 1.022 1.005 0.994 R1 0.055 0.038 0.028 0.023 0.021 0.018 0.019 0.015 0.012 0.016 Recommended weighting scheme: WGHT 0.0162 0.2631 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) 0 5 1 67.83 95.87 4.83 0.078 2.48 3 2 1 35.19 20.51 4.23 0.036 2.46 2 6 0 762.54 849.61 3.56 0.234 2.19 10 9 0 29.83 51.70 3.50 0.058 0.82 3 6 0 649.44 584.01 3.36 0.194 1.94 8 3 4 6.30 21.13 3.20 0.037 0.81 1 7 1 681.43 751.69 3.18 0.220 1.88 3 5 0 2384.98 2582.63 3.05 0.407 2.16 -3 4 2 261.29 297.42 3.03 0.138 1.66 -3 9 5 38.16 71.04 3.03 0.068 0.77 5 17 0 37.76 60.09 2.99 0.062 0.79 3 12 1 172.58 211.15 2.93 0.116 1.11 -4 4 4 768.55 677.78 2.87 0.209 0.99 0 4 5 5.11 14.37 2.83 0.030 0.89 -3 16 1 194.91 161.40 2.82 0.102 0.87 -3 15 3 103.98 146.60 2.80 0.097 0.80 6 1 0 1120.37 1032.55 2.75 0.258 1.58 8 7 3 65.92 83.81 2.75 0.073 0.86 0 3 1 24.71 34.44 2.73 0.047 3.34 -1 7 1 546.71 597.51 2.70 0.196 1.88 2 2 2 1344.89 1472.25 2.68 0.308 1.98 8 5 3 121.32 143.99 2.58 0.096 0.89 0 0 3 72.53 90.76 2.57 0.076 1.52 -5 6 5 10.06 26.83 2.51 0.042 0.78 1 2 1 6484.11 6887.61 2.49 0.665 3.59 4 2 3 1010.19 914.72 2.48 0.242 1.26 0 12 2 2265.20 2099.76 2.39 0.367 1.08 4 7 1 285.40 314.69 2.39 0.142 1.49 0 1 2 2076.67 2275.86 2.35 0.382 2.25 5 0 4 54.00 67.94 2.35 0.066 0.98 -6 1 3 1271.32 1175.86 2.32 0.275 1.10 5 5 0 5.15 0.18 2.31 0.003 1.60 -3 2 2 205.48 228.80 2.30 0.121 1.80 7 2 4 133.95 158.05 2.29 0.101 0.87 0 0 4 5.10 13.58 2.29 0.030 1.14 1 2 2 1256.33 1353.23 2.29 0.295 2.12 -1 12 1 308.12 368.07 2.28 0.154 1.18 9 13 0 205.20 254.64 2.25 0.128 0.77 3 4 2 321.56 351.94 2.25 0.150 1.66 -1 1 3 1902.44 1753.86 2.24 0.336 1.49 -4 2 4 542.18 486.05 2.24 0.177 1.02 -8 6 4 12.71 0.89 2.20 0.008 0.78 0 4 4 70.42 57.96 2.20 0.061 1.09 7 4 1 38.34 19.91 2.20 0.036 1.23 5 14 3 101.88 128.93 2.20 0.091 0.79 -2 2 2 1522.34 1631.02 2.17 0.324 1.98 -7 15 1 70.49 91.52 2.17 0.077 0.79 -11 5 1 83.12 64.82 2.17 0.065 0.82 -3 3 5 66.10 89.27 2.16 0.076 0.86 -10 10 1 118.60 145.40 2.16 0.097 0.79 Bond lengths and angles C1 - Distance Angles C6 1.3909 (0.0028) C2 1.3999 (0.0027) 119.99 (0.19) N1 1.4148 (0.0025) 122.06 (0.17) 117.92 (0.19) C1 - C6 C2 C2 - Distance Angles C3 1.3852 (0.0028) C1 1.3999 (0.0027) 118.91 (0.20) H2 0.9500 120.54 120.54 C2 - C3 C1 C3 - Distance Angles C2 1.3852 (0.0028) C4 1.3938 (0.0031) 121.86 (0.20) Br1 1.8963 (0.0021) 118.38 (0.16) 119.75 (0.16) C3 - C2 C4 C4 - Distance Angles C5 1.3866 (0.0032) C3 1.3938 (0.0031) 118.21 (0.19) H4 0.9500 120.90 120.90 C4 - C5 C3 C5 - Distance Angles C4 1.3866 (0.0032) C6 1.3880 (0.0030) 121.21 (0.19) H5 0.9500 119.40 119.40 C5 - C4 C6 C6 - Distance Angles C5 1.3880 (0.0030) C1 1.3909 (0.0028) 119.81 (0.20) H6 0.9500 120.09 120.09 C6 - C5 C1 C7 - Distance Angles O1 1.2391 (0.0038) N1 1.3633 (0.0023) 122.65 (0.13) N1_$2 1.3633 (0.0023) 122.65 (0.13) 114.70 (0.25) C7 - O1 N1 N1 - Distance Angles C7 1.3633 (0.0023) C1 1.4148 (0.0025) 123.05 (0.19) H1N 0.8371 (0.0174) 116.93 (1.99) 119.97 (2.00) N1 - C7 C1 O1 - Distance Angles C7 1.2391 (0.0038) O1 - Br1 - Distance Angles C3 1.8963 (0.0021) Br1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.837(17) 2.06(2) 2.831(3) 153(3) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 3 13 GRID -5.000 -2 -1 5.000 2 1 R1 = 0.0198 for 888 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.1472 0.4173 0.2970 [ 1.20 A from BR1 ] Deepest hole -0.43 at 0.6887 0.0872 0.2824 [ 0.81 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1609 / 18170 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6472 0.0827 0.7030 1.00000 0.05 0.38 1.20 BR1 2.53 C3 2.61 H6 2.67 H4 Q2 1 0.8451 0.2562 -0.4346 1.00000 0.05 0.34 1.66 H5 1.98 H2 2.06 C3 2.15 C5 Q3 1 0.5485 0.4190 0.5685 1.00000 0.05 0.29 0.37 H1N 0.57 N1 1.63 C1 1.80 C7 Q4 1 0.6248 0.0830 0.5626 1.00000 0.05 0.24 0.61 BR1 2.18 C3 2.74 H2 2.86 C2 Q5 1 0.8540 0.2574 0.3124 1.00000 0.05 0.23 1.30 C4 1.60 C5 1.78 C3 1.88 H2 Shortest distances between peaks (including symmetry equivalents) 1 4 0.67 2 5 1.16 3 3 2.56 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.75: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.38: Structure factors and derivatives 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 16:33:14 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++