+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1000p2n started at 10:54:57 on 13-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1000p2n in P2/n CELL 0.71073 12.4636 7.3364 15.1611 90.000 91.529 90.000 ZERR 2.00 0.0008 0.0008 0.0016 0.000 0.006 0.000 LATT 1 SYMM 1/2 - X, Y, 1/2 - Z SFAC C H B N F CL UNIT 54 72 2 4 4 2 V = 1385.81 F(000) = 504.0 Mu = 0.17 mm-1 Cell Wt = 945.68 Rho = 1.133 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 SIMU FMAP 2 PLAN 10 SIZE 0.01 0.05 0.08 ACTA BOND $H WGHT 0.00000 5.54660 L.S. 8 TEMP -153.00 FVAR 0.67702 MOLE 1 C1 1 0.372411 0.217096 0.382267 11.00000 0.05411 0.03639 = 0.02038 -0.00251 -0.00785 0.01137 C2 1 0.326513 0.232423 0.463683 11.00000 0.04779 0.06001 = 0.02891 -0.00112 -0.00408 0.01526 C3 1 0.397600 0.263021 0.536001 11.00000 0.05737 0.07156 = 0.02952 0.00474 -0.00572 0.00274 AFIX 43 H3 2 0.370165 0.275919 0.593529 11.00000 -1.20000 AFIX 0 C4 1 0.506252 0.274348 0.523986 11.00000 0.05807 0.05698 = 0.03662 0.00382 -0.01657 0.00241 AFIX 43 H4 2 0.553406 0.292404 0.573481 11.00000 -1.20000 AFIX 0 C5 1 0.547257 0.259882 0.441423 11.00000 0.04272 0.05893 = 0.04992 0.00834 -0.00560 -0.00099 AFIX 43 H5 2 0.622554 0.269561 0.434387 11.00000 -1.20000 AFIX 0 C6 1 0.481123 0.231462 0.368144 11.00000 0.04985 0.04022 = 0.03294 0.00957 -0.00034 0.00264 C7 1 0.526326 0.216778 0.275451 11.00000 0.06753 0.08979 = 0.04513 0.01159 0.01010 -0.01449 AFIX 13 H7 2 0.464139 0.218040 0.232391 11.00000 -1.20000 AFIX 0 C8 1 0.585088 0.035088 0.264338 11.00000 0.11897 0.11924 = 0.06873 -0.00640 0.03918 0.03585 AFIX 137 H8A 2 0.644696 0.027256 0.307650 11.00000 -1.50000 H8B 2 0.613070 0.027580 0.204650 11.00000 -1.50000 H8C 2 0.535080 -0.065769 0.273606 11.00000 -1.50000 AFIX 0 C9 1 0.597268 0.381867 0.254921 11.00000 0.11106 0.14270 = 0.08607 0.04191 0.02940 -0.05180 AFIX 137 H9A 2 0.556742 0.494399 0.264222 11.00000 -1.50000 H9B 2 0.619185 0.375757 0.193393 11.00000 -1.50000 H9C 2 0.661132 0.380754 0.294051 11.00000 -1.50000 AFIX 0 C10 1 0.206146 0.215652 0.478489 11.00000 0.04367 0.11106 = 0.04398 -0.01078 -0.00206 0.01088 AFIX 13 H10 2 0.168417 0.234540 0.420166 11.00000 -1.20000 AFIX 0 C11 1 0.163157 0.353525 0.541088 11.00000 0.07914 0.22431 = 0.11304 -0.09528 -0.00369 0.05598 AFIX 137 H11A 2 0.202373 0.344684 0.597817 11.00000 -1.50000 H11B 2 0.086757 0.330165 0.549834 11.00000 -1.50000 H11C 2 0.172180 0.476044 0.516620 11.00000 -1.50000 AFIX 0 C12 1 0.179689 0.018177 0.509839 11.00000 0.04571 0.15974 = 0.08597 0.02177 0.00355 -0.01627 AFIX 137 H12A 2 0.218562 -0.006990 0.565549 11.00000 -1.50000 H12B 2 0.201578 -0.069583 0.465028 11.00000 -1.50000 H12C 2 0.102334 0.007260 0.518598 11.00000 -1.50000 AFIX 0 C14 1 0.250000 0.280569 0.250000 10.50000 0.05413 0.03299 = 0.02435 0.00000 -0.00855 0.00000 C15 1 0.283034 -0.011794 0.285839 11.00000 0.08821 0.02256 = 0.03659 0.00630 -0.00903 0.00133 AFIX 43 H15 2 0.311541 -0.115717 0.315596 11.00000 -1.20000 AFIX 0 N13 4 0.301229 0.166820 0.307588 11.00000 0.05985 0.03545 = 0.03136 -0.00055 -0.00997 0.00754 PART -1 B1 3 0.233748 0.500229 0.258570 10.50000 0.02836 F1 5 0.216864 0.566325 0.170567 10.50000 0.17154 0.04128 = 0.08674 -0.00663 -0.08301 -0.00921 F2 5 0.337926 0.570821 0.283102 10.50000 0.09211 0.02389 = 0.09674 -0.00501 -0.04227 -0.00516 CL1 6 0.139459 0.575448 0.329717 10.50000 0.19902 0.05248 = 0.24416 -0.00293 0.09674 0.00899 HKLF 4 Covalent radii and connectivity table for 2008src1000p2n in P2/n C 0.770 H 0.320 B 0.820 N 0.700 F 0.640 CL 0.990 C1 - C2 C6 N13 C2 - C1 C3 C10 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 C7 C7 - C6 C8 C9 C8 - C7 C9 - C7 C10 - C11 C2 C12 C11 - C10 C12 - C10 C14 - N13_$1 N13 B1_$1 B1 C15 - C15_$1 N13 N13 - C14 C15 C1 B1 - F1 F2 C14 Cl1 F1 - B1 F2 - B1 Cl1 - B1 Operators for generating equivalent atoms: $1 -x+1/2, y, -z+1/2 12925 Reflections read, of which 686 rejected -15 =< h =< 15, -9 =< k =< 9, -19 =< l =< 19, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -12 3 2 2.41 1.09 4 8.09 11 4 2 -6.21 2.29 2 16.26 9 0 5 8.44 0.65 5 5.63 3 Inconsistent equivalents 3138 Unique reflections, of which 0 suppressed R(int) = 0.1728 R(sigma) = 0.1928 Friedel opposites merged Maximum memory for data reduction = 2104 / 31074 Special position constraints for C14 x = 0.2500 z = 0.2500 U23 = 0 U12 = 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 = 2601 / 210075 wR2 = 0.3107 before cycle 1 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.001 Maximum = -0.003 for U23 Cl1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for F1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 2 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U12 F1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for F1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 3 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U12 F1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for F1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 4 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U12 F1 Max. shift = 0.000 A for F1 Max. dU = 0.000 for F2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 5 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 Cl1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for F1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 6 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U33 Cl1 Max. shift = 0.000 A for F1 Max. dU = 0.000 for F2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 7 for 3138 data and 167 / 167 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. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for F2 Max. dU = 0.000 for Cl1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2601 / 210075 wR2 = 0.3107 before cycle 8 for 3138 data and 167 / 167 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67702 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C5 Max. shift = 0.000 A for H9B Max. dU = 0.000 for F1 Largest correlation matrix elements -0.744 U12 F1 / U23 F1 0.679 U23 F2 / U12 F1 0.607 U23 F1 / y F1 0.729 y F2 / U12 F1 0.636 U12 F2 / y F1 -0.600 U12 F2 / U23 F2 -0.728 y F2 / U23 F1 0.631 z F2 / x F1 -0.581 U23 F2 / U23 F1 -0.726 y F2 / y F1 0.626 U33 F2 / z F1 0.561 U12 F2 / U23 F1 -0.708 x F2 / U11 F1 -0.625 U12 F1 / y F1 0.542 U11 F2 / U11 F1 -0.706 U23 F2 / y F1 0.624 U23 F2 / y F2 -0.530 U12 F2 / y F2 0.687 U33 F2 / U33 F1 0.615 x F2 / z F1 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.3702 0.2759 0.5935 43 0.950 0.000 C3 C4 C2 H4 0.5534 0.2924 0.5735 43 0.950 0.000 C4 C5 C3 H5 0.6226 0.2696 0.4344 43 0.950 0.000 C5 C4 C6 H7 0.4641 0.2180 0.2324 13 1.000 0.000 C7 C6 C8 C9 H8A 0.6447 0.0273 0.3077 137 0.980 0.000 C8 C7 H8A H8B 0.6131 0.0276 0.2047 137 0.980 0.000 C8 C7 H8A H8C 0.5351 -0.0658 0.2736 137 0.980 0.000 C8 C7 H8A H9A 0.5567 0.4944 0.2642 137 0.980 0.000 C9 C7 H9A H9B 0.6192 0.3758 0.1934 137 0.980 0.000 C9 C7 H9A H9C 0.6611 0.3808 0.2941 137 0.980 0.000 C9 C7 H9A H10 0.1684 0.2345 0.4202 13 1.000 0.000 C10 C11 C2 C12 H11A 0.2024 0.3447 0.5978 137 0.980 0.000 C11 C10 H11A H11B 0.0868 0.3302 0.5498 137 0.980 0.000 C11 C10 H11A H11C 0.1722 0.4760 0.5166 137 0.980 0.000 C11 C10 H11A H12A 0.2186 -0.0070 0.5655 137 0.980 0.000 C12 C10 H12A H12B 0.2016 -0.0696 0.4650 137 0.980 0.000 C12 C10 H12A H12C 0.1023 0.0073 0.5186 137 0.980 0.000 C12 C10 H12A H15 0.3115 -0.1157 0.3156 43 0.950 0.000 C15 C15_$1 N13 2008src1000p2n in P2/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37241 0.21710 0.38227 1.00000 0.05411 0.03639 0.02038 -0.00251 -0.00785 0.01136 0.03712 0.00987 0.00049 0.00081 0.00035 0.00000 0.00391 0.00354 0.00297 0.00276 0.00258 0.00310 0.00147 C2 0.32651 0.23242 0.46368 1.00000 0.04779 0.06001 0.02891 -0.00112 -0.00408 0.01526 0.04566 0.01087 0.00046 0.00094 0.00037 0.00000 0.00379 0.00457 0.00336 0.00331 0.00284 0.00340 0.00170 C3 0.39760 0.26302 0.53600 1.00000 0.05737 0.07155 0.02951 0.00474 -0.00571 0.00275 0.05294 0.01129 0.00052 0.00098 0.00040 0.00000 0.00439 0.00519 0.00343 0.00360 0.00302 0.00389 0.00187 H3 0.37017 0.27592 0.59353 1.00000 0.06352 0.00000 0.00000 C4 0.50625 0.27435 0.52399 1.00000 0.05806 0.05698 0.03662 0.00381 -0.01658 0.00241 0.05087 0.01103 0.00053 0.00093 0.00040 0.00000 0.00441 0.00454 0.00387 0.00344 0.00322 0.00362 0.00180 H4 0.55341 0.29240 0.57348 1.00000 0.06105 0.00000 0.00000 C5 0.54726 0.25988 0.44142 1.00000 0.04273 0.05892 0.04992 0.00834 -0.00559 -0.00098 0.05064 0.01138 0.00051 0.00095 0.00042 0.00000 0.00363 0.00480 0.00418 0.00378 0.00310 0.00345 0.00179 H5 0.62255 0.26956 0.43439 1.00000 0.06077 0.00000 0.00000 C6 0.48112 0.23146 0.36814 1.00000 0.04985 0.04023 0.03293 0.00957 -0.00034 0.00263 0.04103 0.01062 0.00048 0.00085 0.00037 0.00000 0.00391 0.00387 0.00349 0.00307 0.00288 0.00316 0.00155 C7 0.52632 0.21678 0.27545 1.00000 0.06753 0.08979 0.04513 0.01160 0.01010 -0.01448 0.06733 0.01340 0.00059 0.00116 0.00046 0.00000 0.00487 0.00633 0.00433 0.00448 0.00356 0.00469 0.00225 H7 0.46414 0.21804 0.23239 1.00000 0.08080 0.00000 0.00000 C8 0.58509 0.03509 0.26434 1.00000 0.11897 0.11924 0.06874 -0.00640 0.03918 0.03585 0.10166 0.01783 0.00074 0.00138 0.00057 0.00000 0.00781 0.00879 0.00592 0.00602 0.00535 0.00669 0.00334 H8A 0.64469 0.02726 0.30765 1.00000 0.15249 0.00000 0.00000 H8B 0.61307 0.02758 0.20465 1.00000 0.15249 0.00000 0.00000 H8C 0.53508 -0.06577 0.27360 1.00000 0.15249 0.00000 0.00000 C9 0.59727 0.38187 0.25492 1.00000 0.11105 0.14271 0.08607 0.04191 0.02940 -0.05180 0.11280 0.01678 0.00073 0.00143 0.00060 0.00000 0.00761 0.00982 0.00697 0.00683 0.00575 0.00704 0.00382 H9A 0.55674 0.49440 0.26422 1.00000 0.16920 0.00000 0.00000 H9B 0.61918 0.37576 0.19339 1.00000 0.16920 0.00000 0.00000 H9C 0.66113 0.38075 0.29405 1.00000 0.16920 0.00000 0.00000 C10 0.20615 0.21565 0.47849 1.00000 0.04367 0.11106 0.04398 -0.01078 -0.00206 0.01087 0.06630 0.01300 0.00052 0.00125 0.00046 0.00000 0.00416 0.00703 0.00427 0.00471 0.00321 0.00444 0.00230 H10 0.16842 0.23454 0.42017 1.00000 0.07956 0.00000 0.00000 C11 0.16316 0.35353 0.54109 1.00000 0.07914 0.22433 0.11305 -0.09530 -0.00369 0.05598 0.13895 0.01727 0.00071 0.00171 0.00065 0.00000 0.00663 0.01387 0.00831 0.00883 0.00575 0.00754 0.00511 H11A 0.20237 0.34468 0.59782 1.00000 0.20843 0.00000 0.00000 H11B 0.08676 0.33017 0.54983 1.00000 0.20843 0.00000 0.00000 H11C 0.17218 0.47605 0.51662 1.00000 0.20843 0.00000 0.00000 C12 0.17969 0.01818 0.50984 1.00000 0.04571 0.15975 0.08597 0.02176 0.00355 -0.01627 0.09711 0.01576 0.00058 0.00150 0.00056 0.00000 0.00496 0.01037 0.00666 0.00683 0.00426 0.00560 0.00337 H12A 0.21856 -0.00699 0.56555 1.00000 0.14567 0.00000 0.00000 H12B 0.20158 -0.06958 0.46503 1.00000 0.14567 0.00000 0.00000 H12C 0.10233 0.00726 0.51860 1.00000 0.14567 0.00000 0.00000 C14 0.25000 0.28057 0.25000 0.50000 0.05414 0.03298 0.02435 0.00000 -0.00855 0.00000 0.03733 0.00844 0.00000 0.00115 0.00000 0.00000 0.00526 0.00489 0.00420 0.00000 0.00380 0.00000 0.00205 C15 0.28303 -0.01179 0.28584 1.00000 0.08821 0.02256 0.03659 0.00630 -0.00903 0.00132 0.04931 0.01036 0.00055 0.00086 0.00039 0.00000 0.00527 0.00344 0.00361 0.00293 0.00318 0.00341 0.00179 H15 0.31154 -0.11572 0.31560 1.00000 0.05917 0.00000 0.00000 N13 0.30123 0.16682 0.30759 1.00000 0.05985 0.03544 0.03136 -0.00055 -0.00996 0.00754 0.04242 0.00841 0.00041 0.00068 0.00031 0.00000 0.00345 0.00329 0.00291 0.00242 0.00240 0.00260 0.00137 B1 0.23375 0.50023 0.25857 0.50000 0.02836 0.03026 0.00130 0.00149 0.00121 0.00000 0.00304 F1 0.21686 0.56632 0.17057 0.50000 0.17150 0.04128 0.08674 -0.00666 -0.08301 -0.00916 0.10138 0.02220 0.00132 0.00189 0.00096 0.00000 0.01665 0.00603 0.01050 0.00771 0.00894 0.00964 0.00559 F2 0.33793 0.57083 0.28310 0.50000 0.09212 0.02390 0.09674 -0.00498 -0.04226 -0.00518 0.07172 0.02201 0.00112 0.00173 0.00088 0.00000 0.00853 0.00477 0.01138 0.00698 0.00647 0.00560 0.00388 Cl1 0.13946 0.57545 0.32972 0.50000 0.19904 0.05248 0.24414 -0.00295 0.09674 0.00897 0.16361 0.01611 0.00065 0.00076 0.00063 0.00000 0.00769 0.00336 0.00942 0.00454 0.00642 0.00399 0.00321 Final Structure Factor Calculation for 2008src1000p2n in P2/n Total number of l.s. parameters = 167 Maximum vector length = 511 Memory required = 2434 / 25039 wR2 = 0.3107 before cycle 9 for 3138 data and 0 / 167 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 108. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.057 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.033 0.000 0.000 GooF = S = 1.124; Restrained GooF = 1.108 for 108 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1746 for 1280 Fo > 4sig(Fo) and 0.3297 for all 3138 data wR2 = 0.3107, GooF = S = 1.124, Restrained GooF = 1.108 for all data Occupancy sum of asymmetric unit = 16.50 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0619 0.0310 0.0184 C1 0.0708 0.0387 0.0275 C2 0.0723 0.0590 0.0275 C3 0.0686 0.0576 0.0263 C4 0.0649 0.0489 0.0381 C5 0.0506 0.0464 0.0261 C6 0.0979 0.0671 0.0369 C7 0.1600 0.1041 0.0409 C8 0.1855 0.1227 0.0302 C9 0.1146 0.0436 0.0407 C10 0.2929 0.0849 0.0390 C11 may be split into 0.1672 0.3800 0.5341 and 0.1591 0.3270 0.5481 0.1678 0.0809 0.0427 C12 0.0572 0.0330 0.0218 C14 0.0906 0.0375 0.0198 C15 0.0658 0.0342 0.0273 N13 0.2279 0.0489 0.0273 F1 may be split into 0.2309 0.5657 0.1630 and 0.2028 0.5670 0.1781 0.1405 0.0525 0.0221 F2 0.3129 0.1266 0.0514 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.008 0.013 0.017 0.023 0.030 0.041 0.056 0.091 1.000 Number in group 325. 313. 351. 274. 312. 317. 310. 319. 301. 316. GooF 1.202 1.103 1.186 1.198 1.142 1.158 1.126 1.141 0.984 0.966 K 123.824 15.232 6.081 4.176 2.222 1.550 1.291 1.112 0.984 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 330. 309. 305. 318. 306. 319. 313. 312. 311. 315. GooF 1.287 1.183 1.167 1.146 1.148 1.147 1.112 1.038 0.935 1.029 K 3.938 2.879 2.059 1.867 1.583 1.213 1.058 1.045 1.015 1.013 R1 0.685 0.649 0.580 0.546 0.474 0.358 0.245 0.193 0.130 0.062 Recommended weighting scheme: WGHT 0.0000 5.5452 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)/su Fc/Fc(max) Resolution(A) -6 7 11 155.51 3.49 3.79 0.013 0.78 -9 2 13 121.43 17.38 3.29 0.029 0.88 -3 1 19 102.07 1.71 3.24 0.009 0.78 11 2 5 77.55 225.49 3.22 0.106 1.01 -2 1 15 95.35 5.58 3.05 0.017 0.99 -9 5 11 107.80 3.05 2.97 0.012 0.82 7 7 4 137.56 10.15 2.90 0.022 0.88 8 2 13 90.24 1.98 2.89 0.010 0.89 4 4 10 76.38 0.17 2.88 0.003 1.09 11 3 5 157.28 47.98 2.84 0.049 0.97 -13 5 1 132.54 6.05 2.83 0.017 0.80 5 7 0 88.82 0.45 2.78 0.005 0.97 14 3 6 90.24 5.04 2.76 0.016 0.79 -8 6 10 139.88 51.71 2.74 0.051 0.82 -8 1 16 131.03 0.97 2.71 0.007 0.81 -1 6 13 79.94 0.03 2.70 0.001 0.84 3 9 1 106.19 21.97 2.69 0.033 0.80 9 7 6 278.17 3.94 2.68 0.014 0.79 -15 3 2 110.27 2.53 2.65 0.011 0.78 -1 3 13 125.18 16.67 2.63 0.029 1.05 11 2 7 117.37 27.56 2.62 0.037 0.96 6 3 13 165.13 3.71 2.62 0.014 0.93 13 2 10 197.07 0.09 2.61 0.002 0.78 -10 2 3 31.82 2.44 2.60 0.011 1.16 1 4 13 -12.62 41.14 2.59 0.045 0.98 -4 7 1 94.83 18.24 2.59 0.030 0.99 -6 8 6 96.95 1.07 2.57 0.007 0.80 5 9 2 114.01 6.16 2.54 0.017 0.77 -4 8 7 72.69 0.03 2.53 0.001 0.82 7 6 10 74.33 10.13 2.53 0.022 0.83 -5 8 8 101.38 1.50 2.52 0.009 0.79 -10 6 1 76.26 0.02 2.50 0.001 0.87 -7 6 9 3.63 83.75 2.49 0.064 0.87 3 8 0 86.35 16.74 2.49 0.029 0.90 5 4 2 66.41 0.02 2.47 0.001 1.45 12 1 9 138.67 15.83 2.47 0.028 0.87 -4 7 2 127.30 1.08 2.46 0.007 0.99 1 8 7 108.15 23.35 2.45 0.034 0.84 -8 4 9 -15.97 33.14 2.44 0.041 0.98 13 4 6 69.19 0.09 2.44 0.002 0.80 14 3 7 77.73 1.79 2.43 0.009 0.77 11 4 6 -23.70 26.77 2.43 0.036 0.89 -3 2 5 343.36 235.22 2.43 0.108 2.05 -3 0 7 208.35 323.21 2.41 0.127 1.94 0 9 1 195.29 9.21 2.41 0.021 0.81 1 3 10 77.96 19.09 2.40 0.031 1.28 2 1 19 67.70 10.30 2.39 0.023 0.78 7 2 14 41.93 1.88 2.39 0.010 0.89 -8 3 16 92.40 6.56 2.38 0.018 0.78 5 5 15 117.18 9.63 2.37 0.022 0.78 Bond lengths and angles C1 - Distance Angles C2 1.3788 (0.0074) C6 1.3814 (0.0079) 124.38 (0.52) N13 1.4668 (0.0067) 117.04 (0.54) 118.37 (0.51) C1 - C2 C6 C2 - Distance Angles C1 1.3788 (0.0074) C3 1.4091 (0.0077) 116.25 (0.56) C10 1.5278 (0.0085) 123.88 (0.53) 119.87 (0.55) C2 - C1 C3 C3 - Distance Angles C4 1.3737 (0.0085) C2 1.4091 (0.0077) 120.53 (0.59) H3 0.9500 119.73 119.73 C3 - C4 C2 C4 - Distance Angles C5 1.3688 (0.0084) C3 1.3737 (0.0085) 120.67 (0.56) H4 0.9500 119.67 119.67 C4 - C5 C3 C5 - Distance Angles C4 1.3688 (0.0084) C6 1.3814 (0.0079) 121.19 (0.59) H5 0.9500 119.41 119.41 C5 - C4 C6 C6 - Distance Angles C1 1.3814 (0.0079) C5 1.3814 (0.0079) 116.97 (0.55) C7 1.5317 (0.0086) 121.54 (0.54) 121.49 (0.58) C6 - C1 C5 C7 - Distance Angles C6 1.5317 (0.0086) C8 1.5324 (0.0109) 110.53 (0.62) C9 1.5363 (0.0105) 110.99 (0.68) 112.59 (0.70) H7 1.0000 107.50 107.50 107.50 C7 - C6 C8 C9 C8 - Distance Angles C7 1.5324 (0.0109) 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 C7 1.5363 (0.0105) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C11 1.4960 (0.0105) C2 1.5278 (0.0085) 114.11 (0.70) C12 1.5627 (0.0117) 110.60 (0.78) 109.59 (0.61) H10 1.0000 107.42 107.42 107.42 C10 - C11 C2 C12 C11 - Distance Angles C10 1.4960 (0.0105) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5627 (0.0117) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C14 - Distance Angles N13_$1 1.3552 (0.0067) N13 1.3552 (0.0067) 103.98 (0.71) B1_$1 1.6298 (0.0137) 127.95 (0.78) 127.07 (0.79) B1 1.6298 (0.0137) 127.07 (0.78) 127.95 (0.78) 17.19 (0.98) C14 - N13_$1 N13 B1_$1 C15 - Distance Angles C15_$1 1.3458 (0.0112) N13 1.3687 (0.0073) 106.76 (0.31) H15 0.9500 126.62 126.62 C15 - C15_$1 N13 N13 - Distance Angles C14 1.3552 (0.0067) C15 1.3687 (0.0073) 111.23 (0.51) C1 1.4668 (0.0067) 127.40 (0.52) 121.31 (0.46) N13 - C14 C15 B1 - Distance Angles F1 1.4299 (0.0237) F2 1.4376 (0.0233) 103.22 (0.94) C14 1.6298 (0.0137) 106.05 (1.09) 105.28 (1.07) Cl1 1.7078 (0.0150) 113.15 (1.27) 110.62 (1.18) 117.32 (0.79) B1 - F1 F2 C14 F1 - Distance Angles B1 1.4299 (0.0237) F1 - F2 - Distance Angles B1 1.4376 (0.0233) F2 - Cl1 - Distance Angles B1 1.7078 (0.0150) Cl1 - FMAP and GRID set by program FMAP 2 2 19 GRID -3.125 24 -2 3.125 1 2 R1 = 0.3291 for 3138 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.1669 0.1551 0.5555 [ 1.23 A from C12 ] Deepest hole -0.34 at 0.8437 0.4430 0.6197 [ 0.80 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2743 / 27196 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1669 0.1551 0.5555 1.00000 0.05 0.35 1.23 C12 1.35 C10 1.36 H12A 1.45 H12C Q2 1 0.1184 0.5714 0.3421 1.00000 0.05 0.31 0.33 CL1 1.99 F2 2.01 B1 2.07 F1 Q3 1 0.1818 0.5046 0.4868 1.00000 0.05 0.24 0.52 H11C 1.40 C11 2.00 H11B 2.06 H11A Q4 1 0.1164 0.4604 0.5119 1.00000 0.05 0.22 0.71 H11C 1.07 C11 1.18 H11B 1.87 H11A Q5 1 0.1799 0.7230 0.2923 1.00000 0.05 0.21 1.33 CL1 1.61 F2 1.80 F1 1.84 B1 Q6 1 0.3395 0.1941 0.3496 1.00000 0.05 0.21 0.66 C1 0.81 N13 1.76 C2 1.80 C6 Q7 1 0.2417 0.7324 0.1709 1.00000 0.05 0.21 1.26 F1 1.32 H15 1.71 F2 1.88 CL1 Q8 1 0.1102 0.6538 0.5052 1.00000 0.05 0.21 1.52 H11C 2.36 C11 2.41 H12B 2.49 H11B Q9 1 0.3902 0.2240 0.2923 1.00000 0.05 0.21 1.21 N13 1.31 H7 1.39 C1 1.59 C6 Q10 1 0.3657 -0.1026 0.2472 1.00000 0.05 0.19 1.26 H15 1.37 C15 2.02 C15 2.15 H8C Shortest distances between peaks (including symmetry equivalents) 3 4 0.96 6 9 1.11 5 7 1.11 4 8 1.42 3 8 1.44 5 10 1.52 2 5 1.56 5 7 2.02 2 7 2.12 5 5 2.20 7 10 2.21 7 10 2.26 2 3 2.36 7 7 2.40 1 4 2.41 9 10 2.51 2 8 2.55 6 10 2.70 2 4 2.70 5 10 2.75 2 10 2.76 1 3 2.78 10 10 2.89 4 8 2.95 4 4 2.97 Time profile in seconds ----------------------- 0.03: 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. 0.58: 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 1.16: Structure factors and derivatives 1.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1000p2n finished at 10:55:01 Total CPU time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++