+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1280 started at 14:06:45 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1280 in P-1 CELL 0.71073 8.9934 10.0238 10.5796 97.045 107.440 116.265 ZERR 2.00 0.0010 0.0011 0.0012 0.003 0.003 0.004 LATT 1 SFAC C H N O CL UNIT 20 42 12 2 6 V = 778.78 F(000) = 364.0 Mu = 0.59 mm-1 Cell Wt = 695.36 Rho = 1.483 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB N13 Cl2 HTAB N16 Cl2 EQIV_$1 -x-1, -y, -z+1 HTAB N4 Cl1_$1 EQIV_$2 x-1, y-1, z-1 HTAB N4 Cl1_$2 EQIV_$3 x-1, y, z HTAB N12 Cl3_$3 EQIV_$4 -x, -y+1, -z+1 HTAB N15 CL1_$4 HTAB O1W Cl1_$4 EQIV_$5 -x+1, -y+1, -z+1 HTAB N15 CL3_$5 HTAB N16 O1w_$5 EQIV_$6 -x+1, -y+1, -z+2 HTAB N16 Cl2_$6 EQIV_$7 x, y, z-1 HTAB O1w Cl2_$7 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.07 ACTA BOND $H WGHT 0.05080 4.36520 L.S. 8 TEMP -153.00 FVAR 0.76037 MOLE 1 C2 1 -0.541556 -0.183713 0.079245 11.00000 0.02704 0.02427 = 0.01360 -0.00241 0.00292 0.01135 AFIX 23 H2A 2 -0.435676 -0.194899 0.085994 11.00000 -1.20000 H2B 2 -0.605378 -0.192891 -0.018427 11.00000 -1.20000 AFIX 0 C3 1 -0.666919 -0.311042 0.122422 11.00000 0.02740 0.02229 = 0.01950 0.00188 0.00183 0.01325 AFIX 23 H3A 2 -0.712551 -0.414047 0.058395 11.00000 -1.20000 H3B 2 -0.599939 -0.307558 0.217191 11.00000 -1.20000 AFIX 0 C5 1 -0.763775 -0.131212 0.205343 11.00000 0.01964 0.02642 = 0.01913 0.00219 0.00532 0.00934 AFIX 23 H5 2 -0.704210 -0.117768 0.305036 11.00000 -1.20000 H5B 2 -0.870796 -0.119643 0.191638 11.00000 -1.20000 AFIX 0 C6 1 -0.634081 -0.009451 0.160815 11.00000 0.02231 0.02570 = 0.01689 0.00511 0.00396 0.01423 AFIX 23 H6A 2 -0.698577 -0.016479 0.064025 11.00000 -1.20000 H6B 2 -0.589471 0.095516 0.220721 11.00000 -1.20000 AFIX 0 C7 1 -0.319419 0.049257 0.281287 11.00000 0.01571 0.02153 = 0.01578 0.00519 0.00422 0.00666 C8 1 -0.168722 0.034605 0.289668 11.00000 0.02218 0.02631 = 0.01753 0.00473 0.00763 0.01177 AFIX 43 H8 2 -0.179341 -0.039688 0.217356 11.00000 -1.20000 AFIX 0 C9 1 -0.007652 0.125719 0.400291 11.00000 0.02321 0.02767 = 0.01996 0.00671 0.01126 0.01392 AFIX 43 H9 2 0.093116 0.113848 0.406239 11.00000 -1.20000 AFIX 0 C10 1 0.008290 0.238226 0.506292 11.00000 0.01968 0.02336 = 0.01536 0.00754 0.00649 0.00903 C11 1 -0.138404 0.249331 0.498416 11.00000 0.02385 0.02079 = 0.01703 0.00392 0.00715 0.01059 AFIX 43 H11 2 -0.129114 0.324060 0.569507 11.00000 -1.20000 AFIX 0 C14 1 0.315452 0.455736 0.619338 11.00000 0.02058 0.02489 = 0.01972 0.00414 0.00156 0.01566 N1 3 -0.480783 -0.029960 0.169822 11.00000 0.02042 0.02412 = 0.01755 0.00233 0.00416 0.01010 N4 3 -0.821277 -0.290301 0.119790 11.00000 0.02888 0.02222 = 0.01533 0.00530 0.00533 0.00799 AFIX 23 H4A 2 -0.891544 -0.364280 0.152357 11.00000 -1.20000 H4B 2 -0.891275 -0.306832 0.029387 11.00000 -1.20000 AFIX 0 N12 3 -0.299838 0.153437 0.388570 11.00000 0.02253 0.01990 = 0.01585 0.00325 0.00722 0.01155 AFIX 43 H12 2 -0.394918 0.159478 0.387346 11.00000 -1.20000 AFIX 0 N13 3 0.176422 0.336724 0.624867 11.00000 0.02049 0.03058 = 0.00969 0.00561 0.00350 0.01049 AFIX 43 H13 2 0.186653 0.316405 0.704638 11.00000 -1.20000 AFIX 0 N15 3 0.310659 0.488550 0.500827 11.00000 0.01895 0.02414 = 0.01940 0.00574 0.00382 0.00519 AFIX 93 H15A 2 0.213146 0.430189 0.423960 11.00000 -1.20000 H15B 2 0.404997 0.568657 0.499158 11.00000 -1.20000 AFIX 0 N16 3 0.464141 0.542924 0.734653 11.00000 0.01867 0.03156 = 0.01761 0.00306 -0.00224 0.00655 AFIX 93 H16 2 0.468539 0.520673 0.813142 11.00000 -1.20000 H16B 2 0.558188 0.622901 0.732513 11.00000 -1.20000 AFIX 0 MOLE 2 O1W 4 0.158708 0.185944 0.163416 11.00000 0.05579 0.06147 = 0.03213 0.02322 0.02339 0.03985 H1W 2 0.107432 0.235202 0.182819 11.00000 -1.50000 H2W 2 0.157115 0.194402 0.083784 11.00000 -1.50000 MOLE 3 CL3 5 0.434044 0.173977 0.499900 11.00000 0.02236 0.02448 = 0.02038 0.00535 0.00828 0.01213 CL2 5 0.238711 0.321657 0.925626 11.00000 0.02843 0.02884 = 0.01719 0.00433 0.00834 0.01513 CL1 5 0.012849 0.590699 0.790566 11.00000 0.02734 0.02650 = 0.01486 0.00603 0.00419 0.01064 HKLF 4 Covalent radii and connectivity table for 2008src1280 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 C2 - N1 C3 C3 - N4 C2 C5 - N4 C6 C6 - N1 C5 C7 - N12 N1 C8 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 N13 C11 - C10 N12 C14 - N13 N15 N16 N1 - C7 C6 C2 N4 - C3 C5 N12 - C7 C11 N13 - C14 C10 N15 - C14 N16 - C14 O1W - no bonds found Cl3 - no bonds found Cl2 - no bonds found Cl1 - no bonds found Operators for generating equivalent atoms: $1 -x-1, -y, -z+1 $2 x-1, y-1, z-1 $3 x-1, y, z $4 -x, -y+1, -z+1 $5 -x+1, -y+1, -z+1 $6 -x+1, -y+1, -z+2 $7 x, y, z-1 11704 Reflections read, of which 68 rejected -11 =< h =< 11, -12 =< k =< 13, -13 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3520 Unique reflections, of which 0 suppressed R(int) = 0.0816 R(sigma) = 0.0800 Friedel opposites merged Maximum memory for data reduction = 2484 / 35934 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 = 3037 / 233083 wR2 = 0.1981 before cycle 1 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 -0.002 OSF Mean shift/su = 0.001 Maximum = 0.006 for U12 Cl3 Max. shift = 0.000 A for H1W Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 2 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U12 Cl3 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 3 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 4 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2W Max. dU = 0.000 for O1W Least-squares cycle 5 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 5 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Cl2 Max. shift = 0.000 A for H2W Max. dU = 0.000 for O1W Least-squares cycle 6 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 6 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1W Max. dU = 0.000 for N15 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 7 for 3520 data and 187 / 187 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. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Cl2 Max. shift = 0.000 A for H1W Max. dU = 0.000 for C10 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3037 / 233083 wR2 = 0.1981 before cycle 8 for 3520 data and 187 / 187 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.76037 0.00256 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Cl2 Max. shift = 0.000 A for H1W Max. dU = 0.000 for C14 Largest correlation matrix elements 0.911 y H1W / x H1W 0.647 U13 O1W / U23 O1W 0.621 U12 Cl2 / U22 Cl2 0.858 z H2W / x H2W 0.646 z H1W / x H1W 0.617 U12 N12 / U11 N12 0.766 z H2W / y H2W 0.637 y O1W / x O1W 0.617 U12 Cl3 / U22 Cl3 0.680 U12 O1W / U22 O1W 0.631 U12 C6 / U11 C6 0.617 U12 C3 / U11 C3 0.670 U12 O1W / U11 O1W 0.627 U12 Cl2 / U11 Cl2 0.615 U12 N12 / U22 N12 0.669 y H2W / x H2W 0.623 U12 C9 / U11 C9 0.615 U12 C3 / U22 C3 0.656 U12 C14 / U22 C14 0.623 U12 Cl3 / U11 Cl3 0.614 U12 C9 / U22 C9 0.656 U12 C14 / U11 C14 0.623 U12 C6 / U22 C6 0.605 U12 C8 / U11 C8 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.4357 -0.1949 0.0860 23 0.990 0.000 C2 N1 C3 H2B -0.6054 -0.1929 -0.0184 23 0.990 0.000 C2 N1 C3 H3A -0.7126 -0.4140 0.0584 23 0.990 0.000 C3 N4 C2 H3B -0.5999 -0.3076 0.2172 23 0.990 0.000 C3 N4 C2 H5 -0.7042 -0.1178 0.3050 23 0.990 0.000 C5 N4 C6 H5B -0.8708 -0.1196 0.1916 23 0.990 0.000 C5 N4 C6 H6A -0.6986 -0.0165 0.0640 23 0.990 0.000 C6 N1 C5 H6B -0.5895 0.0955 0.2207 23 0.990 0.000 C6 N1 C5 H8 -0.1793 -0.0397 0.2174 43 0.950 0.000 C8 C9 C7 H9 0.0931 0.1138 0.4062 43 0.950 0.000 C9 C8 C10 H11 -0.1291 0.3241 0.5695 43 0.950 0.000 C11 C10 N12 H4A -0.8915 -0.3643 0.1524 23 0.920 0.000 N4 C3 C5 H4B -0.8913 -0.3068 0.0294 23 0.920 0.000 N4 C3 C5 H12 -0.3949 0.1595 0.3873 43 0.880 0.000 N12 C7 C11 H13 0.1867 0.3164 0.7046 43 0.880 0.000 N13 C14 C10 H15A 0.2131 0.4302 0.4240 93 0.880 0.000 N15 C14 N13 H15B 0.4050 0.5687 0.4992 93 0.880 0.000 N15 C14 N13 H16 0.4685 0.5207 0.8131 93 0.880 0.000 N16 C14 N13 H16B 0.5582 0.6229 0.7325 93 0.880 0.000 N16 C14 N13 2008src1280 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.54156 -0.18371 0.07924 1.00000 0.02704 0.02427 0.01360 -0.00241 0.00292 0.01135 0.02454 0.01394 0.00074 0.00061 0.00053 0.00000 0.00282 0.00274 0.00235 0.00202 0.00211 0.00232 0.00113 H2A -0.43568 -0.19490 0.08599 1.00000 0.02945 0.00000 0.00000 H2B -0.60538 -0.19289 -0.01843 1.00000 0.02945 0.00000 0.00000 C3 -0.66692 -0.31104 0.12242 1.00000 0.02740 0.02229 0.01950 0.00188 0.00183 0.01325 0.02524 0.01438 0.00073 0.00062 0.00056 0.00000 0.00287 0.00271 0.00257 0.00212 0.00222 0.00235 0.00115 H3A -0.71255 -0.41405 0.05839 1.00000 0.03029 0.00000 0.00000 H3B -0.59994 -0.30756 0.21719 1.00000 0.03029 0.00000 0.00000 C5 -0.76377 -0.13121 0.20534 1.00000 0.01964 0.02642 0.01913 0.00219 0.00532 0.00934 0.02382 0.01402 0.00070 0.00062 0.00055 0.00000 0.00259 0.00278 0.00254 0.00213 0.00211 0.00223 0.00111 H5 -0.70421 -0.11777 0.30504 1.00000 0.02858 0.00000 0.00000 H5B -0.87080 -0.11964 0.19164 1.00000 0.02858 0.00000 0.00000 C6 -0.63408 -0.00945 0.16082 1.00000 0.02231 0.02570 0.01689 0.00511 0.00396 0.01423 0.02192 0.01420 0.00069 0.00062 0.00053 0.00000 0.00263 0.00271 0.00241 0.00206 0.00207 0.00226 0.00107 H6A -0.69858 -0.01648 0.06402 1.00000 0.02630 0.00000 0.00000 H6B -0.58947 0.09552 0.22072 1.00000 0.02630 0.00000 0.00000 C7 -0.31942 0.04926 0.28129 1.00000 0.01571 0.02153 0.01578 0.00519 0.00422 0.00666 0.01941 0.01336 0.00066 0.00059 0.00051 0.00000 0.00240 0.00254 0.00236 0.00197 0.00194 0.00204 0.00102 C8 -0.16872 0.03461 0.28967 1.00000 0.02218 0.02631 0.01753 0.00473 0.00763 0.01177 0.02248 0.01419 0.00069 0.00063 0.00053 0.00000 0.00266 0.00277 0.00245 0.00210 0.00212 0.00228 0.00108 H8 -0.17934 -0.03969 0.21736 1.00000 0.02698 0.00000 0.00000 C9 -0.00765 0.12572 0.40029 1.00000 0.02321 0.02767 0.01996 0.00671 0.01126 0.01392 0.02250 0.01437 0.00071 0.00062 0.00053 0.00000 0.00266 0.00280 0.00252 0.00214 0.00216 0.00231 0.00108 H9 0.09312 0.11385 0.40624 1.00000 0.02700 0.00000 0.00000 C10 0.00829 0.23823 0.50629 1.00000 0.01968 0.02336 0.01536 0.00754 0.00649 0.00903 0.02019 0.01380 0.00068 0.00060 0.00051 0.00000 0.00253 0.00264 0.00235 0.00201 0.00202 0.00217 0.00104 C11 -0.13840 0.24933 0.49842 1.00000 0.02385 0.02079 0.01703 0.00392 0.00715 0.01059 0.02129 0.01375 0.00069 0.00059 0.00052 0.00000 0.00267 0.00260 0.00244 0.00204 0.00211 0.00222 0.00106 H11 -0.12911 0.32406 0.56951 1.00000 0.02555 0.00000 0.00000 C14 0.31545 0.45574 0.61934 1.00000 0.02058 0.02489 0.01972 0.00414 0.00156 0.01566 0.02198 0.01402 0.00070 0.00062 0.00054 0.00000 0.00256 0.00272 0.00251 0.00210 0.00207 0.00226 0.00108 N1 -0.48078 -0.02996 0.16982 1.00000 0.02042 0.02412 0.01755 0.00233 0.00416 0.01010 0.02250 0.01159 0.00058 0.00051 0.00044 0.00000 0.00222 0.00233 0.00212 0.00178 0.00179 0.00191 0.00094 N4 -0.82128 -0.29030 0.11979 1.00000 0.02888 0.02222 0.01533 0.00530 0.00533 0.00799 0.02517 0.01193 0.00062 0.00052 0.00045 0.00000 0.00248 0.00233 0.00211 0.00178 0.00186 0.00199 0.00099 H4A -0.89154 -0.36428 0.15236 1.00000 0.03020 0.00000 0.00000 H4B -0.89127 -0.30683 0.02939 1.00000 0.03020 0.00000 0.00000 N12 -0.29984 0.15344 0.38857 1.00000 0.02253 0.01990 0.01585 0.00325 0.00722 0.01155 0.01941 0.01128 0.00058 0.00048 0.00042 0.00000 0.00222 0.00216 0.00204 0.00166 0.00175 0.00184 0.00088 H12 -0.39492 0.15948 0.38735 1.00000 0.02330 0.00000 0.00000 N13 0.17642 0.33672 0.62487 1.00000 0.02049 0.03058 0.00969 0.00561 0.00350 0.01049 0.02198 0.01142 0.00057 0.00052 0.00042 0.00000 0.00223 0.00245 0.00191 0.00173 0.00170 0.00194 0.00093 H13 0.18665 0.31640 0.70464 1.00000 0.02637 0.00000 0.00000 N15 0.31066 0.48855 0.50083 1.00000 0.01895 0.02414 0.01940 0.00574 0.00382 0.00519 0.02432 0.01201 0.00059 0.00052 0.00045 0.00000 0.00222 0.00234 0.00220 0.00182 0.00181 0.00188 0.00097 H15A 0.21315 0.43019 0.42396 1.00000 0.02918 0.00000 0.00000 H15B 0.40500 0.56866 0.49916 1.00000 0.02918 0.00000 0.00000 N16 0.46414 0.54292 0.73465 1.00000 0.01867 0.03156 0.01761 0.00306 -0.00224 0.00655 0.02816 0.01196 0.00060 0.00056 0.00047 0.00000 0.00227 0.00259 0.00222 0.00193 0.00183 0.00200 0.00105 H16 0.46854 0.52067 0.81314 1.00000 0.03380 0.00000 0.00000 H16B 0.55819 0.62290 0.73251 1.00000 0.03380 0.00000 0.00000 O1W 0.15871 0.18594 0.16342 1.00000 0.05579 0.06147 0.03213 0.02322 0.02339 0.03985 0.04299 0.01449 0.00069 0.00062 0.00048 0.00000 0.00307 0.00324 0.00248 0.00235 0.00233 0.00267 0.00115 H1W 0.10743 0.23520 0.18282 1.00000 0.06448 0.22258 0.01028 0.00854 0.00707 0.00000 0.00000 H2W 0.15712 0.19440 0.08378 1.00000 0.06448 0.21397 0.01077 0.00924 0.00424 0.00000 0.00000 Cl3 0.43404 0.17398 0.49990 1.00000 0.02236 0.02448 0.02038 0.00535 0.00828 0.01213 0.02249 0.00343 0.00017 0.00015 0.00013 0.00000 0.00063 0.00066 0.00061 0.00049 0.00050 0.00053 0.00030 Cl2 0.23871 0.32166 0.92563 1.00000 0.02843 0.02884 0.01719 0.00433 0.00834 0.01513 0.02502 0.00358 0.00018 0.00016 0.00013 0.00000 0.00069 0.00069 0.00060 0.00050 0.00051 0.00057 0.00032 Cl1 0.01285 0.59070 0.79057 1.00000 0.02734 0.02650 0.01486 0.00603 0.00419 0.01064 0.02529 0.00346 0.00018 0.00015 0.00013 0.00000 0.00069 0.00068 0.00058 0.00049 0.00050 0.00055 0.00032 Final Structure Factor Calculation for 2008src1280 in P-1 Total number of l.s. parameters = 187 Maximum vector length = 511 Memory required = 2850 / 24017 wR2 = 0.1981 before cycle 9 for 3520 data and 0 / 187 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.116; Restrained GooF = 1.116 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 4.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0847 for 2550 Fo > 4sig(Fo) and 0.1248 for all 3520 data wR2 = 0.1981, GooF = S = 1.116, Restrained GooF = 1.116 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0332 0.0293 0.0111 C2 0.0371 0.0217 0.0169 C3 0.0313 0.0228 0.0173 C5 0.0287 0.0220 0.0150 C6 0.0259 0.0181 0.0143 C7 0.0278 0.0223 0.0173 C8 0.0280 0.0234 0.0160 C9 0.0268 0.0196 0.0142 C10 0.0251 0.0222 0.0166 C11 0.0332 0.0210 0.0118 C14 0.0276 0.0238 0.0161 N1 0.0385 0.0218 0.0152 N4 0.0234 0.0203 0.0145 N12 0.0339 0.0228 0.0092 N13 0.0350 0.0218 0.0162 N15 0.0415 0.0317 0.0114 N16 0.0658 0.0381 0.0251 O1W 0.0255 0.0219 0.0201 Cl3 0.0311 0.0274 0.0166 Cl2 0.0354 0.0262 0.0143 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.028 0.043 0.060 0.078 0.098 0.123 0.154 0.220 1.000 Number in group 359. 353. 364. 349. 362. 337. 339. 352. 352. 353. GooF 1.216 1.274 1.202 1.157 1.032 1.068 1.004 0.993 0.932 1.216 K 10.090 2.057 1.303 1.077 1.050 1.005 1.009 1.003 1.001 1.027 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 363. 342. 364. 342. 358. 348. 346. 351. 353. 353. GooF 1.173 1.260 1.169 1.161 1.132 1.102 0.991 0.881 0.936 1.282 K 1.080 1.155 1.020 1.057 1.014 1.040 0.996 0.998 0.993 1.038 R1 0.245 0.228 0.203 0.187 0.147 0.119 0.093 0.077 0.060 0.058 Recommended weighting scheme: WGHT 0.0508 4.3652 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) 0 0 3 9329.31 6904.75 4.36 0.705 3.21 1 0 5 3849.37 2862.77 4.06 0.454 1.71 4 5 3 64.51 0.70 3.52 0.007 0.88 -3 -9 3 93.10 8.75 3.38 0.025 0.82 0 -5 12 136.03 27.60 3.35 0.045 0.83 0 1 2 1807.79 1365.98 3.34 0.314 3.75 2 -1 4 2180.24 1656.58 3.33 0.345 1.86 3 -7 11 80.89 211.32 3.29 0.123 0.79 -5 5 9 59.54 2.11 3.16 0.012 0.96 -7 -5 9 109.01 29.54 3.01 0.046 0.78 0 1 3 2072.15 1621.34 3.00 0.342 2.75 1 0 2 7081.46 5797.32 2.96 0.646 3.46 -5 9 8 -0.88 115.49 2.94 0.091 0.79 -5 -6 6 57.98 0.03 2.93 0.001 0.91 -1 -9 10 2.57 94.61 2.91 0.083 0.80 -5 -1 10 73.92 4.15 2.89 0.017 1.00 -3 -3 13 96.94 207.46 2.88 0.122 0.81 7 -7 3 45.70 3.03 2.88 0.015 1.02 -6 1 9 43.80 5.23 2.87 0.019 1.05 -4 -7 7 179.90 80.92 2.86 0.076 0.89 -9 0 11 117.20 22.51 2.79 0.040 0.77 8 0 2 307.51 103.84 2.79 0.086 0.85 -1 -4 10 40.44 0.04 2.75 0.002 1.01 4 6 0 -10.50 33.30 2.74 0.049 0.93 -3 -6 9 42.30 0.68 2.71 0.007 0.94 0 0 2 155.57 85.43 2.71 0.078 4.82 8 -9 3 75.26 3.11 2.70 0.015 0.88 -10 4 10 82.47 3.28 2.69 0.015 0.78 -6 6 8 81.52 22.35 2.69 0.040 0.97 -5 10 7 84.12 5.14 2.69 0.019 0.78 -7 -4 6 87.04 0.03 2.68 0.001 0.88 -7 6 7 39.71 1.67 2.68 0.011 1.00 1 0 1 445.29 312.98 2.66 0.150 4.99 2 -2 4 3803.95 3130.65 2.66 0.475 1.93 1 1 2 2569.20 2044.57 2.66 0.384 2.80 2 6 5 8.36 82.53 2.63 0.077 0.86 8 -4 2 54.26 6.81 2.63 0.022 0.98 5 -5 9 91.37 13.90 2.62 0.032 0.83 -1 8 3 71.28 1.56 2.59 0.011 1.00 -2 -7 9 55.87 8.45 2.59 0.025 0.92 -8 5 1 50.53 8.75 2.59 0.025 1.10 -8 6 9 58.89 4.33 2.58 0.018 0.86 -9 5 9 -7.89 43.88 2.57 0.056 0.85 1 -1 2 1326.19 1040.34 2.56 0.274 3.87 -5 0 8 39.31 1.28 2.56 0.010 1.20 1 -1 3 670.06 502.64 2.56 0.190 2.83 -8 -1 5 52.22 4.24 2.55 0.017 0.95 -11 7 2 348.89 233.15 2.55 0.130 0.80 0 -1 3 4086.63 3418.92 2.54 0.496 3.35 3 -6 11 69.88 15.34 2.53 0.033 0.80 Bond lengths and angles C2 - Distance Angles N1 1.4733 (0.0066) C3 1.5123 (0.0077) 109.82 (0.43) H2A 0.9900 109.70 109.70 H2B 0.9900 109.70 109.70 108.19 C2 - N1 C3 H2A C3 - Distance Angles N4 1.4849 (0.0070) C2 1.5123 (0.0077) 110.09 (0.43) H3A 0.9900 109.64 109.64 H3B 0.9900 109.64 109.64 108.15 C3 - N4 C2 H3A C5 - Distance Angles N4 1.5050 (0.0068) C6 1.5108 (0.0073) 108.83 (0.42) H5 0.9900 109.92 109.92 H5B 0.9900 109.92 109.92 108.32 C5 - N4 C6 H5 C6 - Distance Angles N1 1.4591 (0.0063) C5 1.5108 (0.0073) 111.53 (0.43) H6A 0.9900 109.32 109.32 H6B 0.9900 109.32 109.32 107.97 C6 - N1 C5 H6A C7 - Distance Angles N12 1.3552 (0.0063) N1 1.3608 (0.0064) 118.26 (0.44) C8 1.4048 (0.0069) 117.72 (0.45) 123.96 (0.47) C7 - N12 N1 C8 - Distance Angles C9 1.3612 (0.0073) C7 1.4048 (0.0069) 120.71 (0.48) H8 0.9500 119.65 119.65 C8 - C9 C7 C9 - Distance Angles C8 1.3612 (0.0073) C10 1.4143 (0.0071) 119.38 (0.48) H9 0.9500 120.31 120.31 C9 - C8 C10 C10 - Distance Angles C11 1.3514 (0.0070) C9 1.4143 (0.0071) 119.37 (0.48) N13 1.4397 (0.0064) 119.59 (0.46) 120.99 (0.45) C10 - C11 C9 C11 - Distance Angles C10 1.3514 (0.0070) N12 1.3645 (0.0065) 120.14 (0.47) H11 0.9500 119.93 119.93 C11 - C10 N12 C14 - Distance Angles N13 1.3156 (0.0069) N15 1.3279 (0.0067) 121.30 (0.47) N16 1.3291 (0.0065) 119.00 (0.49) 119.69 (0.51) C14 - N13 N15 N1 - Distance Angles C7 1.3608 (0.0064) C6 1.4591 (0.0063) 123.27 (0.43) C2 1.4733 (0.0066) 121.21 (0.44) 110.93 (0.42) N1 - C7 C6 N4 - Distance Angles C3 1.4849 (0.0070) C5 1.5050 (0.0068) 113.29 (0.41) H4A 0.9200 108.92 108.92 H4B 0.9200 108.92 108.92 107.74 N4 - C3 C5 H4A N12 - Distance Angles C7 1.3552 (0.0063) C11 1.3645 (0.0065) 122.55 (0.44) H12 0.8800 118.73 118.73 N12 - C7 C11 N13 - Distance Angles C14 1.3156 (0.0070) C10 1.4397 (0.0064) 122.96 (0.43) H13 0.8800 118.52 118.52 N13 - C14 C10 N15 - Distance Angles C14 1.3279 (0.0067) H15A 0.8800 120.00 H15B 0.8800 120.00 120.00 N15 - C14 H15A N16 - Distance Angles C14 1.3291 (0.0065) H16 0.8800 120.00 H16B 0.8800 120.00 120.00 N16 - C14 H16 O1W - Distance Angles H1W 0.8556 (0.0195) H2W 0.8535 (0.0196) 103.52 (3.01) O1W - H1W Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.23 3.096(4) 167.3 N13-H13...Cl2 0.88 2.84 3.562(5) 140.1 N16-H16...Cl2 0.92 2.29 3.166(5) 158.9 N4-H4A...Cl1_$1 0.92 2.34 3.174(5) 151.3 N4-H4B...Cl1_$2 0.88 2.25 3.037(4) 148.9 N12-H12...Cl3_$3 0.88 2.46 3.252(5) 149.5 N15-H15A...Cl1_$4 0.86(2) 2.46(3) 3.297(5) 168(6) O1W-H1W...Cl1_$4 0.88 2.33 3.140(5) 152.9 N15-H15B...Cl3_$5 0.88 2.20 2.997(7) 150.1 N16-H16B...O1W_$5 0.88 2.82 3.426(5) 127.3 N16-H16...Cl2_$6 0.85(2) 2.32(4) 3.123(5) 156(7) O1W-H2W...Cl2_$7 FMAP and GRID set by program FMAP 2 1 27 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.1240 for 3520 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.75 at 0.4663 0.7454 0.5016 [ 0.91 A from CL3 ] Deepest hole -0.50 at 0.4586 0.9357 0.0598 [ 1.06 A from N1 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 2883 / 23400 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5337 0.2546 0.4984 1.00000 0.05 0.75 0.91 CL3 1.60 H15B 1.85 H12 2.32 N15 Q2 1 0.1168 0.6812 0.7942 1.00000 0.05 0.74 0.96 CL1 2.32 H2B 2.50 H4B 2.56 H1W Q3 1 -0.0972 0.5094 0.7824 1.00000 0.05 0.70 0.93 CL1 1.66 H4A 2.40 H15A 2.45 N4 Q4 1 0.1684 0.3787 0.9201 1.00000 0.05 0.70 1.02 CL2 1.99 H3A 2.31 H4A 2.36 H13 Q5 1 0.3038 0.2637 0.9258 1.00000 0.05 0.67 0.99 CL2 1.64 H2A 2.12 H8 2.41 H2W Q6 1 -0.0087 0.4799 0.7837 1.00000 0.05 0.64 1.03 CL1 1.50 H4A 2.22 H11 2.42 N4 Q7 1 0.3374 0.0798 0.4964 1.00000 0.05 0.63 0.95 CL3 2.31 H9 2.46 H5 2.70 N12 Q8 1 0.0095 0.6721 0.7939 1.00000 0.05 0.59 0.83 CL1 1.73 H1W 2.28 H15A 2.33 H4B Q9 1 0.2148 0.2162 0.8979 1.00000 0.05 0.57 0.97 CL2 1.86 H8 2.05 H2A 2.19 H2W Q10 1 0.3497 0.3491 0.9294 1.00000 0.05 0.57 0.90 CL2 2.02 H2A 2.28 H13 2.30 H16 Shortest distances between peaks (including symmetry equivalents) 5 9 0.66 5 10 0.76 2 8 0.93 3 6 0.96 9 10 1.26 3 8 1.45 4 10 1.76 2 6 1.79 6 8 1.85 1 7 1.85 4 9 1.86 2 3 1.89 4 5 2.01 4 6 2.46 10 10 2.81 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.55: 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 0.97: Structure factors and derivatives 1.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1280 finished at 14:06:49 Total CPU time: 3.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++