+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0260 started at 22:44:00 on 19-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0260 in P4(1)2(1)2 CELL 0.71073 9.4197 9.4197 42.3480 90.000 90.000 90.000 ZERR 8.00 0.0001 0.0001 0.0009 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - Y, 1/2 + X, 1/4 + Z SYMM 1/2 + Y, 1/2 - X, 3/4 + Z SYMM 1/2 - X, 1/2 + Y, 1/4 - Z SYMM 1/2 + X, 1/2 - Y, 3/4 - Z SYMM Y, X, - Z SYMM - Y, - X, 1/2 - Z SFAC C H N O P CL UNIT 120 136 32 8 24 16 V = 3757.57 F(000) = 1776.0 Mu = 0.61 mm-1 Cell Wt = 3465.09 Rho = 1.531 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.12 0.12 0.16 ACTA BOND WGHT 0.09740 L.S. 4 TEMP -153.00 FVAR 0.15646 C1 1 0.524109 0.269833 0.058539 11.00000 0.04692 0.02901 = 0.06050 0.00052 -0.00072 -0.01170 AFIX 23 H1A 2 0.521839 0.181376 0.071153 11.00000 -1.20000 H1B 2 0.538771 0.243707 0.036131 11.00000 -1.20000 AFIX 0 C2 1 0.383312 0.348019 0.062056 11.00000 0.03525 0.05323 = 0.06786 -0.00156 0.00362 -0.01910 AFIX 23 H2A 2 0.307732 0.294662 0.050965 11.00000 -1.20000 H2B 2 0.357540 0.353700 0.084685 11.00000 -1.20000 AFIX 0 C3 1 0.393405 0.493166 0.048745 11.00000 0.03687 0.13620 = 0.32669 0.16522 0.03120 0.00885 AFIX 23 H3A 2 0.341310 0.491229 0.028446 11.00000 -1.20000 H3B 2 0.338459 0.555559 0.063047 11.00000 -1.20000 AFIX 0 C4 1 0.946782 0.820644 0.072313 11.00000 0.02126 0.02932 = 0.03020 0.00491 -0.00270 0.00477 C5 1 0.897192 0.898107 0.098487 11.00000 0.03046 0.03610 = 0.03024 0.00249 0.00603 0.00340 AFIX 43 H5 2 0.863829 0.849403 0.116676 11.00000 -1.20000 AFIX 0 C6 1 0.896834 1.044787 0.097838 11.00000 0.03118 0.03936 = 0.05015 -0.00730 0.00505 -0.00033 AFIX 43 H6 2 0.861565 1.096597 0.115413 11.00000 -1.20000 AFIX 0 C7 1 0.948090 1.116861 0.071463 11.00000 0.02859 0.02239 = 0.05283 0.00237 -0.00047 0.00236 AFIX 43 H7 2 0.945761 1.217649 0.070855 11.00000 -1.20000 AFIX 0 C8 1 1.001427 1.042772 0.046604 11.00000 0.03676 0.02736 = 0.03647 0.00476 0.00252 0.00276 AFIX 43 H8 2 1.038275 1.092610 0.028907 11.00000 -1.20000 AFIX 0 C9 1 1.002902 0.893809 0.046677 11.00000 0.03567 0.03257 = 0.02699 -0.00042 0.00670 0.00222 AFIX 43 H9 2 1.042000 0.843275 0.029320 11.00000 -1.20000 AFIX 0 C10 1 1.010970 0.555137 0.104834 11.00000 0.02717 0.02635 = 0.02820 -0.00216 0.00136 0.00142 C11 1 1.143162 0.604695 0.114618 11.00000 0.02932 0.04541 = 0.04366 0.00566 -0.00425 -0.00040 AFIX 43 H11 2 1.187992 0.680950 0.103843 11.00000 -1.20000 AFIX 0 C12 1 1.209638 0.539652 0.140866 11.00000 0.03145 0.06436 = 0.04433 -0.01295 -0.01597 0.01099 AFIX 43 H12 2 1.299042 0.572900 0.148151 11.00000 -1.20000 AFIX 0 C13 1 1.143585 0.427807 0.155738 11.00000 0.05950 0.04558 = 0.03150 -0.00608 -0.00378 0.02663 AFIX 43 H13 2 1.188244 0.384897 0.173443 11.00000 -1.20000 AFIX 0 C14 1 1.014874 0.376594 0.145668 11.00000 0.05608 0.03224 = 0.03014 0.00381 0.00058 0.00740 AFIX 43 H14 2 0.971692 0.298285 0.156041 11.00000 -1.20000 AFIX 0 C15 1 0.949429 0.440268 0.120368 11.00000 0.03716 0.03370 = 0.03077 -0.00384 0.00135 -0.00064 AFIX 43 H15 2 0.860331 0.405202 0.113322 11.00000 -1.20000 AFIX 0 N1 3 0.757231 0.599652 0.073656 11.00000 0.02440 0.03299 = 0.03488 0.00131 -0.00040 -0.00549 N2 3 1.000218 0.572702 0.039541 11.00000 0.02495 0.03199 = 0.02870 0.00185 -0.00235 -0.00114 N3 3 0.750784 0.467365 0.017278 11.00000 0.04196 0.03386 = 0.03840 -0.00152 -0.00683 -0.01193 N4 3 0.512776 0.558248 0.043245 11.00000 0.02929 0.03607 = 0.07536 0.01968 -0.01550 -0.00337 AFIX 43 H4 2 0.506765 0.643020 0.034616 11.00000 -1.20000 AFIX 0 O1 4 0.640556 0.358844 0.069163 11.00000 0.03226 0.03029 = 0.04189 0.00997 0.00247 -0.00356 P1 5 0.670321 0.500338 0.050531 11.00000 0.02375 0.02821 = 0.04011 0.00598 -0.00565 -0.00292 P2 5 0.922684 0.631779 0.071010 11.00000 0.02215 0.02777 = 0.02865 0.00121 -0.00035 -0.00194 P3 5 0.909159 0.511469 0.011863 11.00000 0.03366 0.02365 = 0.02997 0.00249 -0.00130 -0.00068 CL1 6 0.915664 0.643807 -0.025703 11.00000 0.04835 0.03067 = 0.03515 0.00958 -0.00343 0.00118 CL2 6 1.016774 0.344888 -0.006618 11.00000 0.05613 0.02684 = 0.03932 0.00052 0.00592 0.00466 HKLF 4 Covalent radii and connectivity table for 2007src0260 in P4(1)2(1)2 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 - N4 C2 C4 - C9 C5 P2 C5 - C6 C4 C6 - C5 C7 C7 - C8 C6 C8 - C7 C9 C9 - C4 C8 C10 - C15 C11 P2 C11 - C10 C12 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 N1 - P1 P2 N2 - P3 P2 N3 - P3 P1 N4 - C3 P1 O1 - C1 P1 P1 - O1 N1 N4 N3 P2 - N1 N2 C4 C10 P3 - N2 N3 Cl1 Cl2 Cl1 - P3 Cl2 - P3 h k l Fo^2 Sigma Why rejected 0 3 0 0.50 0.10 observed but should be systematically absent 7199 Reflections read, of which 46 rejected -12 =< h =< 12, -8 =< k =< 8, -52 =< l =< 36, Max. 2-theta = 55.00 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 3 -0.46 0.20 2 1.55 2 4 3 30.71 0.74 2 4.50 0 7 3 55.79 1.53 2 8.55 1 4 5 33.66 0.70 2 3.80 -3 5 5 24.30 0.70 2 5.90 -2 3 13 12.30 0.38 2 1.95 2 5 13 21.39 0.80 2 5.15 4 5 17 10.26 0.68 2 4.30 2 2 20 10.85 0.41 2 2.15 -2 4 22 30.13 1.11 2 6.05 -2 4 25 23.67 0.95 2 5.30 -2 3 26 11.43 0.55 2 3.00 0 4 28 64.11 1.95 2 11.85 -2 4 29 9.80 0.85 2 4.90 1 5 29 5.82 0.64 2 3.40 0 2 32 37.01 1.32 2 7.40 16 Inconsistent equivalents 4159 Unique reflections, of which 0 suppressed R(int) = 0.0477 R(sigma) = 0.0898 Friedel opposites not merged Maximum memory for data reduction = 2163 / 44841 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 = 2791 / 282114 wR2 = 0.1695 before cycle 1 for 4159 data and 226 / 226 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0974 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15636 0.00046 -0.214 OSF Mean shift/esd = 0.033 Maximum = -0.214 for OSF Max. shift = 0.001 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2791 / 282114 wR2 = 0.1695 before cycle 2 for 4159 data and 226 / 226 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0974 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15632 0.00046 -0.096 OSF Mean shift/esd = 0.011 Maximum = -0.096 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2791 / 282114 wR2 = 0.1695 before cycle 3 for 4159 data and 226 / 226 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0974 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15632 0.00046 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.004 for x Cl2 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2791 / 282114 wR2 = 0.1695 before cycle 4 for 4159 data and 226 / 226 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0974 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15632 0.00046 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U22 C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Largest correlation matrix elements 0.681 U23 C3 / U22 C3 0.652 U23 C3 / U33 C3 0.594 U12 C3 / U13 C3 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5218 0.1814 0.0712 23 0.990 0.000 C1 O1 C2 H1B 0.5388 0.2437 0.0361 23 0.990 0.000 C1 O1 C2 H2A 0.3077 0.2947 0.0510 23 0.990 0.000 C2 C3 C1 H2B 0.3576 0.3539 0.0847 23 0.990 0.000 C2 C3 C1 H3A 0.3414 0.4911 0.0284 23 0.990 0.000 C3 N4 C2 H3B 0.3383 0.5556 0.0630 23 0.990 0.000 C3 N4 C2 H5 0.8638 0.8494 0.1167 43 0.950 0.000 C5 C6 C4 H6 0.8616 1.0966 0.1154 43 0.950 0.000 C6 C5 C7 H7 0.9458 1.2176 0.0709 43 0.950 0.000 C7 C8 C6 H8 1.0382 1.0926 0.0289 43 0.950 0.000 C8 C7 C9 H9 1.0421 0.8433 0.0293 43 0.950 0.000 C9 C4 C8 H11 1.1880 0.6810 0.1038 43 0.950 0.000 C11 C10 C12 H12 1.2991 0.5729 0.1481 43 0.950 0.000 C12 C13 C11 H13 1.1882 0.3849 0.1734 43 0.950 0.000 C13 C14 C12 H14 0.9718 0.2983 0.1560 43 0.950 0.000 C14 C13 C15 H15 0.8604 0.4052 0.1133 43 0.950 0.000 C15 C14 C10 H4 0.5068 0.6431 0.0346 43 0.880 0.000 N4 C3 P1 2007src0260 in P4(1)2(1)2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.52414 0.26984 0.05855 1.00000 0.04683 0.02889 0.06054 0.00046 -0.00082 -0.01178 0.04542 0.00889 0.00058 0.00054 0.00014 0.00000 0.00320 0.00261 0.00371 0.00240 0.00271 0.00229 0.00137 H1A 0.52185 0.18141 0.07117 1.00000 0.05450 0.00000 0.00000 H1B 0.53881 0.24367 0.03614 1.00000 0.05450 0.00000 0.00000 C2 0.38333 0.34808 0.06205 1.00000 0.03507 0.05312 0.06771 -0.00156 0.00361 -0.01905 0.05197 0.00979 0.00057 0.00062 0.00015 0.00000 0.00295 0.00355 0.00394 0.00306 0.00282 0.00251 0.00152 H2A 0.30774 0.29467 0.05098 1.00000 0.06236 0.00000 0.00000 H2B 0.35760 0.35387 0.08468 1.00000 0.06236 0.00000 0.00000 C3 0.39336 0.49315 0.04871 1.00000 0.03703 0.13583 0.32499 0.16452 0.03140 0.00895 0.16595 0.02212 0.00076 0.00107 0.00032 0.00000 0.00397 0.00816 0.01608 0.00992 0.00654 0.00477 0.00618 H3A 0.34142 0.49107 0.02839 1.00000 0.19914 0.00000 0.00000 H3B 0.33826 0.55558 0.06298 1.00000 0.19914 0.00000 0.00000 C4 0.94680 0.82064 0.07231 1.00000 0.02108 0.02927 0.03011 0.00497 -0.00266 0.00480 0.02682 0.00786 0.00045 0.00047 0.00011 0.00000 0.00214 0.00228 0.00262 0.00199 0.00187 0.00172 0.00099 C5 0.89720 0.89811 0.09848 1.00000 0.03019 0.03602 0.03028 0.00249 0.00605 0.00337 0.03216 0.00793 0.00047 0.00050 0.00011 0.00000 0.00250 0.00265 0.00258 0.00207 0.00197 0.00197 0.00107 H5 0.86384 0.84942 0.11667 1.00000 0.03860 0.00000 0.00000 C6 0.89684 1.04480 0.09782 1.00000 0.03122 0.03919 0.04995 -0.00734 0.00506 -0.00041 0.04012 0.00883 0.00051 0.00053 0.00013 0.00000 0.00265 0.00287 0.00334 0.00244 0.00236 0.00207 0.00125 H6 0.86155 1.09663 0.11540 1.00000 0.04814 0.00000 0.00000 C7 0.94808 1.11682 0.07146 1.00000 0.02838 0.02246 0.05268 0.00228 -0.00046 0.00235 0.03451 0.00812 0.00047 0.00047 0.00013 0.00000 0.00245 0.00225 0.00323 0.00222 0.00232 0.00182 0.00114 H7 0.94576 1.21761 0.07085 1.00000 0.04141 0.00000 0.00000 C8 1.00139 1.04274 0.04661 1.00000 0.03662 0.02728 0.03635 0.00479 0.00241 0.00261 0.03342 0.00805 0.00052 0.00046 0.00011 0.00000 0.00262 0.00234 0.00281 0.00195 0.00229 0.00207 0.00108 H8 1.03821 1.09259 0.02891 1.00000 0.04010 0.00000 0.00000 C9 1.00292 0.89381 0.04668 1.00000 0.03559 0.03240 0.02678 -0.00035 0.00667 0.00227 0.03159 0.00849 0.00053 0.00049 0.00011 0.00000 0.00254 0.00246 0.00263 0.00187 0.00211 0.00209 0.00106 H9 1.04205 0.84329 0.02932 1.00000 0.03791 0.00000 0.00000 C10 1.01096 0.55516 0.10484 1.00000 0.02702 0.02624 0.02816 -0.00232 0.00130 0.00141 0.02714 0.00753 0.00049 0.00044 0.00010 0.00000 0.00221 0.00220 0.00233 0.00178 0.00192 0.00176 0.00094 C11 1.14317 0.60472 0.11461 1.00000 0.02935 0.04540 0.04352 0.00567 -0.00421 -0.00052 0.03942 0.00894 0.00053 0.00059 0.00011 0.00000 0.00254 0.00311 0.00306 0.00243 0.00227 0.00215 0.00121 H11 1.18798 0.68098 0.10384 1.00000 0.04731 0.00000 0.00000 C12 1.20969 0.53967 0.14085 1.00000 0.03143 0.06440 0.04421 -0.01312 -0.01609 0.01117 0.04668 0.00925 0.00057 0.00062 0.00013 0.00000 0.00266 0.00386 0.00327 0.00283 0.00235 0.00247 0.00140 H12 1.29914 0.57286 0.14812 1.00000 0.05602 0.00000 0.00000 C13 1.14355 0.42782 0.15573 1.00000 0.05928 0.04538 0.03157 -0.00612 -0.00372 0.02662 0.04541 0.01014 0.00062 0.00059 0.00013 0.00000 0.00361 0.00315 0.00284 0.00254 0.00261 0.00273 0.00134 H13 1.18817 0.38494 0.17345 1.00000 0.05449 0.00000 0.00000 C14 1.01493 0.37663 0.14567 1.00000 0.05599 0.03226 0.02988 0.00390 0.00055 0.00750 0.03938 0.00906 0.00060 0.00052 0.00011 0.00000 0.00335 0.00255 0.00280 0.00202 0.00240 0.00242 0.00119 H14 0.97176 0.29831 0.15604 1.00000 0.04725 0.00000 0.00000 C15 0.94945 0.44031 0.12036 1.00000 0.03714 0.03378 0.03061 -0.00372 0.00139 -0.00065 0.03384 0.00832 0.00052 0.00051 0.00011 0.00000 0.00277 0.00269 0.00276 0.00200 0.00204 0.00202 0.00114 H15 0.86036 0.40523 0.11332 1.00000 0.04061 0.00000 0.00000 N1 0.75724 0.59964 0.07366 1.00000 0.02428 0.03294 0.03463 0.00128 -0.00042 -0.00556 0.03062 0.00627 0.00037 0.00041 0.00009 0.00000 0.00195 0.00206 0.00234 0.00177 0.00170 0.00154 0.00090 N2 1.00026 0.57270 0.03954 1.00000 0.02477 0.03180 0.02866 0.00179 -0.00237 -0.00106 0.02841 0.00612 0.00039 0.00039 0.00008 0.00000 0.00185 0.00195 0.00204 0.00159 0.00165 0.00160 0.00080 N3 0.75076 0.46738 0.01727 1.00000 0.04180 0.03381 0.03819 -0.00162 -0.00677 -0.01186 0.03793 0.00649 0.00044 0.00042 0.00010 0.00000 0.00249 0.00226 0.00253 0.00184 0.00189 0.00184 0.00102 N4 0.51278 0.55823 0.04324 1.00000 0.02899 0.03582 0.07550 0.01972 -0.01543 -0.00342 0.04677 0.00745 0.00044 0.00044 0.00011 0.00000 0.00220 0.00237 0.00328 0.00221 0.00230 0.00186 0.00120 H4 0.50679 0.64305 0.03464 1.00000 0.05612 0.00000 0.00000 O1 0.64054 0.35884 0.06916 1.00000 0.03226 0.03016 0.04183 0.00990 0.00243 -0.00366 0.03475 0.00561 0.00033 0.00034 0.00008 0.00000 0.00178 0.00176 0.00194 0.00159 0.00157 0.00133 0.00078 P1 0.67032 0.50033 0.05053 1.00000 0.02371 0.02814 0.03999 0.00601 -0.00565 -0.00294 0.03061 0.00211 0.00012 0.00013 0.00003 0.00000 0.00061 0.00064 0.00078 0.00056 0.00051 0.00050 0.00030 P2 0.92269 0.63178 0.07101 1.00000 0.02208 0.02772 0.02858 0.00122 -0.00035 -0.00194 0.02613 0.00193 0.00012 0.00012 0.00003 0.00000 0.00056 0.00059 0.00065 0.00049 0.00049 0.00045 0.00027 P3 0.90916 0.51146 0.01186 1.00000 0.03359 0.02360 0.02992 0.00248 -0.00130 -0.00068 0.02903 0.00206 0.00013 0.00013 0.00003 0.00000 0.00065 0.00057 0.00066 0.00048 0.00049 0.00048 0.00029 Cl1 0.91566 0.64381 -0.02570 1.00000 0.04831 0.03060 0.03505 0.00959 -0.00344 0.00119 0.03799 0.00219 0.00014 0.00012 0.00003 0.00000 0.00072 0.00062 0.00070 0.00051 0.00056 0.00052 0.00031 Cl2 1.01676 0.34489 -0.00662 1.00000 0.05607 0.02675 0.03923 0.00052 0.00589 0.00466 0.04068 0.00224 0.00015 0.00012 0.00003 0.00000 0.00081 0.00059 0.00073 0.00049 0.00058 0.00054 0.00033 Final Structure Factor Calculation for 2007src0260 in P4(1)2(1)2 Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 2567 / 27090 wR2 = 0.1695 before cycle 5 for 4159 data and 2 / 226 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0974 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0563 for 3248 Fo > 4sig(Fo) and 0.0886 for all 4159 data wR2 = 0.1695, GooF = S = 1.109, Restrained GooF = 1.109 for all data Flack x parameter = 0.1263 with esd 0.1392 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0607 0.0525 0.0231 C1 0.0700 0.0630 0.0229 C2 0.4228 0.0461 0.0290 C3 may be split into 0.3960 0.5094 0.0550 and 0.3907 0.4769 0.0425 0.0348 0.0284 0.0172 C4 0.0403 0.0320 0.0242 C5 0.0546 0.0361 0.0297 C6 0.0529 0.0292 0.0215 C7 0.0409 0.0343 0.0250 C8 0.0396 0.0321 0.0230 C9 0.0297 0.0280 0.0236 C10 0.0507 0.0395 0.0281 C11 0.0776 0.0421 0.0204 C12 0.0808 0.0316 0.0239 C13 0.0583 0.0335 0.0263 C14 0.0381 0.0353 0.0281 C15 0.0366 0.0337 0.0216 N1 0.0331 0.0285 0.0236 N2 0.0520 0.0385 0.0233 N3 0.0878 0.0293 0.0233 N4 0.0475 0.0342 0.0225 O1 0.0444 0.0257 0.0217 P1 0.0297 0.0272 0.0215 P2 0.0342 0.0302 0.0227 P3 0.0493 0.0421 0.0226 Cl1 0.0586 0.0374 0.0260 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.031 0.050 0.067 0.082 0.100 0.121 0.148 0.185 0.254 1.000 Number in group 433. 406. 421. 417. 407. 411. 422. 415. 414. 413. GooF 0.961 1.020 1.168 1.101 1.131 1.119 1.036 1.089 0.835 1.516 K 1.331 0.986 1.617 0.862 0.968 0.978 1.010 1.013 1.038 0.969 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.33 1.67 inf Number in group 422. 414. 414. 420. 416. 417. 409. 418. 413. 416. GooF 1.061 1.168 1.086 0.960 1.079 0.984 0.982 0.897 0.849 1.759 K 0.931 0.963 1.310 1.013 0.974 0.991 1.051 1.049 1.013 0.937 R1 0.224 0.206 0.178 0.104 0.112 0.083 0.054 0.042 0.031 0.053 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0970 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 1 3 -18.78 41457.66 14.28 1.000 6.02 1 1 0 0.00 14923.23 14.27 0.600 6.66 1 1 2 10.91 6625.36 14.24 0.400 6.35 4 6 40 306.94 1213.35 7.45 0.171 0.82 1 1 1 0.00 20.25 5.90 0.022 6.58 3 3 14 28.65 80.71 3.95 0.044 1.79 7 9 13 182.91 427.32 3.85 0.102 0.80 1 4 45 40773.39 141.35 3.82 0.058 0.87 7 9 12 186.36 420.71 3.81 0.101 0.80 5 10 9 54.49 261.55 3.56 0.079 0.83 3 4 0 217.56 339.09 3.55 0.090 1.88 1 9 32 1673.82 851.45 3.39 0.143 0.82 2 4 29 409.25 640.75 3.25 0.124 1.20 0 4 9 360.88 249.29 3.20 0.078 2.11 6 6 0 937.18 599.20 3.19 0.120 1.11 0 4 1 603.41 429.35 3.17 0.102 2.35 2 4 21 77.50 122.95 3.16 0.054 1.46 2 3 11 367.48 232.95 3.16 0.075 2.16 -5 8 17 90.03 290.52 3.14 0.084 0.93 5 9 15 -40.92 155.75 3.10 0.061 0.87 5 7 39 -73.66 184.35 3.04 0.067 0.77 5 8 32 28.65 236.91 3.04 0.076 0.80 3 3 22 83.93 133.61 2.97 0.057 1.45 -2 4 24 51.16 109.86 2.89 0.051 1.35 4 5 43 40.92 264.62 2.88 0.080 0.82 -2 9 35 -53.20 126.53 2.88 0.055 0.78 -4 10 10 394.45 672.56 2.88 0.127 0.86 0 3 22 83.69 160.74 2.88 0.062 1.64 -4 6 16 67.37 134.18 2.87 0.057 1.17 3 6 42 237.36 459.62 2.86 0.105 0.82 0 6 3 39.56 76.50 2.86 0.043 1.56 0 5 36 171.88 332.50 2.83 0.090 1.00 1 2 22 69.57 39.66 2.79 0.031 1.75 2 10 19 408.60 702.03 2.78 0.130 0.85 2 8 33 544.30 288.25 2.76 0.083 0.85 0 7 17 190.48 286.26 2.76 0.083 1.18 1 6 36 433.80 252.49 2.74 0.078 0.94 5 5 44 396.97 727.12 2.74 0.132 0.78 5 5 32 1064.05 691.01 2.74 0.129 0.94 -2 3 11 349.92 256.99 2.73 0.079 2.16 4 6 43 90.03 230.71 2.69 0.075 0.79 -2 6 45 155.51 350.88 2.69 0.092 0.80 0 3 13 192.35 135.68 2.66 0.057 2.26 0 3 7 118.68 85.47 2.65 0.045 2.79 -3 9 32 1305.50 848.50 2.65 0.143 0.79 1 5 36 257.83 67.66 2.64 0.040 0.99 0 3 16 523.84 392.06 2.63 0.097 2.02 -7 9 9 103.72 244.64 2.62 0.077 0.81 -3 8 8 153.91 83.60 2.62 0.045 1.08 1 12 1 365.87 162.05 2.61 0.063 0.78 Bond lengths and angles C1 - Distance Angles O1 1.4515 (0.0055) C2 1.5246 (0.0080) 110.35 (0.40) C1 - O1 C2 - Distance Angles C3 1.4817 (0.0096) C1 1.5246 (0.0080) 110.69 (0.50) C2 - C3 C3 - Distance Angles N4 1.3019 (0.0080) C2 1.4817 (0.0096) 123.86 (0.64) C3 - N4 C4 - Distance Angles C9 1.3902 (0.0063) C5 1.4068 (0.0064) 118.96 (0.41) P2 1.7944 (0.0045) 121.04 (0.35) 119.76 (0.34) C4 - C9 C5 C5 - Distance Angles C6 1.3821 (0.0069) C4 1.4068 (0.0064) 120.23 (0.47) C5 - C6 C6 - Distance Angles C5 1.3821 (0.0069) C7 1.3927 (0.0071) 120.16 (0.49) C6 - C5 C7 - Distance Angles C8 1.3590 (0.0065) C6 1.3927 (0.0071) 119.92 (0.42) C7 - C8 C8 - Distance Angles C7 1.3590 (0.0065) C9 1.4030 (0.0062) 121.04 (0.45) C8 - C7 C9 - Distance Angles C4 1.3902 (0.0063) C8 1.4030 (0.0062) 119.57 (0.43) C9 - C4 C10 - Distance Angles C15 1.3923 (0.0064) C11 1.3930 (0.0067) 119.48 (0.43) P2 1.8068 (0.0045) 119.56 (0.35) 120.88 (0.36) C10 - C15 C11 C11 - Distance Angles C10 1.3930 (0.0067) C12 1.4151 (0.0069) 118.96 (0.49) C11 - C10 C12 - Distance Angles C13 1.3768 (0.0083) C11 1.4151 (0.0069) 119.37 (0.50) C12 - C13 C13 - Distance Angles C14 1.3719 (0.0078) C12 1.3768 (0.0083) 121.76 (0.49) C13 - C14 C14 - Distance Angles C13 1.3719 (0.0078) C15 1.3742 (0.0068) 119.03 (0.49) C14 - C13 C15 - Distance Angles C14 1.3742 (0.0068) C10 1.3923 (0.0064) 121.38 (0.47) C15 - C14 N1 - Distance Angles P1 1.5827 (0.0037) P2 1.5915 (0.0037) 125.12 (0.25) N1 - P1 N2 - Distance Angles P3 1.5629 (0.0037) P2 1.6186 (0.0038) 119.77 (0.24) N2 - P3 N3 - Distance Angles P3 1.5657 (0.0042) P1 1.6291 (0.0044) 121.28 (0.25) N3 - P3 N4 - Distance Angles C3 1.3019 (0.0080) P1 1.6109 (0.0042) 127.05 (0.47) N4 - C3 O1 - Distance Angles C1 1.4515 (0.0055) P1 1.5740 (0.0033) 117.94 (0.31) O1 - C1 P1 - Distance Angles O1 1.5740 (0.0033) N1 1.5827 (0.0037) 106.41 (0.20) N4 1.6109 (0.0042) 102.62 (0.20) 113.26 (0.22) N3 1.6291 (0.0044) 110.78 (0.20) 114.02 (0.20) 109.11 (0.24) P1 - O1 N1 N4 P2 - Distance Angles N1 1.5915 (0.0037) N2 1.6186 (0.0038) 115.77 (0.20) C4 1.7944 (0.0045) 108.08 (0.20) 108.00 (0.21) C10 1.8068 (0.0045) 108.59 (0.21) 107.93 (0.19) 108.26 (0.21) P2 - N1 N2 C4 P3 - Distance Angles N2 1.5629 (0.0037) N3 1.5657 (0.0042) 120.76 (0.21) Cl1 2.0220 (0.0016) 110.23 (0.15) 107.91 (0.17) Cl2 2.0252 (0.0017) 107.52 (0.16) 109.15 (0.17) 99.12 (0.07) P3 - N2 N3 Cl1 Cl1 - Distance Angles P3 2.0220 (0.0016) Cl1 - Cl2 - Distance Angles P3 2.0252 (0.0017) Cl2 - FMAP and GRID set by program FMAP 2 3 25 GRID -0.568 -2 -2 0.568 2 2 R1 = 0.0790 for 2501 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.87 at 0.3845 0.4585 0.0386 [ 0.55 A from C3 ] Deepest hole -0.65 at 0.8656 0.6559 0.0597 [ 0.76 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.19 e/A^3, Highest memory used = 2410 / 18203 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3845 0.4585 0.0386 1.00000 0.05 0.87 0.55 C3 0.67 H3A 1.44 C2 1.45 H3B Q2 1 0.2934 0.5431 0.0418 1.00000 0.05 0.64 0.88 H3A 1.00 H3B 1.09 C3 2.07 N4 Q3 1 0.3973 0.5163 0.0635 1.00000 0.05 0.62 0.66 C3 0.67 H3B 1.44 N4 1.59 C2 Q4 1 0.3048 0.6535 0.0277 1.00000 0.05 0.54 1.57 H3A 1.78 H3B 1.93 H4 1.94 C3 Q5 1 0.4039 0.6398 0.0629 1.00000 0.05 0.52 1.01 H3B 1.51 C3 1.53 N4 1.54 H4 Q6 1 1.0664 0.7648 -0.0331 1.00000 0.05 0.51 1.85 CL1 2.31 C8 2.42 C7 2.59 H8 Q7 1 0.2990 0.6396 0.0503 1.00000 0.05 0.51 1.03 H3B 1.64 C3 1.73 H3A 2.07 H4 Q8 1 0.7970 1.0890 0.0568 1.00000 0.05 0.50 1.57 C7 1.95 H7 2.02 C6 2.02 C8 Q9 1 0.8584 1.1211 0.0848 1.00000 0.05 0.50 0.98 C6 1.02 C7 1.32 H6 1.36 H7 Q10 1 0.8244 1.0240 0.0443 1.00000 0.05 0.48 1.68 C8 1.86 C7 2.08 C9 2.13 CL1 Q11 1 0.7216 0.1206 0.0396 1.00000 0.05 0.46 2.08 H1B 2.15 CL1 2.38 H1A 2.47 C1 Q12 1 0.6284 0.1624 -0.0018 1.00000 0.05 0.46 1.97 H1B 2.27 N2 2.40 H3A 2.60 H9 Q13 1 0.2819 0.6166 0.0051 1.00000 0.05 0.46 1.64 H3A 1.93 H1B 2.36 N3 2.42 C3 Q14 1 0.9972 0.1997 0.1506 1.00000 0.05 0.46 0.99 H14 1.69 C14 2.19 H6 2.56 C13 Q15 1 0.3748 0.5822 0.0906 1.00000 0.05 0.46 1.24 H3B 1.97 C3 2.07 H11 2.17 H2B Q16 1 0.7377 0.1756 0.0233 1.00000 0.05 0.45 2.05 H1B 2.61 CL1 2.66 C1 2.74 H9 Q17 1 0.2222 0.5581 0.0217 1.00000 0.05 0.45 1.32 H3A 2.06 H3B 2.07 C3 2.23 N2 Q18 1 0.3922 0.5957 0.0847 1.00000 0.05 0.45 1.12 H3B 1.80 C3 2.12 N4 2.24 H11 Q19 1 1.1300 0.7612 -0.0117 1.00000 0.05 0.45 2.07 H9 2.38 CL1 2.57 H1B 2.73 H8 Q20 1 1.1205 0.7127 0.0056 1.00000 0.05 0.45 1.75 H9 2.26 N2 2.43 CL1 2.68 C9 Shortest distances between peaks (including symmetry equivalents) 15 18 0.32 16 19 0.69 6 11 0.71 6 10 0.84 8 10 0.85 19 20 0.87 11 16 0.88 12 20 0.90 4 7 0.97 2 7 0.98 5 18 1.02 4 13 1.04 13 17 1.05 8 11 1.06 6 8 1.07 6 19 1.08 2 17 1.09 5 7 1.12 6 16 1.14 12 13 1.14 3 5 1.16 3 18 1.17 1 2 1.18 1 3 1.19 2 4 1.20 12 17 1.21 4 17 1.22 11 19 1.24 3 15 1.32 5 15 1.32 10 11 1.34 16 20 1.35 8 9 1.35 2 3 1.37 12 19 1.41 12 16 1.49 14 18 1.56 3 7 1.59 7 17 1.61 2 5 1.65 14 15 1.68 2 13 1.70 8 16 1.73 4 12 1.75 7 18 1.75 4 5 1.76 13 20 1.77 6 20 1.79 10 19 1.80 10 16 1.87 17 20 1.87 5 14 1.89 11 20 1.92 7 15 1.93 1 17 1.93 7 13 1.93 13 16 1.94 1 7 1.95 9 10 1.97 8 19 1.98 11 12 2.00 1 5 2.00 1 4 2.04 4 20 2.05 2 18 2.10 13 19 2.10 6 12 2.16 3 4 2.17 2 15 2.23 2 12 2.24 1 13 2.27 9 11 2.31 1 18 2.34 6 9 2.42 7 12 2.42 3 17 2.45 1 15 2.49 3 14 2.51 10 20 2.53 17 19 2.53 4 19 2.56 5 17 2.56 16 17 2.59 4 16 2.60 4 18 2.61 7 20 2.62 11 13 2.62 5 13 2.71 2 20 2.75 8 20 2.78 4 15 2.82 3 13 2.86 7 14 2.89 9 16 2.89 6 13 2.95 10 12 2.99 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: 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 0.01: Analyse other restraints etc. 1.71: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.55: Structure factors and derivatives 2.34: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.53: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0260 finished at 22:44:11 Total CPU time: 9.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++