+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 14:16:46 on 23-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC988 in P2(1)/n CELL 0.71073 12.5600 9.1084 14.2275 90.000 102.860 90.000 ZERR 2.00 0.0008 0.0008 0.0011 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL UNIT 32 68 20 8 12 8 V = 1586.82 F(000) = 780.0 Mu = 0.72 mm-1 Cell Wt = 1516.30 Rho = 1.587 MERG 2 OMIT -3.00 55.00 EXTI 0.00032 EQIV $1 0.5-X, 0.5+Y, 0.5-Z BIND C8 C7_$1 BIND C8' C7_$1 FMAP 2 PLAN 10 OMIT 0 0 2 CONF SIZE 0.08 0.06 0.02 TEMP -153 ACTA BOND $H WGHT 0.06570 L.S. 4 FVAR 0.15272 0.56499 H4N 2 0.477142 0.014061 0.612087 11.00000 0.00661 C1 1 0.374853 0.310944 0.225749 11.00000 0.04930 0.03397 = 0.03130 0.00724 0.01866 0.00769 AFIX 23 H1A 2 0.434835 0.304326 0.193203 11.00000 -1.20000 H1B 2 0.364212 0.413546 0.239463 11.00000 -1.20000 AFIX 0 C2 1 0.271698 0.249930 0.161163 11.00000 0.05951 0.02913 = 0.02647 0.00584 0.00495 0.00811 AFIX 23 H2A 2 0.253832 0.306686 0.102051 11.00000 -1.20000 H2B 2 0.284322 0.149220 0.144324 11.00000 -1.20000 AFIX 0 C3 1 0.177936 0.254781 0.209731 11.00000 0.04808 0.03728 = 0.03045 0.01143 -0.00724 0.00485 AFIX 23 H3A 2 0.161960 0.355872 0.223044 11.00000 -1.20000 H3B 2 0.113587 0.213069 0.167627 11.00000 -1.20000 AFIX 0 C4 1 0.442072 0.018222 0.732612 11.00000 0.04177 0.03722 = 0.02567 0.00145 0.00590 0.00978 AFIX 23 H4A 2 0.420057 0.102547 0.765365 11.00000 -1.20000 H4B 2 0.514118 -0.011801 0.767601 11.00000 -1.20000 AFIX 0 C5 1 0.362289 -0.105759 0.732430 11.00000 0.04434 0.04325 = 0.02377 0.00560 0.00863 0.00079 AFIX 23 H5A 2 0.385200 -0.190411 0.700567 11.00000 -1.20000 H5B 2 0.362871 -0.133271 0.798406 11.00000 -1.20000 AFIX 0 C6 1 0.247968 -0.063622 0.681818 11.00000 0.03823 0.05867 = 0.03710 0.01393 0.01174 -0.00034 AFIX 23 H6A 2 0.200161 -0.147406 0.681268 11.00000 -1.20000 H6B 2 0.222542 0.014499 0.717664 11.00000 -1.20000 AFIX 0 C7 1 0.128019 0.010293 0.527017 11.00000 0.03350 0.09166 = 0.06450 0.04062 0.00127 -0.01300 AFIX 23 H7A 2 0.133555 0.055818 0.466655 11.00000 -1.20000 H7B 2 0.096215 -0.086019 0.510906 11.00000 -1.20000 PART 1 AFIX 0 C8 1 0.058200 0.084310 0.559274 21.00000 0.02548 0.07903 = 0.04295 -0.00891 -0.00471 0.00806 AFIX 23 H8A 2 0.082047 0.130573 0.621837 21.00000 -1.20000 H8B 2 -0.016596 0.049245 0.545156 21.00000 -1.20000 PART 2 AFIX 0 C8' 1 0.054809 -0.110458 0.517061 -21.00000 0.01250 0.01587 = 0.04726 0.00935 0.00204 -0.00618 AFIX 23 H8'1 2 -0.019712 -0.093141 0.522711 -21.00000 -1.20000 H8'2 2 0.084020 -0.207503 0.535301 -21.00000 -1.20000 PART 0 AFIX 0 N1 3 0.342922 0.092835 0.452333 11.00000 0.03398 0.02219 = 0.02500 -0.00190 0.00637 0.00057 N2 3 0.292180 0.378986 0.414621 11.00000 0.05315 0.02719 = 0.02483 0.00270 0.01192 0.00284 N3 3 0.298426 0.268920 0.591914 11.00000 0.03927 0.03275 = 0.02564 -0.00229 0.01162 0.00667 N4 3 0.446624 0.059840 0.632967 11.00000 0.02997 0.03083 = 0.02210 -0.00332 0.00375 0.00823 N5 3 0.240571 -0.014253 0.581816 11.00000 0.02532 0.04138 = 0.03015 0.01032 0.00150 -0.00379 O1 4 0.401269 0.227808 0.315802 11.00000 0.03321 0.03147 = 0.02603 0.00517 0.01169 0.00532 O2 4 0.204814 0.171868 0.299732 11.00000 0.03829 0.03331 = 0.02840 0.00230 0.00151 -0.00538 P1 5 0.331796 0.106306 0.561384 11.00000 0.02976 0.02686 = 0.02538 0.00029 0.00532 0.00147 P2 5 0.310452 0.218851 0.376140 11.00000 0.03329 0.02296 = 0.02602 -0.00085 0.00618 0.00218 P3 5 0.287939 0.401760 0.522753 11.00000 0.04943 0.02641 = 0.03173 -0.00129 0.01598 0.00422 CL1 6 0.396694 0.557655 0.578150 11.00000 0.11604 0.05081 = 0.05227 -0.02077 0.02716 -0.03654 CL2 6 0.148698 0.509791 0.526105 11.00000 0.09109 0.06725 = 0.06376 0.02979 0.04881 0.04928 HKLF 4 Covalent radii and connectivity table for 01SRC988 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3 C1 C3 - O2 C2 C4 - N4 C5 C5 - C6 C4 C6 - N5 C5 C7 - C8_a C8'_b N5 C8_a - C7 C7_$1 C8'_b - C7 C7_$1 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 N4 - C4 P1 N5 - C7 C6 P1 O1 - C1 P2 O2 - C3 P2 P1 - N1 N3 N4 N5 P2 - N1 O1 O2 N2 P3 - N3 N2 Cl1 Cl2 Cl1 - P3 Cl2 - P3 Operators for generating equivalent atoms: $1 -x+1/2, y+1/2, -z+1/2 12469 Reflections read, of which 367 rejected -16 =< h =< 15, -10 =< k =< 11, -18 =< l =< 18, Max. 2-theta = 54.90 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 1 1 80.11 3.98 2 36.96 -3 0 5 84.14 2.24 2 63.00 -3 0 7 162.83 4.43 2 105.26 -5 1 7 33.04 0.95 5 5.08 -3 2 7 29.49 0.93 4 6.35 -8 2 10 21.21 0.96 5 4.92 -7 2 13 6.55 1.16 2 8.41 -4 2 15 11.14 0.96 3 4.90 8 Inconsistent equivalents 3558 Unique reflections, of which 0 suppressed R(int) = 0.1215 R(sigma) = 0.1586 Friedel opposites merged Maximum memory for data reduction = 2510 / 35455 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 = 3069 / 245049 wR2 = 0.1540 before cycle 1 for 3558 data and 196 / 196 parameters GooF = S = 0.957; Restrained GooF = 0.957 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15269 0.00046 -0.070 OSF 2 0.56454 0.01140 -0.040 FVAR 2 3 0.00000 0.00070 -1.017 EXTI Mean shift/esd = 0.052 Maximum = -1.017 for EXTI Max. shift = 0.007 A for H4N Max. dU = 0.001 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3069 / 245049 wR2 = 0.1539 before cycle 2 for 3558 data and 196 / 196 parameters GooF = S = 0.957; Restrained GooF = 0.957 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15268 0.00046 -0.020 OSF 2 0.56440 0.01140 -0.012 FVAR 2 3 0.00000 0.00067 -0.833 EXTI Mean shift/esd = 0.022 Maximum = -0.833 for EXTI Max. shift = 0.003 A for H4N Max. dU = 0.001 for H4N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3069 / 245049 wR2 = 0.1539 before cycle 3 for 3558 data and 196 / 196 parameters GooF = S = 0.957; Restrained GooF = 0.957 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15268 0.00046 0.005 OSF 2 0.56440 0.01140 0.000 FVAR 2 3 0.00000 0.00067 -0.834 EXTI Mean shift/esd = 0.007 Maximum = -0.834 for EXTI Max. shift = 0.002 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3069 / 245049 wR2 = 0.1539 before cycle 4 for 3558 data and 196 / 196 parameters GooF = S = 0.957; Restrained GooF = 0.957 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15268 0.00046 -0.003 OSF 2 0.56441 0.01140 0.001 FVAR 2 3 0.00000 0.00067 -0.835 EXTI Mean shift/esd = 0.005 Maximum = -0.835 for EXTI Max. shift = 0.001 A for H4N Max. dU = 0.000 for H4N Largest correlation matrix elements 0.594 U13 Cl2 / U11 Cl2 0.554 U13 Cl2 / U33 Cl2 0.545 U12 Cl2 / U23 Cl2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4361 0.3043 0.1925 23 0.990 0.000 C1 O1 C2 H1B 0.3639 0.4157 0.2397 23 0.990 0.000 C1 O1 C2 H2A 0.2535 0.3077 0.1007 23 0.990 0.000 C2 C3 C1 H2B 0.2846 0.1470 0.1439 23 0.990 0.000 C2 C3 C1 H3A 0.1616 0.3580 0.2232 23 0.990 0.000 C3 O2 C2 H3B 0.1122 0.2123 0.1667 23 0.990 0.000 C3 O2 C2 H4A 0.4196 0.1043 0.7660 23 0.990 0.000 C4 N4 C5 H4B 0.5157 -0.0123 0.7684 23 0.990 0.000 C4 N4 C5 H5A 0.3857 -0.1923 0.6999 23 0.990 0.000 C5 C6 C4 H5B 0.3629 -0.1340 0.7998 23 0.990 0.000 C5 C6 C4 H6A 0.1990 -0.1491 0.6812 23 0.990 0.000 C6 N5 C5 H6B 0.2219 0.0161 0.7184 23 0.990 0.000 C6 N5 C5 H7A 0.1337 0.0567 0.4653 23 0.990 0.000 C7 C8_a N5 H7B 0.0956 -0.0881 0.5104 23 0.990 0.000 C7 C8_a N5 H8A 0.0823 0.1316 0.6230 23 0.990 0.000 C8_a C7 C7_$1 H8B -0.0183 0.0485 0.5447 23 0.990 0.000 C8_a C7 C7_$1 H8'1 -0.0213 -0.0925 0.5229 23 0.990 0.000 C8'_b C7 C7_$1 H8'2 0.0844 -0.2095 0.5356 23 0.990 0.000 C8'_b C7 C7_$1 01SRC988 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H4N 0.47755 0.01399 0.61140 1.00000 0.00925 0.07739 0.00322 0.00466 0.00306 0.00000 0.01330 C1 0.37486 0.31101 0.22569 1.00000 0.04909 0.03391 0.03123 0.00742 0.01848 0.00762 0.03659 0.00959 0.00040 0.00055 0.00032 0.00000 0.00319 0.00307 0.00266 0.00228 0.00265 0.00246 0.00125 H1A 0.43610 0.30430 0.19250 1.00000 0.04391 0.00000 0.00000 H1B 0.36394 0.41571 0.23967 1.00000 0.04391 0.00000 0.00000 C2 0.27167 0.24986 0.16103 1.00000 0.05907 0.02921 0.02646 0.00568 0.00493 0.00783 0.03896 0.00942 0.00041 0.00054 0.00034 0.00000 0.00339 0.00306 0.00254 0.00210 0.00266 0.00253 0.00129 H2A 0.25345 0.30771 0.10067 1.00000 0.04675 0.00000 0.00000 H2B 0.28457 0.14704 0.14392 1.00000 0.04675 0.00000 0.00000 C3 0.17789 0.25484 0.20965 1.00000 0.04790 0.03734 0.03046 0.01167 -0.00721 0.00486 0.04105 0.00990 0.00042 0.00057 0.00034 0.00000 0.00307 0.00327 0.00272 0.00231 0.00251 0.00246 0.00130 H3A 0.16165 0.35804 0.22324 1.00000 0.04926 0.00000 0.00000 H3B 0.11218 0.21231 0.16670 1.00000 0.04926 0.00000 0.00000 C4 0.44212 0.01825 0.73264 1.00000 0.04145 0.03718 0.02570 0.00142 0.00600 0.00962 0.03501 0.00912 0.00038 0.00054 0.00033 0.00000 0.00292 0.00310 0.00243 0.00216 0.00235 0.00244 0.00120 H4A 0.41961 0.10432 0.76603 1.00000 0.04201 0.00000 0.00000 H4B 0.51566 -0.01233 0.76836 1.00000 0.04201 0.00000 0.00000 C5 0.36231 -0.10589 0.73246 1.00000 0.04400 0.04315 0.02407 0.00577 0.00846 0.00079 0.03693 0.00919 0.00038 0.00056 0.00033 0.00000 0.00308 0.00324 0.00248 0.00227 0.00240 0.00256 0.00124 H5A 0.38570 -0.19227 0.69992 1.00000 0.04432 0.00000 0.00000 H5B 0.36291 -0.13400 0.79979 1.00000 0.04432 0.00000 0.00000 C6 0.24785 -0.06363 0.68178 1.00000 0.03795 0.05868 0.03731 0.01416 0.01162 -0.00027 0.04414 0.01021 0.00039 0.00064 0.00035 0.00000 0.00303 0.00378 0.00297 0.00262 0.00260 0.00267 0.00137 H6A 0.19902 -0.14910 0.68121 1.00000 0.05297 0.00000 0.00000 H6B 0.22193 0.01614 0.71836 1.00000 0.05297 0.00000 0.00000 C7 0.12801 0.01020 0.52687 1.00000 0.03294 0.09106 0.06445 0.04018 0.00074 -0.01301 0.06439 0.01193 0.00043 0.00077 0.00044 0.00000 0.00326 0.00543 0.00409 0.00377 0.00319 0.00352 0.00196 H7A_a 0.13373 0.05666 0.46528 1.00000 0.07727 0.00000 0.00000 H7B_a 0.09558 -0.08811 0.51042 1.00000 0.07727 0.00000 0.00000 C8_a 0.05806 0.08431 0.55911 0.56441 0.02566 0.07823 0.04264 -0.00833 -0.00454 0.00765 0.05074 0.01847 0.00074 0.00117 0.00070 0.01140 0.00546 0.00845 0.00591 0.00535 0.00457 0.00508 0.00341 H8A_a 0.08234 0.13156 0.62295 0.56441 0.06088 0.01140 0.00000 H8B_a -0.01827 0.04849 0.54467 0.56441 0.06088 0.01140 0.00000 C8'_b 0.05466 -0.11035 0.51705 0.43559 0.01340 0.01653 0.04677 0.00924 0.00243 -0.00624 0.02623 0.01813 0.00074 0.00110 0.00073 0.01140 0.00536 0.00588 0.00699 0.00483 0.00479 0.00436 0.00324 H8'1_b -0.02134 -0.09248 0.52293 0.43559 0.03148 0.01140 0.00000 H8'2_b 0.08437 -0.20947 0.53560 0.43559 0.03148 0.01140 0.00000 N1 0.34293 0.09284 0.45236 1.00000 0.03400 0.02239 0.02501 -0.00190 0.00638 0.00063 0.02716 0.00664 0.00029 0.00038 0.00024 0.00000 0.00213 0.00218 0.00196 0.00165 0.00177 0.00173 0.00088 N2 0.29217 0.37901 0.41465 1.00000 0.05334 0.02722 0.02489 0.00268 0.01195 0.00272 0.03465 0.00732 0.00032 0.00040 0.00025 0.00000 0.00264 0.00239 0.00203 0.00177 0.00201 0.00200 0.00101 N3 0.29839 0.26894 0.59186 1.00000 0.03943 0.03273 0.02570 -0.00234 0.01172 0.00661 0.03192 0.00703 0.00029 0.00042 0.00025 0.00000 0.00230 0.00244 0.00207 0.00171 0.00191 0.00190 0.00096 N4 0.44666 0.05979 0.63294 1.00000 0.02993 0.03090 0.02184 -0.00325 0.00371 0.00800 0.02788 0.00739 0.00033 0.00047 0.00028 0.00000 0.00236 0.00258 0.00212 0.00183 0.00191 0.00199 0.00100 N5 0.24055 -0.01429 0.58179 1.00000 0.02577 0.04128 0.03018 0.01033 0.00166 -0.00387 0.03313 0.00727 0.00029 0.00043 0.00027 0.00000 0.00211 0.00265 0.00216 0.00186 0.00181 0.00186 0.00098 O1 0.40128 0.22780 0.31583 1.00000 0.03329 0.03156 0.02621 0.00518 0.01189 0.00537 0.02953 0.00564 0.00023 0.00033 0.00020 0.00000 0.00175 0.00193 0.00166 0.00138 0.00149 0.00146 0.00076 O2 0.20481 0.17187 0.29974 1.00000 0.03840 0.03328 0.02866 0.00232 0.00156 -0.00531 0.03437 0.00566 0.00025 0.00034 0.00021 0.00000 0.00188 0.00201 0.00171 0.00147 0.00155 0.00155 0.00081 P1 0.33180 0.10630 0.56138 1.00000 0.02976 0.02688 0.02542 0.00027 0.00533 0.00147 0.02748 0.00228 0.00010 0.00013 0.00008 0.00000 0.00068 0.00072 0.00063 0.00053 0.00055 0.00056 0.00033 P2 0.31046 0.21885 0.37615 1.00000 0.03326 0.02298 0.02601 -0.00086 0.00617 0.00219 0.02748 0.00227 0.00010 0.00013 0.00008 0.00000 0.00070 0.00070 0.00065 0.00052 0.00057 0.00056 0.00033 P3 0.28793 0.40176 0.52274 1.00000 0.04940 0.02643 0.03172 -0.00130 0.01596 0.00421 0.03477 0.00254 0.00011 0.00014 0.00009 0.00000 0.00082 0.00075 0.00069 0.00057 0.00064 0.00063 0.00037 Cl1 0.39670 0.55765 0.57813 1.00000 0.11594 0.05082 0.05230 -0.02077 0.02709 -0.03654 0.07172 0.00289 0.00015 0.00017 0.00011 0.00000 0.00142 0.00100 0.00090 0.00075 0.00095 0.00097 0.00056 Cl2 0.14869 0.50979 0.52609 1.00000 0.09106 0.06731 0.06379 0.02981 0.04877 0.04937 0.06913 0.00361 0.00014 0.00017 0.00011 0.00000 0.00115 0.00114 0.00097 0.00082 0.00093 0.00093 0.00056 Final Structure Factor Calculation for 01SRC988 in P2(1)/n Total number of l.s. parameters = 196 Maximum vector length = 511 Memory required = 2873 / 25039 wR2 = 0.1539 before cycle 5 for 3558 data and 0 / 196 parameters GooF = S = 0.957; Restrained GooF = 0.957 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0612 for 1742 Fo > 4sig(Fo) and 0.1633 for all 3558 data wR2 = 0.1539, GooF = S = 0.957, Restrained GooF = 0.957 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0554 0.0314 0.0230 C1 0.0626 0.0330 0.0213 C2 0.0623 0.0437 0.0172 C3 0.0496 0.0300 0.0254 C4 0.0449 0.0439 0.0220 C5 0.0658 0.0388 0.0278 C6 0.1278 0.0360 0.0294 C7 0.0834 0.0475 0.0213 C8_a 0.0523 0.0190 0.0074 C8'_b 0.0342 0.0260 0.0212 N1 0.0536 0.0279 0.0224 N2 0.0435 0.0317 0.0206 N3 0.0404 0.0231 0.0202 N4 0.0504 0.0257 0.0233 N5 0.0402 0.0270 0.0214 O1 0.0461 0.0301 0.0269 O2 0.0307 0.0265 0.0253 P1 0.0340 0.0262 0.0222 P2 0.0511 0.0298 0.0234 P3 0.1328 0.0543 0.0280 Cl1 0.1430 0.0369 0.0275 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.019 0.029 0.040 0.051 0.068 0.086 0.112 0.172 1.000 Number in group 364. 364. 356. 364. 346. 369. 327. 358. 354. 356. GooF 0.867 0.858 0.926 0.882 0.969 1.016 1.004 1.063 1.041 0.930 K 4.755 2.288 1.078 1.068 0.919 1.000 0.990 1.025 1.013 1.020 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.33 1.66 inf Number in group 357. 359. 354. 354. 357. 352. 363. 350. 353. 359. GooF 0.888 0.843 0.865 0.884 0.927 0.947 1.005 0.931 1.006 1.220 K 1.063 1.116 1.081 1.074 1.058 1.033 1.000 1.011 1.017 1.008 R1 0.448 0.392 0.324 0.276 0.214 0.168 0.112 0.062 0.057 0.044 Recommended weighting scheme: WGHT 0.0598 0.0000 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) 1 0 3 1857.01 1386.76 3.83 0.174 4.04 6 3 2 190.80 107.44 3.68 0.048 1.58 0 3 6 580.17 417.65 3.63 0.095 1.84 3 3 1 1294.58 1017.39 3.62 0.149 2.35 -7 0 15 0.00 517.27 3.60 0.106 0.90 0 1 7 1690.06 1337.92 3.53 0.170 1.94 7 5 10 -101.59 131.54 3.48 0.053 0.87 -3 1 5 464.04 606.79 3.42 0.115 2.48 3 5 9 -25.38 88.89 3.40 0.044 1.08 -1 1 5 1489.88 1197.33 3.37 0.161 2.72 -5 2 14 217.56 114.90 3.29 0.050 0.98 -5 1 13 245.80 349.98 3.29 0.087 1.06 -10 5 8 6.74 98.18 3.21 0.046 0.96 -10 0 2 169.42 314.32 3.19 0.083 1.25 2 1 5 952.11 1187.66 3.13 0.161 2.27 -3 4 2 132.87 57.25 3.13 0.035 1.97 -2 1 15 12.78 99.18 3.11 0.046 0.94 2 0 2 2310.69 1789.87 3.10 0.197 4.15 -1 3 6 418.03 569.12 3.09 0.111 1.87 -1 3 10 377.22 280.73 3.04 0.078 1.28 5 0 3 1826.73 1487.86 3.02 0.180 1.99 -14 3 3 253.37 82.94 2.96 0.042 0.86 -4 2 4 370.60 476.70 2.95 0.102 2.26 -9 3 13 238.01 98.27 2.94 0.046 0.91 0 2 1 126.98 30.19 2.88 0.026 4.33 -5 3 11 91.32 1.09 2.87 0.005 1.15 8 1 0 127.00 189.66 2.87 0.064 1.51 -5 4 10 73.59 146.16 2.84 0.056 1.16 5 1 4 423.66 536.43 2.81 0.108 1.78 -5 2 9 127.26 44.39 2.74 0.031 1.39 -13 1 7 63.65 139.78 2.73 0.055 0.93 0 0 6 2268.99 1886.21 2.71 0.202 2.31 0 1 2 1099.56 922.51 2.71 0.142 5.52 -12 0 6 1594.36 1216.05 2.71 0.163 1.02 9 2 5 253.14 364.52 2.71 0.089 1.09 -1 5 7 968.84 781.40 2.70 0.130 1.36 -7 9 7 706.88 197.16 2.70 0.065 0.84 -11 5 13 251.63 1.63 2.66 0.006 0.79 2 3 1 364.29 263.22 2.66 0.076 2.62 -11 6 12 251.20 3.02 2.66 0.008 0.78 -10 3 12 612.22 375.34 2.65 0.090 0.91 -12 2 5 390.34 275.76 2.63 0.077 1.01 -6 3 17 231.01 1.97 2.63 0.007 0.79 5 1 2 3724.45 3142.90 2.63 0.261 2.10 -5 2 3 482.86 591.33 2.62 0.113 2.12 -3 1 3 742.12 886.33 2.60 0.139 3.24 -12 5 2 387.56 198.01 2.59 0.066 0.91 -5 3 13 97.81 27.36 2.57 0.024 1.01 4 11 0 821.15 497.01 2.56 0.104 0.80 -1 1 4 2199.97 1853.72 2.56 0.201 3.31 Bond lengths and angles C1 - Distance Angles O1 1.4628 (0.0051) C2 1.5183 (0.0067) 109.74 (0.38) H1A 0.9900 109.72 109.72 H1B 0.9900 109.72 109.72 108.20 C1 - O1 C2 H1A C2 - Distance Angles C3 1.4936 (0.0067) C1 1.5183 (0.0067) 111.29 (0.39) H2A 0.9900 109.37 109.37 H2B 0.9900 109.37 109.37 108.00 C2 - C3 C1 H2A C3 - Distance Angles O2 1.4613 (0.0052) C2 1.4936 (0.0067) 109.76 (0.40) H3A 0.9900 109.71 109.71 H3B 0.9900 109.71 109.71 108.20 C3 - O2 C2 H3A C4 - Distance Angles N4 1.4813 (0.0060) C5 1.5107 (0.0066) 110.89 (0.38) H4A 0.9900 109.46 109.46 H4B 0.9900 109.46 109.46 108.05 C4 - N4 C5 H4A C5 - Distance Angles C6 1.5078 (0.0064) C4 1.5107 (0.0066) 111.80 (0.41) H5A 0.9900 109.26 109.26 H5B 0.9900 109.26 109.26 107.93 C5 - C6 C4 H5A C6 - Distance Angles N5 1.4752 (0.0057) C5 1.5078 (0.0064) 112.77 (0.36) H6A 0.9900 109.04 109.04 H6B 0.9900 109.04 109.04 107.81 C6 - N5 C5 H6A C7 - Distance Angles C8_a 1.2718 (0.0103) C8'_b 1.4201 (0.0107) 87.75 (0.68) N5 1.4719 (0.0063) 123.22 (0.68) 117.41 (0.61) H7A_a 0.9900 106.52 114.62 106.52 H7B_a 0.9900 106.52 18.84 106.52 106.52 C7 - C8_a C8'_b N5 H7A_a C8_a - Distance Angles C7 1.2718 (0.0103) C7_$1 10.7113 (0.0130) 60.53 (0.51) H8A_a 0.9900 117.72 117.72 H8B_a 0.9900 117.72 117.72 114.84 C8_a - C7 C7_$1 H8A_a C8'_b - Distance Angles C7 1.4201 (0.0107) C7_$1 11.0204 (0.0117) 49.03 (0.47) H8'1_b 0.9900 118.76 118.76 H8'2_b 0.9900 118.76 118.76 116.15 C8'_b - C7 C7_$1 H8'1_b N1 - Distance Angles P2 1.5692 (0.0036) P1 1.5929 (0.0035) 123.43 (0.23) N1 - P2 N2 - Distance Angles P3 1.5645 (0.0037) P2 1.5928 (0.0038) 119.89 (0.23) N2 - P3 N3 - Distance Angles P3 1.5461 (0.0040) P1 1.6247 (0.0039) 122.28 (0.22) N3 - P3 N4 - Distance Angles C4 1.4813 (0.0060) P1 1.6258 (0.0041) 116.64 (0.32) H4N 0.6866 (0.0389) 114.71 (3.80) 112.93 (3.63) N4 - C4 P1 N5 - Distance Angles C7 1.4719 (0.0063) C6 1.4752 (0.0057) 113.86 (0.36) P1 1.6591 (0.0038) 115.21 (0.32) 118.25 (0.32) N5 - C7 C6 O1 - Distance Angles C1 1.4628 (0.0051) P2 1.5750 (0.0029) 117.00 (0.26) O1 - C1 O2 - Distance Angles C3 1.4613 (0.0052) P2 1.5760 (0.0032) 117.36 (0.29) O2 - C3 P1 - Distance Angles N1 1.5929 (0.0035) N3 1.6247 (0.0039) 114.46 (0.19) N4 1.6258 (0.0042) 109.38 (0.21) 108.44 (0.21) N5 1.6591 (0.0038) 109.46 (0.20) 109.11 (0.19) 105.61 (0.20) P1 - N1 N3 N4 P2 - Distance Angles N1 1.5692 (0.0036) O1 1.5750 (0.0029) 107.82 (0.18) O2 1.5760 (0.0032) 109.12 (0.18) 103.82 (0.16) N2 1.5928 (0.0039) 117.87 (0.19) 108.50 (0.18) 108.80 (0.19) P2 - N1 O1 O2 P3 - Distance Angles N3 1.5461 (0.0040) N2 1.5645 (0.0037) 120.33 (0.20) Cl1 2.0061 (0.0020) 110.49 (0.16) 108.10 (0.16) Cl2 2.0164 (0.0019) 108.55 (0.15) 107.90 (0.16) 99.42 (0.09) P3 - N3 N2 Cl1 Cl1 - Distance Angles P3 2.0061 (0.0020) Cl1 - Cl2 - Distance Angles P3 2.0164 (0.0019) Cl2 - Selected torsion angles 58.03 ( 0.51) O1 - C1 - C2 - C3 -58.04 ( 0.52) C1 - C2 - C3 - O2 -61.06 ( 0.51) N4 - C4 - C5 - C6 56.60 ( 0.58) C4 - C5 - C6 - N5 -127.31 ( 0.58) C8'_b - C7 - C8_a - C7_$1 111.03 ( 0.70) N5 - C7 - C8_a - C7_$1 116.96 ( 0.64) C8_a - C7 - C8'_b - C7_$1 -116.36 ( 0.76) N5 - C7 - C8'_b - C7_$1 56.43 ( 0.48) C5 - C4 - N4 - P1 48.40 ( 0.91) C8_a - C7 - N5 - C6 -58.26 ( 0.84) C8'_b - C7 - N5 - C6 -92.88 ( 0.76) C8_a - C7 - N5 - P1 160.46 ( 0.60) C8'_b - C7 - N5 - P1 172.86 ( 0.49) C5 - C6 - N5 - C7 -47.11 ( 0.57) C5 - C6 - N5 - P1 -56.22 ( 0.44) C2 - C1 - O1 - P2 56.82 ( 0.47) C2 - C3 - O2 - P2 -7.38 ( 0.35) P2 - N1 - P1 - N3 -129.27 ( 0.28) P2 - N1 - P1 - N4 115.45 ( 0.28) P2 - N1 - P1 - N5 -4.84 ( 0.35) P3 - N3 - P1 - N1 117.57 ( 0.28) P3 - N3 - P1 - N4 -127.86 ( 0.27) P3 - N3 - P1 - N5 -160.41 ( 0.33) C4 - N4 - P1 - N1 74.14 ( 0.38) C4 - N4 - P1 - N3 -42.70 ( 0.40) C4 - N4 - P1 - N5 -64.65 ( 0.44) C7 - N5 - P1 - N1 155.85 ( 0.34) C6 - N5 - P1 - N1 61.30 ( 0.43) C7 - N5 - P1 - N3 -78.20 ( 0.38) C6 - N5 - P1 - N3 177.69 ( 0.41) C7 - N5 - P1 - N4 38.19 ( 0.40) C6 - N5 - P1 - N4 137.87 ( 0.25) P1 - N1 - P2 - O1 -109.98 ( 0.26) P1 - N1 - P2 - O2 14.71 ( 0.37) P1 - N1 - P2 - N2 164.95 ( 0.31) C1 - O1 - P2 - N1 49.27 ( 0.34) C1 - O1 - P2 - O2 -66.34 ( 0.35) C1 - O1 - P2 - N2 -164.24 ( 0.32) C3 - O2 - P2 - N1 -49.48 ( 0.35) C3 - O2 - P2 - O1 65.92 ( 0.36) C3 - O2 - P2 - N2 -9.92 ( 0.38) P3 - N2 - P2 - N1 -132.74 ( 0.26) P3 - N2 - P2 - O1 114.93 ( 0.27) P3 - N2 - P2 - O2 9.26 ( 0.39) P1 - N3 - P3 - N2 -117.81 ( 0.24) P1 - N3 - P3 - Cl1 134.15 ( 0.22) P1 - N3 - P3 - Cl2 -1.60 ( 0.40) P2 - N2 - P3 - N3 126.55 ( 0.24) P2 - N2 - P3 - Cl1 -126.79 ( 0.24) P2 - N2 - P3 - Cl2 FMAP and GRID set by program FMAP 2 2 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.1627 for 3558 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.59 at 0.9655 0.1631 0.4173 [ 1.10 A from H8'2 ] Deepest hole -0.37 at 0.0320 0.0797 0.4731 [ 0.19 A from H8'1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3152 / 21119 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0345 -0.1631 0.5827 1.00000 0.05 0.59 1.10 H8'2 1.13 C8' 1.17 H8'1 1.57 H7B Q2 1 0.3218 0.5791 0.5790 1.00000 0.05 0.46 0.96 CL1 1.81 P3 2.23 CL2 2.71 H5A Q3 1 0.4049 0.5398 0.5587 1.00000 0.05 0.45 0.36 CL1 1.92 P3 2.66 N2 2.90 N3 Q4 1 0.3328 0.4817 0.5215 1.00000 0.05 0.39 0.92 P3 1.22 CL1 1.76 N2 2.27 N3 Q5 1 0.2377 0.0831 0.5430 1.00000 0.05 0.36 1.04 N5 1.17 P1 1.50 C7 1.53 H7A Q6 1 -0.0951 -0.2145 0.5203 1.00000 0.05 0.34 1.44 H8'1 1.55 H7A 1.77 C8 1.99 C7 Q7 1 0.1067 -0.1595 0.4858 1.00000 0.05 0.34 0.77 H7B 0.94 H8'2 0.98 C8' 1.49 H8B Q8 1 0.0321 0.0284 0.6290 1.00000 0.05 0.31 1.15 H8A 1.22 C8 1.24 H8B 1.87 H8'1 Q9 1 0.0653 0.5301 0.5300 1.00000 0.05 0.31 1.08 CL2 2.38 H8'2 2.65 CL2 2.82 H5B Q10 1 0.1120 0.2222 0.5760 1.00000 0.05 0.31 1.17 H8A 1.42 C8 1.99 H8'1 2.08 C7 Shortest distances between peaks (including symmetry equivalents) 3 4 1.08 2 3 1.20 2 4 1.24 6 10 1.34 1 6 1.74 9 9 1.76 1 7 1.81 1 8 1.87 5 10 2.16 5 6 2.18 8 10 2.24 7 8 2.42 1 10 2.63 6 7 2.73 7 10 2.75 5 7 2.77 9 10 2.91 1 9 2.94 6 8 2.96 6 8 2.96 7 9 2.97 7 8 2.97 Time profile in seconds ----------------------- 0.11: 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. 0.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.05: Structure factors and derivatives 0.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:16:48 Total elapsed time: 2.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++