+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:13:15 on 02-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0073 in P-1 CELL 0.71073 10.0230 10.8755 15.3970 79.211 77.133 69.254 ZERR 2.00 0.0004 0.0005 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H N O P CL UNIT 20 44 20 0 12 16 V = 1519.28 F(000) = 756.0 Mu = 1.08 mm-1 Cell Wt = 1503.59 Rho = 1.643 MERG 2 FMAP 2 PLAN 10 ISOR DFIX 0.87 0.001 N7 H7N DFIX 0.87 0.001 N4 H4N SIZE 0.35 0.14 0.12 BOND $H CONF OMIT -1 1 2 OMIT 2 -2 3 OMIT -2 1 0 ACTA WGHT 0.09590 3.83250 L.S. 4 TEMP -153.00 FVAR 0.28861 H4N 2 0.524682 0.395668 0.160050 11.00000 0.04002 H7N 2 -0.498287 1.326758 0.351116 11.00000 0.01811 MOLE 1 C1 1 0.402262 0.388822 0.089600 11.00000 0.04024 0.06458 = 0.05174 -0.03748 0.00256 -0.01945 AFIX 23 H1A 2 0.468564 0.303646 0.073118 11.00000 -1.20000 H1B 2 0.388733 0.448972 0.034749 11.00000 -1.20000 AFIX 0 C2 1 0.260936 0.373172 0.134188 11.00000 0.05273 0.06915 = 0.09740 -0.04980 0.02027 -0.03498 AFIX 23 H2A 2 0.277288 0.282313 0.161547 11.00000 -1.20000 H2B 2 0.200998 0.389487 0.088999 11.00000 -1.20000 AFIX 0 C3 1 0.181079 0.462901 0.204033 11.00000 0.03911 0.03772 = 0.06480 -0.02108 0.00811 -0.01574 AFIX 23 H3A 2 0.077909 0.483946 0.206567 11.00000 -1.20000 H3B 2 0.204297 0.417246 0.261957 11.00000 -1.20000 AFIX 0 C4 1 0.094881 0.710509 0.183640 11.00000 0.04112 0.03964 = 0.05272 -0.01109 -0.01049 -0.00197 AFIX 23 H4A 2 0.033028 0.705183 0.145147 11.00000 -1.20000 H4B 2 0.133264 0.781608 0.156123 11.00000 -1.20000 AFIX 0 C5 1 0.004232 0.745484 0.272591 11.00000 0.04300 0.02913 = 0.05081 -0.01083 -0.00676 0.00005 AFIX 23 H5A 2 0.064249 0.754325 0.310972 11.00000 -1.20000 H5B 2 -0.033821 0.674533 0.301134 11.00000 -1.20000 AFIX 0 C6 1 -0.120627 0.873954 0.262657 11.00000 0.04232 0.03134 = 0.05655 -0.01009 -0.00383 -0.00480 AFIX 23 H6A 2 -0.082302 0.944090 0.232445 11.00000 -1.20000 H6B 2 -0.181591 0.864053 0.225355 11.00000 -1.20000 AFIX 0 C7 1 -0.211446 0.913363 0.351554 11.00000 0.04287 0.02755 = 0.05807 -0.00663 0.00043 -0.00139 AFIX 23 H7A 2 -0.250112 0.843204 0.381178 11.00000 -1.20000 H7B 2 -0.149490 0.921239 0.388995 11.00000 -1.20000 AFIX 0 C8 1 -0.466876 1.037455 0.325454 11.00000 0.04951 0.05060 = 0.10001 -0.02259 -0.01712 -0.02632 AFIX 23 H8A 2 -0.464477 0.946609 0.329637 11.00000 -1.20000 H8B 2 -0.476599 1.078169 0.264502 11.00000 -1.20000 AFIX 0 C9 1 -0.596946 1.111469 0.389775 11.00000 0.04085 0.04912 = 0.13667 -0.01384 -0.00020 -0.02244 AFIX 23 H9A 2 -0.678677 1.152165 0.358331 11.00000 -1.20000 H9B 2 -0.622047 1.048416 0.438442 11.00000 -1.20000 AFIX 0 C10 1 -0.572497 1.214959 0.427959 11.00000 0.03378 0.05029 = 0.07245 -0.01005 0.00723 -0.01894 AFIX 23 H10A 2 -0.664004 1.284601 0.441666 11.00000 -1.20000 H10B 2 -0.535723 1.177028 0.483612 11.00000 -1.20000 AFIX 0 N1 3 0.405251 0.705722 0.125349 11.00000 0.05208 0.03738 = 0.03335 -0.00406 -0.00638 -0.02022 N2 3 0.516707 0.768238 0.249032 11.00000 0.09440 0.04331 = 0.04718 -0.00490 -0.01774 -0.04064 N3 3 0.429193 0.553610 0.282901 11.00000 0.04346 0.02542 = 0.02956 -0.00570 -0.00771 -0.01230 N4 3 0.467375 0.438427 0.144157 11.00000 0.03418 0.03411 = 0.04394 -0.01978 -0.00825 -0.00339 N5 3 0.215564 0.586195 0.187277 11.00000 0.02715 0.02914 = 0.05420 -0.01251 -0.00757 -0.00190 N6 3 -0.332369 1.038339 0.345048 11.00000 0.02737 0.02462 = 0.06910 -0.01170 -0.00425 -0.00639 N7 3 -0.470568 1.271674 0.366850 11.00000 0.02657 0.02239 = 0.05135 -0.00402 -0.00404 -0.00589 N8 3 -0.271030 1.243504 0.227235 11.00000 0.02937 0.04440 = 0.04149 -0.00489 -0.00272 -0.01182 N9 3 -0.003430 1.229185 0.245363 11.00000 0.03036 0.06775 = 0.09318 0.00616 -0.00545 -0.02830 N10 3 -0.190240 1.168990 0.388134 11.00000 0.02617 0.04611 = 0.05172 -0.01221 -0.00838 -0.00874 P1 5 0.381476 0.575178 0.185918 11.00000 0.03045 0.02616 = 0.03371 -0.00922 -0.00348 -0.00814 P2 5 0.467077 0.799770 0.155205 11.00000 0.06445 0.03441 = 0.03924 -0.00387 -0.00132 -0.02640 P3 5 0.492223 0.646359 0.314434 11.00000 0.04483 0.02805 = 0.03799 -0.00990 -0.00912 -0.01124 P4 5 -0.309634 1.181974 0.329894 11.00000 0.02238 0.02450 = 0.04357 -0.00810 -0.00432 -0.00795 P5 5 -0.123041 1.263384 0.185518 11.00000 0.03271 0.04968 = 0.06038 0.00619 0.00310 -0.01416 P6 5 -0.039569 1.182384 0.347764 11.00000 0.02538 0.05047 = 0.07260 -0.01987 -0.01360 -0.01105 CL1 6 0.324599 0.982563 0.149362 11.00000 0.12710 0.03213 = 0.07891 -0.00082 -0.02253 -0.01225 CL2 6 0.637419 0.819662 0.067575 11.00000 0.15165 0.12447 = 0.06398 -0.00985 0.01098 -0.09663 CL3 6 0.373890 0.709906 0.429663 11.00000 0.07010 0.05769 = 0.04207 -0.02394 -0.00519 -0.01075 CL4 6 0.680480 0.540684 0.355963 11.00000 0.05456 0.05294 = 0.10090 -0.01707 -0.03287 -0.01189 CL5 6 -0.035671 1.164030 0.077272 11.00000 0.07297 0.11759 = 0.07281 -0.01172 0.02149 -0.01734 CL6 6 -0.163264 1.451569 0.124690 11.00000 0.06210 0.07547 = 0.13383 0.03546 -0.02010 -0.03381 CL7 6 -0.003552 1.287447 0.430712 11.00000 0.06111 0.08440 = 0.21052 -0.03514 -0.02837 -0.02963 CL8 6 0.112622 1.009354 0.376260 11.00000 0.03044 0.05770 = 0.08375 -0.01132 -0.01651 -0.00475 HKLF 4 Covalent radii and connectivity table for 03src0073 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - N4 C2 C2 - C1 C3 C3 - N5 C2 C4 - N5 C5 C5 - C4 C6 C6 - C7 C5 C7 - N6 C6 C8 - N6 C9 C9 - C10 C8 C10 - N7 C9 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 N4 - C1 P1 N5 - C4 C3 P1 N6 - C8 C7 P4 N7 - C10 P4 N8 - P5 P4 N9 - P6 P5 N10 - P6 P4 P1 - N4 N1 N3 N5 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl3 Cl4 P4 - N7 N10 N8 N6 P5 - N8 N9 Cl5 Cl6 P6 - N10 N9 Cl8 Cl7 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Cl5 - P5 Cl6 - P5 Cl7 - P6 Cl8 - P6 23097 Reflections read, of which 10 rejected -12 =< h =< 12, -14 =< k =< 14, -19 =< l =< 19, Max. 2-theta = 54.81 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 2 0 918.15 16.04 4 88.53 8 8 0 45.18 0.85 5 7.15 -4 -1 1 366.78 6.46 4 36.53 -3 -1 1 868.42 14.61 4 76.99 2 -1 1 510.10 8.71 4 47.18 -1 1 1 1406.32 31.48 2 329.37 -2 3 1 225.11 3.87 5 22.66 -3 5 1 563.39 10.37 4 54.75 3 5 1 664.31 5.81 4 125.69 4 7 1 70.81 1.38 4 11.53 5 8 1 149.74 2.25 5 22.30 -2 0 2 776.33 13.06 4 83.24 7 0 2 260.30 5.13 4 27.43 2 2 2 1114.47 19.14 3 475.97 6 5 2 102.57 1.78 4 9.49 5 11 2 40.77 0.87 5 6.33 2 4 3 122.49 1.03 5 20.69 4 -2 4 606.84 10.97 4 57.36 3 -1 4 429.15 7.64 4 45.19 -2 0 4 790.97 13.25 4 68.55 0 2 4 485.49 9.46 3 79.56 3 6 4 42.96 0.72 5 5.57 -3 5 5 357.11 7.45 4 40.63 4 10 5 19.81 0.69 4 3.96 4 11 5 39.99 0.89 5 6.27 4 11 6 48.77 0.97 5 7.33 4 5 7 269.24 1.13 7 27.52 7 5 7 97.23 1.52 6 12.79 3 8 8 228.47 6.65 2 33.95 4 10 8 25.39 0.87 5 4.57 4 11 8 41.15 0.93 5 5.75 4 9 9 96.39 1.08 4 22.07 7 7 10 24.92 0.75 4 4.24 6 7 11 39.35 0.88 5 7.20 34 Inconsistent equivalents 6805 Unique reflections, of which 0 suppressed R(int) = 0.1145 R(sigma) = 0.0842 Friedel opposites merged Maximum memory for data reduction = 3396 / 68233 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 = 4242 / 397369 wR2 = 0.2183 before cycle 1 for 6805 data and 315 / 315 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.5937 0.8700 -0.2763 0.0010 DFIX N7 H7N 0.6609 0.8700 -0.2091 0.0010 DFIX N4 H4N 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. 204. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.245 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.000 GooF = S = 1.048; Restrained GooF = 4.456 for 206 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0959 * P )^2 + 3.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28860 0.00346 -0.004 OSF Mean shift/esd = 0.042 Maximum = 2.350 for y H7N Max. shift = 0.213 A for H7N Max. dU = 0.014 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4242 / 397369 wR2 = 0.2184 before cycle 2 for 6805 data and 315 / 315 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.8003 0.8700 -0.0697 0.0010 DFIX N7 H7N 0.8178 0.8700 -0.0522 0.0010 DFIX N4 H4N 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. 204. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.062 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.000 GooF = S = 1.049; Restrained GooF = 1.502 for 206 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0959 * P )^2 + 3.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28858 0.00117 -0.017 OSF Mean shift/esd = 0.058 Maximum = 2.599 for y H7N Max. shift = 0.074 A for H7N Max. dU = 0.018 for H7N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4242 / 397369 wR2 = 0.2185 before cycle 3 for 6805 data and 315 / 315 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. 204. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.000 GooF = S = 1.049; Restrained GooF = 1.033 for 206 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0959 * P )^2 + 3.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28860 0.00080 0.028 OSF Mean shift/esd = 0.024 Maximum = 0.621 for U11 H7N Max. shift = 0.014 A for H4N Max. dU = 0.010 for H7N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4242 / 397369 wR2 = 0.2184 before cycle 4 for 6805 data and 315 / 315 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.8743 0.8700 0.0043 0.0010 DFIX N4 H4N 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. 204. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.000 GooF = S = 1.049; Restrained GooF = 1.035 for 206 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0959 * P )^2 + 3.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28861 0.00080 0.006 OSF Mean shift/esd = 0.008 Maximum = -0.221 for z H4N Max. shift = 0.015 A for H4N Max. dU = 0.001 for H7N Largest correlation matrix elements 0.822 z H7N / y H7N -0.591 U12 N9 / U11 N9 -0.542 U12 C9 / U11 C9 -0.741 U12 Cl2 / U22 Cl2 -0.590 U12 C2 / U11 C2 -0.539 U12 Cl6 / U22 Cl6 -0.739 U12 Cl2 / U11 Cl2 -0.583 U12 C2 / U22 C2 -0.537 U12 C8 / U22 C8 -0.737 z H4N / x H4N -0.566 U12 Cl6 / U11 Cl6 -0.537 U12 C9 / U22 C9 -0.657 y Cl2 / x Cl2 -0.565 U12 N9 / U22 N9 -0.518 U23 C2 / U33 C2 -0.651 U13 Cl2 / U23 Cl2 -0.558 U12 P2 / U11 P2 -0.517 U12 C10 / U11 C10 -0.613 U12 N2 / U11 N2 -0.550 U12 P2 / U22 P2 -0.506 U23 C2 / U22 C2 -0.601 U12 N2 / U22 N2 -0.546 U12 C8 / U11 C8 -0.505 U12 C10 / U22 C10 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4697 0.3020 0.0724 23 0.990 0.000 C1 N4 C2 H1B 0.3884 0.4506 0.0336 23 0.990 0.000 C1 N4 C2 H2A 0.2774 0.2805 0.1618 23 0.990 0.000 C2 C1 C3 H2B 0.1995 0.3902 0.0879 23 0.990 0.000 C2 C1 C3 H3A 0.0757 0.4845 0.2067 23 0.990 0.000 C3 N5 C2 H3B 0.2048 0.4161 0.2631 23 0.990 0.000 C3 N5 C2 H4A 0.0317 0.7053 0.1442 23 0.990 0.000 C4 N5 C5 H4B 0.1340 0.7833 0.1555 23 0.990 0.000 C4 N5 C5 H5A 0.0653 0.7543 0.3117 23 0.990 0.000 C5 C4 C6 H5B -0.0349 0.6732 0.3014 23 0.990 0.000 C5 C4 C6 H6A -0.0812 0.9454 0.2320 23 0.990 0.000 C6 C7 C5 H6B -0.1827 0.8640 0.2246 23 0.990 0.000 C6 C7 C5 H7A -0.2507 0.8416 0.3819 23 0.990 0.000 C7 N6 C6 H7B -0.1481 0.9214 0.3899 23 0.990 0.000 C7 N6 C6 H8A -0.4643 0.9447 0.3294 23 0.990 0.000 C8 N6 C9 H8B -0.4769 1.0792 0.2631 23 0.990 0.000 C8 N6 C9 H9A -0.6800 1.1525 0.3578 23 0.990 0.000 C9 C10 C8 H9B -0.6217 1.0465 0.4393 23 0.990 0.000 C9 C10 C8 H10A -0.6659 1.2853 0.4426 23 0.990 0.000 C10 N7 C9 H10B -0.5340 1.1758 0.4847 23 0.990 0.000 C10 N7 C9 03src0073 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H4N 0.54358 0.38153 0.16500 1.00000 0.05163 0.08168 0.00335 0.00450 0.00344 0.00000 0.01742 H7N -0.50828 1.35319 0.34206 1.00000 0.06028 0.09121 0.00634 0.00232 0.00404 0.00000 0.01907 C1 0.40225 0.38888 0.08942 1.00000 0.04069 0.06498 0.05147 -0.03739 0.00252 -0.02005 0.04910 0.00692 0.00060 0.00064 0.00040 0.00000 0.00294 0.00365 0.00327 0.00288 0.00246 0.00278 0.00142 H1A 0.46970 0.30200 0.07235 1.00000 0.05892 0.00000 0.00000 H1B 0.38840 0.45058 0.03357 1.00000 0.05892 0.00000 0.00000 C2 0.26078 0.37333 0.13402 1.00000 0.05245 0.06906 0.09650 -0.04945 0.01973 -0.03455 0.06850 0.00925 0.00073 0.00073 0.00054 0.00000 0.00371 0.00424 0.00532 0.00399 0.00352 0.00349 0.00207 H2A 0.27738 0.28055 0.16181 1.00000 0.08219 0.00000 0.00000 H2B 0.19954 0.39024 0.08791 1.00000 0.08219 0.00000 0.00000 C3 0.18099 0.46289 0.20408 1.00000 0.03881 0.03704 0.06475 -0.02072 0.00800 -0.01543 0.04678 0.00798 0.00060 0.00053 0.00042 0.00000 0.00285 0.00270 0.00369 0.00255 0.00256 0.00239 0.00134 H3A 0.07567 0.48445 0.20672 1.00000 0.05614 0.00000 0.00000 H3B 0.20477 0.41613 0.26315 1.00000 0.05614 0.00000 0.00000 C4 0.09474 0.71076 0.18355 1.00000 0.04091 0.03954 0.05258 -0.01117 -0.01011 -0.00166 0.04636 0.00828 0.00061 0.00055 0.00039 0.00000 0.00290 0.00283 0.00334 0.00246 0.00248 0.00240 0.00128 H4A 0.03172 0.70531 0.14419 1.00000 0.05563 0.00000 0.00000 H4B 0.13395 0.78332 0.15553 1.00000 0.05563 0.00000 0.00000 C5 0.00408 0.74556 0.27245 1.00000 0.04280 0.02938 0.05096 -0.01124 -0.00626 -0.00025 0.04362 0.00805 0.00060 0.00050 0.00038 0.00000 0.00294 0.00244 0.00317 0.00223 0.00242 0.00225 0.00122 H5A 0.06535 0.75434 0.31171 1.00000 0.05234 0.00000 0.00000 H5B -0.03485 0.67316 0.30144 1.00000 0.05234 0.00000 0.00000 C6 -0.12045 0.87388 0.26271 1.00000 0.04226 0.03110 0.05625 -0.00997 -0.00396 -0.00455 0.04532 0.00828 0.00061 0.00051 0.00040 0.00000 0.00295 0.00251 0.00338 0.00233 0.00251 0.00229 0.00126 H6A -0.08125 0.94544 0.23195 1.00000 0.05439 0.00000 0.00000 H6B -0.18275 0.86399 0.22461 1.00000 0.05439 0.00000 0.00000 C7 -0.21129 0.91324 0.35168 1.00000 0.04297 0.02740 0.05788 -0.00651 0.00058 -0.00141 0.04685 0.00896 0.00062 0.00050 0.00040 0.00000 0.00299 0.00244 0.00352 0.00232 0.00254 0.00225 0.00131 H7A -0.25070 0.84161 0.38194 1.00000 0.05623 0.00000 0.00000 H7B -0.14812 0.92141 0.38988 1.00000 0.05623 0.00000 0.00000 C8 -0.46681 1.03742 0.32527 1.00000 0.04901 0.05032 0.09951 -0.02258 -0.01705 -0.02598 0.06095 0.00823 0.00067 0.00064 0.00053 0.00000 0.00347 0.00341 0.00525 0.00340 0.00341 0.00299 0.00174 H8A -0.46427 0.94469 0.32939 1.00000 0.07314 0.00000 0.00000 H8B -0.47687 1.07921 0.26312 1.00000 0.07314 0.00000 0.00000 C9 -0.59640 1.11103 0.38971 1.00000 0.04116 0.04961 0.13703 -0.01397 -0.00015 -0.02312 0.07574 0.01119 0.00071 0.00068 0.00064 0.00000 0.00344 0.00365 0.00721 0.00411 0.00392 0.00308 0.00232 H9A -0.68000 1.15252 0.35777 1.00000 0.09089 0.00000 0.00000 H9B -0.62173 1.04646 0.43932 1.00000 0.09089 0.00000 0.00000 C10 -0.57229 1.21472 0.42815 1.00000 0.03443 0.05023 0.07282 -0.01044 0.00760 -0.01944 0.05329 0.00907 0.00062 0.00061 0.00046 0.00000 0.00283 0.00327 0.00412 0.00293 0.00269 0.00263 0.00149 H10A -0.66590 1.28531 0.44263 1.00000 0.06395 0.00000 0.00000 H10B -0.53397 1.17580 0.48469 1.00000 0.06395 0.00000 0.00000 N1 0.40518 0.70569 0.12540 1.00000 0.05216 0.03728 0.03315 -0.00370 -0.00656 -0.02027 0.03948 0.00582 0.00050 0.00042 0.00028 0.00000 0.00261 0.00224 0.00219 0.00176 0.00190 0.00207 0.00096 N2 0.51610 0.76863 0.24908 1.00000 0.09472 0.04311 0.04715 -0.00462 -0.01822 -0.04074 0.05570 0.00633 0.00065 0.00047 0.00032 0.00000 0.00416 0.00259 0.00281 0.00215 0.00273 0.00288 0.00137 N3 0.42907 0.55362 0.28297 1.00000 0.04347 0.02571 0.02950 -0.00594 -0.00744 -0.01258 0.03196 0.00516 0.00045 0.00037 0.00025 0.00000 0.00228 0.00184 0.00200 0.00153 0.00169 0.00173 0.00085 N4 0.46804 0.43803 0.14427 1.00000 0.03455 0.03391 0.04266 -0.01987 -0.00717 -0.00469 0.03660 0.00546 0.00045 0.00041 0.00028 0.00000 0.00222 0.00213 0.00238 0.00184 0.00184 0.00186 0.00093 N5 0.21565 0.58613 0.18738 1.00000 0.02714 0.02884 0.05450 -0.01266 -0.00746 -0.00181 0.03769 0.00579 0.00043 0.00040 0.00030 0.00000 0.00200 0.00198 0.00265 0.00184 0.00183 0.00168 0.00094 N6 -0.33249 1.03842 0.34498 1.00000 0.02725 0.02446 0.06925 -0.01167 -0.00408 -0.00630 0.04075 0.00608 0.00044 0.00039 0.00033 0.00000 0.00201 0.00193 0.00307 0.00194 0.00197 0.00167 0.00102 N7 -0.47101 1.27258 0.36655 1.00000 0.02522 0.02477 0.04850 -0.00555 -0.00269 -0.00743 0.03346 0.00569 0.00042 0.00038 0.00029 0.00000 0.00192 0.00191 0.00247 0.00176 0.00174 0.00163 0.00088 N8 -0.27114 1.24356 0.22728 1.00000 0.02937 0.04467 0.04129 -0.00502 -0.00257 -0.01197 0.03906 0.00609 0.00044 0.00044 0.00029 0.00000 0.00209 0.00237 0.00240 0.00190 0.00177 0.00189 0.00095 N9 -0.00351 1.22928 0.24538 1.00000 0.03040 0.06816 0.09284 0.00653 -0.00567 -0.02849 0.06341 0.00822 0.00051 0.00057 0.00041 0.00000 0.00245 0.00346 0.00428 0.00306 0.00255 0.00253 0.00155 N10 -0.19024 1.16899 0.38807 1.00000 0.02649 0.04609 0.05146 -0.01231 -0.00843 -0.00903 0.04092 0.00595 0.00044 0.00045 0.00031 0.00000 0.00204 0.00245 0.00265 0.00204 0.00184 0.00188 0.00099 P1 0.38145 0.57521 0.18592 1.00000 0.03043 0.02610 0.03366 -0.00917 -0.00349 -0.00812 0.02991 0.00160 0.00013 0.00011 0.00008 0.00000 0.00061 0.00056 0.00063 0.00046 0.00048 0.00049 0.00028 P2 0.46704 0.79978 0.15522 1.00000 0.06438 0.03430 0.03925 -0.00378 -0.00139 -0.02634 0.04447 0.00202 0.00018 0.00014 0.00009 0.00000 0.00095 0.00068 0.00075 0.00056 0.00065 0.00069 0.00036 P3 0.49220 0.64634 0.31445 1.00000 0.04485 0.02804 0.03794 -0.00985 -0.00914 -0.01128 0.03594 0.00172 0.00015 0.00012 0.00009 0.00000 0.00074 0.00060 0.00069 0.00050 0.00056 0.00056 0.00031 P4 -0.30964 1.18198 0.32989 1.00000 0.02231 0.02448 0.04360 -0.00810 -0.00435 -0.00791 0.02970 0.00160 0.00012 0.00011 0.00008 0.00000 0.00055 0.00055 0.00070 0.00048 0.00048 0.00046 0.00028 P5 -0.12305 1.26337 0.18554 1.00000 0.03273 0.04973 0.06026 0.00616 0.00310 -0.01419 0.05097 0.00253 0.00016 0.00016 0.00011 0.00000 0.00072 0.00085 0.00096 0.00071 0.00065 0.00065 0.00040 P6 -0.03956 1.18236 0.34777 1.00000 0.02543 0.05059 0.07257 -0.01989 -0.01354 -0.01116 0.04726 0.00193 0.00014 0.00015 0.00012 0.00000 0.00064 0.00083 0.00103 0.00073 0.00063 0.00061 0.00038 Cl1 0.32464 0.98255 0.14935 1.00000 0.12728 0.03201 0.07876 -0.00074 -0.02256 -0.01216 0.08315 0.00312 0.00028 0.00016 0.00014 0.00000 0.00180 0.00074 0.00124 0.00075 0.00118 0.00092 0.00063 Cl2 0.63751 0.81961 0.06755 1.00000 0.15221 0.12501 0.06382 -0.00961 0.01083 -0.09707 0.10446 0.00337 0.00034 0.00028 0.00014 0.00000 0.00233 0.00197 0.00122 0.00121 0.00132 0.00193 0.00088 Cl3 0.37395 0.70985 0.42965 1.00000 0.07015 0.05768 0.04205 -0.02398 -0.00512 -0.01079 0.05764 0.00215 0.00019 0.00016 0.00010 0.00000 0.00100 0.00086 0.00076 0.00065 0.00068 0.00076 0.00041 Cl4 0.68049 0.54071 0.35593 1.00000 0.05452 0.05310 0.10090 -0.01723 -0.03282 -0.01191 0.06668 0.00222 0.00018 0.00017 0.00014 0.00000 0.00091 0.00088 0.00136 0.00086 0.00090 0.00074 0.00048 Cl5 -0.03550 1.16378 0.07733 1.00000 0.07298 0.11739 0.07302 -0.01157 0.02138 -0.01737 0.09717 0.00411 0.00025 0.00028 0.00015 0.00000 0.00130 0.00181 0.00132 0.00122 0.00104 0.00125 0.00073 Cl6 -0.16336 1.45164 0.12470 1.00000 0.06197 0.07555 0.13374 0.03551 -0.02015 -0.03373 0.09338 0.00376 0.00022 0.00022 0.00018 0.00000 0.00112 0.00125 0.00193 0.00126 0.00116 0.00101 0.00075 Cl7 -0.00336 1.28727 0.43064 1.00000 0.06113 0.08433 0.21194 -0.03561 -0.02821 -0.02968 0.11417 0.00371 0.00024 0.00025 0.00025 0.00000 0.00122 0.00150 0.00315 0.00173 0.00155 0.00115 0.00099 Cl8 0.11259 1.00939 0.37626 1.00000 0.03042 0.05770 0.08374 -0.01131 -0.01653 -0.00476 0.05840 0.00224 0.00015 0.00016 0.00012 0.00000 0.00066 0.00088 0.00112 0.00077 0.00068 0.00062 0.00041 Final Structure Factor Calculation for 03src0073 in P-1 Total number of l.s. parameters = 315 Maximum vector length = 511 Memory required = 3927 / 25039 wR2 = 0.2184 before cycle 5 for 6805 data and 0 / 315 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. 204. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.000 GooF = S = 1.049; Restrained GooF = 1.033 for 206 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0959 * P )^2 + 3.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0742 for 4657 Fo > 4sig(Fo) and 0.1087 for all 6805 data wR2 = 0.2184, GooF = S = 1.049, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 34.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0866 0.0386 0.0221 C1 0.1324 0.0400 0.0330 C2 0.0774 0.0343 0.0287 C3 0.0592 0.0485 0.0313 C4 0.0550 0.0517 0.0241 C5 0.0588 0.0492 0.0279 C6 0.0692 0.0471 0.0243 C7 0.1017 0.0565 0.0247 C8 0.1437 0.0516 0.0320 C9 0.0828 0.0493 0.0277 C10 0.0529 0.0332 0.0323 N1 0.0965 0.0462 0.0244 N2 0.0436 0.0305 0.0217 N3 0.0547 0.0349 0.0202 N4 0.0560 0.0351 0.0220 N5 0.0707 0.0290 0.0225 N6 0.0501 0.0261 0.0241 N7 0.0459 0.0427 0.0286 N8 0.1057 0.0641 0.0204 N9 0.0557 0.0414 0.0256 N10 0.0362 0.0312 0.0223 P1 0.0682 0.0393 0.0260 P2 0.0463 0.0388 0.0227 P3 0.0443 0.0233 0.0216 P4 0.0806 0.0444 0.0280 P5 0.0776 0.0432 0.0210 P6 0.1381 0.0795 0.0318 Cl1 0.1849 0.0791 0.0494 Cl2 0.0807 0.0645 0.0277 Cl3 0.1075 0.0507 0.0419 Cl4 0.1444 0.1030 0.0440 Cl5 0.1710 0.0641 0.0451 Cl6 0.2129 0.0809 0.0486 Cl7 may be split into -0.0069 1.2808 0.4424 and 0.0002 1.2938 0.4189 0.0841 0.0634 0.0277 Cl8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.028 0.039 0.051 0.066 0.086 0.115 0.179 1.000 Number in group 734. 685. 622. 724. 660. 687. 668. 674. 672. 679. GooF 0.929 0.965 1.005 1.053 1.073 1.159 1.070 1.150 1.093 0.972 K 3.641 1.374 1.029 1.056 1.015 1.013 1.019 1.019 1.036 0.991 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.66 inf Number in group 707. 664. 692. 680. 663. 692. 668. 673. 684. 682. GooF 0.848 0.851 0.890 0.878 0.939 1.000 0.988 1.071 1.179 1.613 K 1.005 1.008 1.027 1.020 1.034 1.040 1.028 1.033 1.015 0.982 R1 0.266 0.227 0.184 0.150 0.129 0.119 0.087 0.069 0.065 0.068 Recommended weighting scheme: WGHT 0.0948 3.9436 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) 4 3 6 261.87 587.67 4.99 0.130 1.94 2 6 2 63.83 4.96 4.93 0.012 1.81 -1 1 0 1225.44 664.38 4.88 0.138 5.92 0 -3 4 177.83 423.51 4.80 0.110 2.36 -2 -4 1 140.33 43.10 4.79 0.035 2.47 1 0 6 7.11 96.36 4.68 0.053 2.51 -4 1 2 83.04 15.69 4.58 0.021 1.96 1 0 2 1392.10 2448.70 4.43 0.265 6.35 9 -1 14 -11.24 124.34 4.35 0.060 0.79 2 1 5 48.46 166.23 4.33 0.069 2.86 2 -2 1 23.29 114.17 4.27 0.057 2.93 0 2 5 263.41 518.49 4.20 0.122 2.71 3 2 2 25.05 129.79 4.16 0.061 3.17 2 4 11 163.30 63.77 4.06 0.043 1.33 -3 -2 2 200.89 403.87 4.03 0.108 2.65 -4 0 2 60.42 4.86 3.99 0.012 2.11 -1 3 2 49.10 5.56 3.96 0.013 2.73 -2 4 4 137.32 294.16 3.93 0.092 1.75 1 7 6 76.92 17.37 3.91 0.022 1.38 -3 2 0 40.93 0.81 3.91 0.005 2.31 4 -1 8 803.63 482.84 3.89 0.118 1.50 0 1 2 5259.17 8276.53 3.88 0.487 6.37 1 0 5 781.16 483.10 3.79 0.118 2.99 2 -3 4 215.19 414.13 3.77 0.109 2.01 1 1 9 218.51 107.16 3.76 0.055 1.71 3 4 3 746.06 1219.57 3.74 0.187 2.37 3 0 6 181.11 357.26 3.74 0.101 2.12 5 1 13 102.54 30.32 3.70 0.029 1.09 2 -2 10 484.07 278.87 3.70 0.089 1.35 0 0 5 241.79 442.88 3.69 0.113 2.98 2 3 5 251.31 456.67 3.65 0.114 2.52 4 -2 2 401.11 214.94 3.58 0.078 1.87 -5 -1 2 94.84 33.42 3.57 0.031 1.79 5 3 14 198.32 94.95 3.57 0.052 1.04 4 8 5 108.18 33.27 3.54 0.031 1.30 1 0 10 225.99 420.76 3.50 0.110 1.51 -3 1 3 1921.48 1234.31 3.50 0.188 2.27 5 3 11 91.36 33.55 3.41 0.031 1.26 1 -2 5 660.19 427.17 3.40 0.111 2.35 -3 1 2 66.77 18.78 3.39 0.023 2.45 -1 6 3 35.89 1.57 3.37 0.007 1.53 2 1 0 1044.00 1609.91 3.36 0.215 4.84 7 0 0 188.57 88.20 3.36 0.050 1.32 4 -1 2 47.24 8.45 3.32 0.016 2.10 2 5 4 166.18 302.47 3.28 0.093 2.03 -1 -4 3 1237.90 815.98 3.27 0.153 2.20 6 3 0 191.27 96.69 3.26 0.053 1.61 1 7 2 28.72 0.35 3.26 0.003 1.52 0 1 4 1566.85 1079.28 3.25 0.176 3.64 0 3 12 40.04 1.18 3.20 0.006 1.21 Bond lengths and angles C1 - Distance Angles N4 1.4493 (0.0062) C2 1.4844 (0.0080) 114.06 (0.48) H1A 0.9900 108.74 108.74 H1B 0.9900 108.74 108.73 107.64 C1 - N4 C2 H1A C2 - Distance Angles C1 1.4844 (0.0080) C3 1.4863 (0.0079) 113.99 (0.48) H2A 0.9900 108.75 108.75 H2B 0.9900 108.76 108.76 107.65 C2 - C1 C3 H2A C3 - Distance Angles N5 1.4643 (0.0064) C2 1.4863 (0.0080) 112.80 (0.48) H3A 0.9900 109.03 109.03 H3B 0.9900 109.03 109.03 107.80 C3 - N5 C2 H3A C4 - Distance Angles N5 1.4654 (0.0065) C5 1.4963 (0.0077) 114.82 (0.46) H4A 0.9900 108.56 108.56 H4B 0.9900 108.56 108.56 107.54 C4 - N5 C5 H4A C5 - Distance Angles C4 1.4963 (0.0077) C6 1.5162 (0.0071) 111.67 (0.47) H5A 0.9900 109.29 109.28 H5B 0.9900 109.29 109.29 107.95 C5 - C4 C6 H5A C6 - Distance Angles C7 1.5088 (0.0080) C5 1.5162 (0.0072) 112.75 (0.48) H6A 0.9900 109.04 109.04 H6B 0.9900 109.04 109.04 107.81 C6 - C7 C5 H6A C7 - Distance Angles N6 1.4736 (0.0065) C6 1.5088 (0.0080) 114.31 (0.47) H7A 0.9900 108.68 108.68 H7B 0.9900 108.68 108.68 107.61 C7 - N6 C6 H7A C8 - Distance Angles N6 1.4486 (0.0069) C9 1.5163 (0.0099) 111.49 (0.54) H8A 0.9900 109.33 109.33 H8B 0.9900 109.33 109.32 107.97 C8 - N6 C9 H8A C9 - Distance Angles C10 1.4788 (0.0093) C8 1.5163 (0.0099) 113.84 (0.49) H9A 0.9900 108.79 108.79 H9B 0.9900 108.79 108.79 107.67 C9 - C10 C8 H9A C10 - Distance Angles N7 1.4582 (0.0067) C9 1.4788 (0.0093) 111.92 (0.55) H10A 0.9900 109.22 109.23 H10B 0.9900 109.23 109.23 107.92 C10 - N7 C9 H10A N1 - Distance Angles P2 1.5473 (0.0043) P1 1.6074 (0.0042) 124.50 (0.28) N1 - P2 N2 - Distance Angles P3 1.5673 (0.0047) P2 1.5685 (0.0050) 119.05 (0.29) N2 - P3 N3 - Distance Angles P3 1.5569 (0.0038) P1 1.6195 (0.0039) 124.56 (0.25) N3 - P3 N4 - Distance Angles C1 1.4493 (0.0062) P1 1.6073 (0.0040) 120.49 (0.37) H4N 0.8702 (0.0013) 116.58 (4.19) 120.90 (4.17) N4 - C1 P1 N5 - Distance Angles C4 1.4654 (0.0065) C3 1.4643 (0.0065) 117.39 (0.42) P1 1.6188 (0.0042) 124.53 (0.36) 117.69 (0.34) N5 - C4 C3 N6 - Distance Angles C8 1.4486 (0.0069) C7 1.4736 (0.0065) 119.26 (0.44) P4 1.6241 (0.0040) 116.08 (0.37) 122.28 (0.35) N6 - C8 C7 N7 - Distance Angles C10 1.4582 (0.0067) P4 1.6056 (0.0040) 120.91 (0.36) H7N 0.8702 (0.0014) 115.96 (4.35) 121.72 (4.36) N7 - C10 P4 N8 - Distance Angles P5 1.5532 (0.0042) P4 1.6152 (0.0044) 123.71 (0.28) N8 - P5 N9 - Distance Angles P6 1.5659 (0.0061) P5 1.5720 (0.0056) 118.88 (0.29) N9 - P6 N10 - Distance Angles P6 1.5465 (0.0044) P4 1.6014 (0.0042) 124.25 (0.31) N10 - P6 P1 - Distance Angles N4 1.6073 (0.0040) N1 1.6074 (0.0042) 115.86 (0.24) N3 1.6195 (0.0039) 105.30 (0.22) 111.96 (0.21) N5 1.6188 (0.0042) 101.04 (0.21) 106.56 (0.23) 115.95 (0.23) P1 - N4 N1 N3 P2 - Distance Angles N1 1.5473 (0.0043) N2 1.5685 (0.0050) 120.26 (0.24) Cl2 1.9781 (0.0028) 110.57 (0.19) 105.03 (0.24) Cl1 1.9942 (0.0024) 109.34 (0.21) 106.99 (0.21) 103.27 (0.13) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5569 (0.0038) N2 1.5673 (0.0047) 119.55 (0.23) Cl3 1.9926 (0.0019) 109.93 (0.17) 108.26 (0.20) Cl4 2.0039 (0.0021) 110.10 (0.17) 107.42 (0.23) 99.74 (0.09) P3 - N3 N2 Cl3 P4 - Distance Angles N7 1.6056 (0.0040) N10 1.6014 (0.0042) 115.14 (0.23) N8 1.6152 (0.0044) 105.84 (0.22) 112.11 (0.23) N6 1.6241 (0.0040) 100.09 (0.21) 106.70 (0.24) 116.67 (0.24) P4 - N7 N10 N8 P5 - Distance Angles N8 1.5532 (0.0042) N9 1.5720 (0.0057) 119.92 (0.26) Cl5 2.0175 (0.0030) 109.07 (0.20) 108.24 (0.25) Cl6 2.0242 (0.0025) 107.65 (0.19) 110.21 (0.22) 99.89 (0.13) P5 - N8 N9 Cl5 P6 - Distance Angles N10 1.5465 (0.0044) N9 1.5659 (0.0061) 119.91 (0.25) Cl8 2.0034 (0.0021) 108.77 (0.19) 107.98 (0.22) Cl7 2.0262 (0.0032) 105.41 (0.20) 114.71 (0.24) 97.72 (0.11) P6 - N10 N9 Cl8 Cl1 - Distance Angles P2 1.9942 (0.0024) Cl1 - Cl2 - Distance Angles P2 1.9781 (0.0028) Cl2 - Cl3 - Distance Angles P3 1.9926 (0.0019) Cl3 - Cl4 - Distance Angles P3 2.0039 (0.0021) Cl4 - Cl5 - Distance Angles P5 2.0175 (0.0030) Cl5 - Cl6 - Distance Angles P5 2.0242 (0.0025) Cl6 - Cl7 - Distance Angles P6 2.0262 (0.0032) Cl7 - Cl8 - Distance Angles P6 2.0034 (0.0021) Cl8 - Selected torsion angles 26.57 ( 0.92) N4 - C1 - C2 - C3 27.93 ( 0.90) C1 - C2 - C3 - N5 -178.71 ( 0.46) N5 - C4 - C5 - C6 -178.43 ( 0.49) C4 - C5 - C6 - C7 179.31 ( 0.46) C5 - C6 - C7 - N6 26.46 ( 0.91) N6 - C8 - C9 - C10 30.43 ( 0.89) C8 - C9 - C10 - N7 -55.94 ( 0.72) C2 - C1 - N4 - P1 74.05 ( 0.63) C5 - C4 - N5 - C3 -98.55 ( 0.55) C5 - C4 - N5 - P1 124.81 ( 0.59) C2 - C3 - N5 - C4 -62.06 ( 0.67) C2 - C3 - N5 - P1 131.14 ( 0.58) C9 - C8 - N6 - C7 -65.97 ( 0.68) C9 - C8 - N6 - P4 83.02 ( 0.67) C6 - C7 - N6 - C8 -78.78 ( 0.61) C6 - C7 - N6 - P4 -58.29 ( 0.69) C9 - C10 - N7 - P4 -90.91 ( 0.47) C1 - N4 - P1 - N1 144.80 ( 0.42) C1 - N4 - P1 - N3 23.76 ( 0.48) C1 - N4 - P1 - N5 -120.37 ( 0.34) P2 - N1 - P1 - N4 0.40 ( 0.44) P2 - N1 - P1 - N3 128.16 ( 0.35) P2 - N1 - P1 - N5 126.03 ( 0.31) P3 - N3 - P1 - N4 -0.69 ( 0.40) P3 - N3 - P1 - N1 -123.25 ( 0.31) P3 - N3 - P1 - N5 -153.75 ( 0.43) C4 - N5 - P1 - N4 33.67 ( 0.45) C3 - N5 - P1 - N4 -32.31 ( 0.48) C4 - N5 - P1 - N1 155.11 ( 0.39) C3 - N5 - P1 - N1 93.06 ( 0.46) C4 - N5 - P1 - N3 -79.53 ( 0.43) C3 - N5 - P1 - N3 1.91 ( 0.51) P1 - N1 - P2 - N2 124.57 ( 0.31) P1 - N1 - P2 - Cl2 -122.38 ( 0.31) P1 - N1 - P2 - Cl1 -3.94 ( 0.56) P3 - N2 - P2 - N1 -129.24 ( 0.36) P3 - N2 - P2 - Cl2 121.46 ( 0.35) P3 - N2 - P2 - Cl1 -1.33 ( 0.47) P1 - N3 - P3 - N2 124.73 ( 0.27) P1 - N3 - P3 - Cl3 -126.35 ( 0.27) P1 - N3 - P3 - Cl4 3.64 ( 0.54) P2 - N2 - P3 - N3 -123.20 ( 0.34) P2 - N2 - P3 - Cl3 129.93 ( 0.35) P2 - N2 - P3 - Cl4 -91.98 ( 0.47) C10 - N7 - P4 - N10 143.59 ( 0.44) C10 - N7 - P4 - N8 21.97 ( 0.49) C10 - N7 - P4 - N6 -134.31 ( 0.32) P6 - N10 - P4 - N7 -13.23 ( 0.43) P6 - N10 - P4 - N8 115.64 ( 0.35) P6 - N10 - P4 - N6 136.87 ( 0.32) P5 - N8 - P4 - N7 10.56 ( 0.42) P5 - N8 - P4 - N10 -112.88 ( 0.34) P5 - N8 - P4 - N6 39.19 ( 0.49) C8 - N6 - P4 - N7 -158.47 ( 0.44) C7 - N6 - P4 - N7 159.46 ( 0.45) C8 - N6 - P4 - N10 -38.21 ( 0.50) C7 - N6 - P4 - N10 -74.36 ( 0.49) C8 - N6 - P4 - N8 87.97 ( 0.48) C7 - N6 - P4 - N8 -3.09 ( 0.50) P4 - N8 - P5 - N9 122.44 ( 0.30) P4 - N8 - P5 - Cl5 -130.05 ( 0.29) P4 - N8 - P5 - Cl6 -3.04 ( 0.56) P6 - N9 - P5 - N8 -128.96 ( 0.36) P6 - N9 - P5 - Cl5 122.73 ( 0.34) P6 - N9 - P5 - Cl6 8.29 ( 0.50) P4 - N10 - P6 - N9 -116.57 ( 0.30) P4 - N10 - P6 - Cl8 139.49 ( 0.30) P4 - N10 - P6 - Cl7 0.61 ( 0.56) P5 - N9 - P6 - N10 125.84 ( 0.35) P5 - N9 - P6 - Cl8 -126.41 ( 0.34) P5 - N9 - P6 - Cl7 FMAP and GRID set by program FMAP 2 3 40 GRID -1.351 -2 -2 1.351 2 2 R1 = 0.1084 for 6805 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.68 at 0.0021 0.2949 0.3592 [ 1.08 A from CL7 ] Deepest hole -1.44 at -0.0014 0.2724 0.4047 [ 0.45 A from CL7 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3784 / 29955 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0021 1.2949 0.3592 1.00000 0.05 1.68 1.08 CL7 1.48 P6 2.03 N9 2.65 N10 Q2 1 -0.0066 1.4229 0.4829 1.00000 0.05 1.57 1.80 CL7 3.17 H10A 3.36 H5B 3.43 H5A Q3 1 0.6945 0.9790 0.0705 1.00000 0.05 0.91 2.02 CL2 2.79 H6B 3.25 H8B 3.37 CL1 Q4 1 -0.0929 1.3917 0.1613 1.00000 0.05 0.77 0.98 CL6 1.49 P5 2.03 N9 2.52 H3A Q5 1 0.7204 0.8624 0.0680 1.00000 0.05 0.68 1.09 CL2 2.80 H6B 2.84 P2 3.30 N2 Q6 1 0.2470 0.9993 0.1258 1.00000 0.05 0.61 0.88 CL1 2.54 P2 2.87 H4B 2.94 CL5 Q7 1 -0.1340 1.5941 0.0584 1.00000 0.05 0.60 1.77 CL6 2.44 H2B 2.70 CL2 2.99 H4A Q8 1 -0.5695 1.1393 0.2983 1.00000 0.05 0.57 1.03 H8B 1.25 H9A 1.29 C8 1.37 C9 Q9 1 -0.0611 1.1985 0.1348 1.00000 0.05 0.55 0.97 CL5 1.08 P5 2.03 N9 2.21 N8 Q10 1 0.6547 0.6239 0.3339 1.00000 0.05 0.53 0.87 CL4 1.65 P3 2.14 N2 2.79 CL3 Shortest distances between peaks (including symmetry equivalents) 3 5 1.21 2 2 1.90 4 9 2.11 4 7 2.42 1 2 2.53 5 7 2.78 3 6 2.93 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.94: 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 1.20: Structure factors and derivatives 3.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:13:21 Total CPU time: 6.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++