+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0567 started at 22:52:17 on 04-May-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0567 in Cc CELL 0.71073 14.8296 6.0926 15.4113 90.000 109.500 90.000 ZERR 4.00 0.0009 0.0003 0.0012 0.000 0.003 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O P CL UNIT 16 32 12 8 12 16 V = 1312.56 F(000) = 728.0 Mu = 1.25 mm-1 Cell Wt = 1459.38 Rho = 1.846 MERG 2 OMIT -3.00 55.00 OMIT -2 0 0 OMIT -1 1 3 OMIT -2 4 4 ISOR 0.01 C2 C4 FMAP 2 PLAN 10 SIZE 0.20 0.20 0.40 ACTA BOND WGHT 0.07170 17.65970 L.S. 4 TEMP -153.00 FVAR 0.38486 C1 1 1.095136 -0.781848 1.045226 11.00000 0.01427 0.01660 = 0.03483 -0.00668 0.01001 -0.00003 AFIX 23 H1A 2 1.108793 -0.940330 1.042703 11.00000 -1.20000 H1B 2 1.043267 -0.766410 1.071876 11.00000 -1.20000 AFIX 0 C2 1 1.184015 -0.667423 1.107255 11.00000 0.01046 0.00437 = 0.02114 0.00629 -0.00126 0.00049 AFIX 13 H2 2 1.237512 -0.691246 1.082403 11.00000 -1.20000 AFIX 0 C3 1 1.212809 -0.755974 1.203427 11.00000 0.02890 0.01321 = 0.00862 -0.00127 -0.00031 -0.00064 AFIX 137 H3A 2 1.277014 -0.703065 1.238697 11.00000 -1.50000 H3B 2 1.212995 -0.916750 1.201560 11.00000 -1.50000 H3C 2 1.167242 -0.705989 1.232890 11.00000 -1.50000 AFIX 0 C4 1 1.164383 -0.424172 1.108170 11.00000 0.01863 0.01995 = 0.01792 -0.00711 -0.00323 -0.00992 AFIX 23 H4A 2 1.112342 -0.399437 1.133912 11.00000 -1.20000 H4B 2 1.222398 -0.348721 1.148430 11.00000 -1.20000 AFIX 0 N1 3 1.040796 -0.365662 0.843642 11.00000 0.02063 0.03811 = 0.01955 0.00744 0.01551 0.00807 N2 3 0.855603 -0.223370 0.804323 11.00000 0.01615 0.02791 = 0.01306 0.00060 0.00643 0.01079 N3 3 0.953352 -0.379996 0.974994 11.00000 0.01899 0.02909 = 0.02389 0.00150 0.01042 0.01090 O1 4 1.063023 -0.693999 0.952890 11.00000 0.02161 0.01460 = 0.00846 0.00395 0.00364 0.00045 O2 4 1.136377 -0.328822 1.013722 11.00000 0.01697 0.01196 = 0.03078 0.00450 0.00288 -0.00627 P1 5 1.044047 -0.438137 0.943521 11.00000 0.01221 0.01828 = 0.01225 0.00102 0.00269 0.00466 P2 5 0.948444 -0.254524 0.774442 11.00000 0.01374 0.02416 = 0.01100 0.00130 0.00415 0.00522 P3 5 0.862245 -0.263305 0.906485 11.00000 0.01183 0.02248 = 0.00912 0.00125 0.00142 0.00440 CL1 6 0.908713 -0.422767 0.655513 11.00000 0.02885 0.02687 = 0.01164 -0.00495 0.00815 -0.00076 CL2 6 0.984155 0.034632 0.733277 11.00000 0.03056 0.02030 = 0.02320 0.00322 0.00614 -0.00238 CL3 6 0.841583 0.022907 0.960656 11.00000 0.02530 0.01999 = 0.02096 -0.00231 0.00811 -0.00078 CL4 6 0.746063 -0.429735 0.905326 11.00000 0.01695 0.02987 = 0.02515 -0.00701 0.00817 -0.00472 HKLF 4 Covalent radii and connectivity table for 2006src0567 in Cc C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3 C4 C1 C3 - C2 C4 - O2 C2 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C4 P1 P1 - O2 O1 N1 N3 P2 - N1 N2 Cl2 Cl1 P3 - N2 N3 Cl4 Cl3 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Floating origin restraints generated h k l Fo^2 Sigma Why rejected -12 0 -3 115.21 27.12 observed but should be systematically absent 2151 Reflections read, of which 108 rejected -19 =< h =< 17, -7 =< k =< 7, -18 =< l =< 18, Max. 2-theta = 55.00 1 Systematic absence violations 0 Inconsistent equivalents 1519 Unique reflections, of which 0 suppressed R(int) = 0.0445 R(sigma) = 0.0948 Friedel opposites not merged Maximum memory for data reduction = 1382 / 22890 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 = 1759 / 185274 wR2 = 0.1817 before cycle 1 for 1519 data and 146 / 146 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.165; Restrained GooF = 1.161 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0717 * P )^2 + 17.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38492 0.00192 0.030 OSF Mean shift/esd = 0.009 Maximum = 0.038 for y O2 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1759 / 185274 wR2 = 0.1817 before cycle 2 for 1519 data and 146 / 146 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.165; Restrained GooF = 1.161 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0717 * P )^2 + 17.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38493 0.00192 0.007 OSF Mean shift/esd = 0.003 Maximum = 0.013 for y O2 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1759 / 185274 wR2 = 0.1817 before cycle 3 for 1519 data and 146 / 146 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.165; Restrained GooF = 1.161 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0717 * P )^2 + 17.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38493 0.00192 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U22 N1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for N1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1759 / 185274 wR2 = 0.1817 before cycle 4 for 1519 data and 146 / 146 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.165; Restrained GooF = 1.161 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0717 * P )^2 + 17.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38493 0.00192 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U12 C1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for N1 Largest correlation matrix elements 0.603 U13 Cl1 / U33 Cl1 0.562 U13 P2 / U33 P2 0.515 U13 N3 / U11 N3 0.600 U13 N1 / U33 N1 0.553 U13 Cl4 / U33 Cl4 0.507 U13 Cl4 / U11 Cl4 0.598 U13 C1 / U33 C1 0.548 U13 N3 / U33 N3 0.501 U13 P1 / U33 P1 0.568 U13 N2 / U33 N2 0.540 U13 O1 / U33 O1 0.568 U13 Cl3 / U33 Cl3 0.518 U13 N1 / U11 N1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 1.1088 -0.9403 1.0427 23 0.990 0.000 C1 O1 C2 H1B 1.0433 -0.7663 1.0719 23 0.990 0.000 C1 O1 C2 H2 1.2375 -0.6913 1.0824 13 1.000 0.000 C2 C3 C4 C1 H3A 1.2770 -0.7031 1.2387 137 0.980 0.000 C3 C2 H3A H3B 1.2130 -0.9168 1.2016 137 0.980 0.000 C3 C2 H3A H3C 1.1673 -0.7060 1.2329 137 0.980 0.000 C3 C2 H3A H4A 1.1124 -0.3994 1.1339 23 0.990 0.000 C4 O2 C2 H4B 1.2224 -0.3488 1.1484 23 0.990 0.000 C4 O2 C2 2006src0567 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.09515 -0.78182 1.04525 1.00000 0.01415 0.01657 0.03462 -0.00661 0.01002 -0.00012 0.02131 0.02594 0.00080 0.00208 0.00108 0.00000 0.00615 0.00651 0.01097 0.00653 0.00692 0.00525 0.00333 H1A 1.10880 -0.94031 1.04274 1.00000 0.02557 0.00000 0.00000 H1B 1.04328 -0.76635 1.07190 1.00000 0.02557 0.00000 0.00000 C2 1.18400 -0.66743 1.10725 1.00000 0.01053 0.00446 0.02129 0.00627 -0.00107 0.00056 0.01369 0.02451 0.00076 0.00177 0.00097 0.00000 0.00492 0.00449 0.00717 0.00458 0.00489 0.00385 0.00280 H2 1.23750 -0.69127 1.08240 1.00000 0.01643 0.00000 0.00000 C3 1.21281 -0.75600 1.20344 1.00000 0.02894 0.01328 0.00874 -0.00132 -0.00018 -0.00054 0.01861 0.02582 0.00092 0.00208 0.00100 0.00000 0.00708 0.00634 0.00851 0.00515 0.00636 0.00502 0.00306 H3A 1.27703 -0.70313 1.23870 1.00000 0.02791 0.00000 0.00000 H3B 1.21298 -0.91677 1.20157 1.00000 0.02791 0.00000 0.00000 H3C 1.16726 -0.70598 1.23291 1.00000 0.02791 0.00000 0.00000 C4 1.16440 -0.42419 1.10819 1.00000 0.01872 0.02006 0.01799 -0.00707 -0.00314 -0.00992 0.02124 0.02544 0.00092 0.00208 0.00103 0.00000 0.00516 0.00542 0.00713 0.00503 0.00502 0.00464 0.00302 H4A 1.11237 -0.39944 1.13395 1.00000 0.02549 0.00000 0.00000 H4B 1.22243 -0.34877 1.14844 1.00000 0.02549 0.00000 0.00000 N1 1.04080 -0.36557 0.84366 1.00000 0.02059 0.03806 0.01972 0.00747 0.01547 0.00800 0.02393 0.02505 0.00072 0.00206 0.00086 0.00000 0.00550 0.00702 0.00787 0.00553 0.00547 0.00478 0.00279 N2 0.85559 -0.22337 0.80431 1.00000 0.01611 0.02795 0.01300 0.00056 0.00635 0.01070 0.01864 0.02173 0.00066 0.00177 0.00083 0.00000 0.00510 0.00563 0.00749 0.00512 0.00507 0.00450 0.00252 N3 0.95336 -0.37997 0.97500 1.00000 0.01901 0.02915 0.02373 0.00163 0.01030 0.01085 0.02317 0.02389 0.00073 0.00182 0.00089 0.00000 0.00518 0.00595 0.00783 0.00546 0.00540 0.00471 0.00266 O1 1.06303 -0.69399 0.95289 1.00000 0.02166 0.01455 0.00863 0.00390 0.00367 0.00041 0.01529 0.01718 0.00056 0.00138 0.00064 0.00000 0.00445 0.00405 0.00573 0.00368 0.00414 0.00352 0.00196 O2 1.13637 -0.32875 1.01374 1.00000 0.01693 0.01199 0.03074 0.00445 0.00283 -0.00626 0.02117 0.01707 0.00056 0.00132 0.00069 0.00000 0.00423 0.00396 0.00718 0.00403 0.00457 0.00333 0.00237 P1 1.04404 -0.43813 0.94352 1.00000 0.01221 0.01824 0.01223 0.00101 0.00268 0.00463 0.01458 0.00669 0.00021 0.00054 0.00025 0.00000 0.00136 0.00151 0.00206 0.00139 0.00139 0.00120 0.00074 P2 0.94844 -0.25454 0.77444 1.00000 0.01374 0.02415 0.01104 0.00128 0.00416 0.00520 0.01631 0.00695 0.00022 0.00058 0.00026 0.00000 0.00144 0.00176 0.00219 0.00144 0.00146 0.00130 0.00080 P3 0.86224 -0.26329 0.90648 1.00000 0.01186 0.02251 0.00916 0.00126 0.00145 0.00439 0.01502 0.00657 0.00020 0.00056 0.00025 0.00000 0.00144 0.00173 0.00214 0.00150 0.00138 0.00122 0.00079 Cl1 0.90871 -0.42277 0.65551 1.00000 0.02883 0.02689 0.01164 -0.00488 0.00812 -0.00073 0.02211 0.00654 0.00022 0.00054 0.00025 0.00000 0.00155 0.00166 0.00203 0.00144 0.00146 0.00141 0.00076 Cl2 0.98416 0.03465 0.73328 1.00000 0.03056 0.02035 0.02319 0.00322 0.00613 -0.00240 0.02542 0.00684 0.00022 0.00055 0.00027 0.00000 0.00175 0.00175 0.00229 0.00150 0.00158 0.00135 0.00085 Cl3 0.84159 0.02289 0.96065 1.00000 0.02531 0.01995 0.02094 -0.00232 0.00809 -0.00077 0.02197 0.00643 0.00021 0.00053 0.00025 0.00000 0.00162 0.00172 0.00229 0.00144 0.00160 0.00133 0.00082 Cl4 0.74607 -0.42973 0.90533 1.00000 0.01694 0.02986 0.02513 -0.00701 0.00816 -0.00473 0.02369 0.00634 0.00020 0.00056 0.00026 0.00000 0.00143 0.00183 0.00237 0.00148 0.00148 0.00133 0.00085 Final Structure Factor Calculation for 2006src0567 in Cc Total number of l.s. parameters = 146 Maximum vector length = 511 Memory required = 1615 / 27090 wR2 = 0.1817 before cycle 5 for 1519 data and 2 / 146 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.165; Restrained GooF = 1.161 for 14 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0717 * P )^2 + 17.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0658 for 1242 Fo > 4sig(Fo) and 0.0961 for all 1519 data wR2 = 0.1817, GooF = S = 1.165, Restrained GooF = 1.161 for all data Flack x parameter = 0.3649 with esd 0.2964 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 Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0370 0.0153 0.0116 C1 0.0290 0.0099 0.0022 C2 0.0342 0.0136 0.0080 C3 0.0331 0.0262 0.0044 C4 0.0434 0.0213 0.0070 N1 0.0345 0.0134 0.0081 N2 0.0361 0.0233 0.0101 N3 0.0228 0.0164 0.0066 O1 0.0376 0.0188 0.0071 O2 0.0209 0.0134 0.0094 P1 0.0263 0.0117 0.0109 P2 0.0242 0.0129 0.0080 P3 0.0291 0.0282 0.0091 Cl1 0.0343 0.0240 0.0179 Cl2 0.0254 0.0225 0.0180 Cl3 0.0351 0.0207 0.0153 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.037 0.055 0.074 0.091 0.108 0.130 0.157 0.192 0.250 1.000 Number in group 156. 149. 152. 150. 153. 151. 152. 153. 150. 153. GooF 1.161 1.219 1.353 1.438 1.264 0.860 0.997 1.010 0.995 1.222 K 1.894 1.212 1.117 0.964 1.021 1.014 1.007 1.010 1.019 0.952 Resolution(A) 0.77 0.82 0.87 0.93 0.99 1.06 1.14 1.25 1.45 1.82 inf Number in group 153. 152. 152. 153. 154. 151. 149. 154. 148. 153. GooF 1.489 1.427 1.254 1.186 1.234 0.925 1.035 1.059 0.733 1.092 K 1.054 1.015 1.022 1.036 0.965 1.010 1.007 1.019 1.029 0.931 R1 0.254 0.189 0.140 0.123 0.098 0.067 0.057 0.044 0.036 0.046 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0723 17.6160 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) -11 1 6 2078.65 6874.37 7.47 0.264 1.29 -9 1 11 2518.55 5996.70 6.07 0.247 1.20 -7 5 4 168.25 978.05 5.34 0.100 1.05 4 0 -2 61465.26 98377.74 5.04 1.000 3.66 14 2 -6 1405.93 2994.87 4.79 0.174 1.00 1 7 1 1353.76 3190.08 4.76 0.180 0.87 -14 4 5 91.18 2009.01 4.53 0.143 0.87 -4 0 2 67480.87 97787.81 3.96 0.997 3.66 -5 7 8 3214.29 598.13 3.89 0.078 0.79 -9 5 12 -216.64 545.14 3.81 0.074 0.84 -6 4 9 460.95 1141.11 3.63 0.108 1.10 -8 4 -10 -456.97 818.30 3.51 0.091 0.82 4 6 6 -348.04 606.98 3.47 0.079 0.88 -5 3 -12 -326.38 556.71 3.41 0.075 0.89 -4 4 -10 1987.14 457.31 3.23 0.068 0.95 -1 1 1 6865.90 10108.63 3.17 0.321 5.46 -9 5 11 2168.14 782.37 3.13 0.089 0.87 -9 3 13 76.53 554.21 3.13 0.075 0.97 -3 7 9 1318.26 8.43 3.08 0.009 0.78 -2 2 3 6857.13 9815.43 3.05 0.316 2.57 -6 6 7 1117.48 69.05 3.04 0.026 0.90 -10 2 -6 -382.56 495.56 2.97 0.071 1.01 -11 5 13 -579.66 709.03 2.92 0.085 0.78 -6 4 6 848.33 189.80 2.86 0.044 1.22 5 1 -16 981.56 2016.16 2.84 0.143 0.95 -5 5 8 -243.90 433.22 2.83 0.066 1.01 -13 3 13 -349.66 671.42 2.80 0.083 0.86 -13 5 8 1263.66 143.60 2.76 0.038 0.82 -2 6 5 -122.09 551.17 2.71 0.075 0.96 -14 4 12 2648.73 1540.97 2.69 0.125 0.80 -4 6 8 1025.29 237.72 2.67 0.049 0.89 -1 7 5 -282.74 301.63 2.66 0.055 0.84 -7 1 -11 2340.98 851.11 2.65 0.093 0.95 -2 2 13 673.13 148.25 2.59 0.039 1.09 -11 5 -6 1614.74 370.88 2.54 0.061 0.77 -12 4 -7 -300.66 656.80 2.54 0.082 0.77 -13 5 -2 -317.40 565.00 2.52 0.076 0.78 -14 4 13 286.15 912.88 2.50 0.096 0.78 -8 4 -7 1531.99 509.95 2.49 0.072 0.92 3 3 -8 600.04 201.48 2.47 0.045 1.40 -14 4 6 1148.32 135.93 2.47 0.037 0.87 -16 0 2 252.61 708.25 2.45 0.085 0.90 -14 2 -2 4274.13 2905.66 2.38 0.172 0.90 -11 5 6 1521.53 330.37 2.36 0.058 0.90 -14 4 0 12.49 694.35 2.31 0.084 0.84 3 1 -6 2803.69 2103.94 2.30 0.146 2.33 -11 5 10 1080.97 346.78 2.29 0.059 0.84 -4 6 5 378.21 888.69 2.29 0.095 0.95 -2 2 14 1175.38 2296.72 2.29 0.153 1.02 3 5 -2 884.24 1372.87 2.29 0.118 1.18 Bond lengths and angles C1 - Distance Angles O1 1.4445 (0.0180) C2 1.5148 (0.0171) 112.48 (1.04) C1 - O1 C2 - Distance Angles C3 1.4994 (0.0193) C4 1.5112 (0.0163) 109.62 (1.17) C1 1.5148 (0.0171) 111.03 (1.03) 109.12 (0.99) C2 - C3 C4 C3 - Distance Angles C2 1.4994 (0.0193) C3 - C4 - Distance Angles O2 1.4919 (0.0177) C2 1.5112 (0.0162) 111.39 (1.14) C4 - O2 N1 - Distance Angles P2 1.5798 (0.0117) P1 1.5864 (0.0125) 120.87 (0.62) N1 - P2 N2 - Distance Angles P3 1.5635 (0.0123) P2 1.6023 (0.0099) 119.97 (0.65) N2 - P3 N3 - Distance Angles P3 1.5791 (0.0112) P1 1.6140 (0.0109) 120.71 (0.82) N3 - P3 O1 - Distance Angles C1 1.4445 (0.0180) P1 1.5821 (0.0088) 116.43 (0.80) O1 - C1 O2 - Distance Angles C4 1.4919 (0.0177) P1 1.5813 (0.0088) 113.52 (0.71) O2 - C4 P1 - Distance Angles O2 1.5813 (0.0089) O1 1.5821 (0.0089) 105.41 (0.45) N1 1.5864 (0.0125) 106.58 (0.59) 108.06 (0.61) N3 1.6140 (0.0109) 108.65 (0.61) 109.25 (0.54) 118.16 (0.60) P1 - O2 O1 N1 P2 - Distance Angles N1 1.5798 (0.0117) N2 1.6023 (0.0099) 119.42 (0.61) Cl2 2.0029 (0.0048) 109.22 (0.48) 109.28 (0.45) Cl1 2.0091 (0.0053) 108.77 (0.50) 107.70 (0.45) 100.83 (0.23) P2 - N1 N2 Cl2 P3 - Distance Angles N2 1.5635 (0.0124) N3 1.5791 (0.0112) 119.72 (0.58) Cl4 1.9941 (0.0044) 107.83 (0.42) 108.72 (0.47) Cl3 2.0004 (0.0049) 108.52 (0.45) 109.23 (0.49) 101.23 (0.19) P3 - N2 N3 Cl4 Cl1 - Distance Angles P2 2.0091 (0.0053) Cl1 - Cl2 - Distance Angles P2 2.0029 (0.0048) Cl2 - Cl3 - Distance Angles P3 2.0004 (0.0049) Cl3 - Cl4 - Distance Angles P3 1.9941 (0.0044) Cl4 - FMAP and GRID set by program FMAP 2 2 32 GRID -3.448 -1 -1 3.448 1 1 R1 = 0.1059 for 1171 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.79 at 0.1315 0.4466 0.3638 [ 1.37 A from N1 ] Deepest hole -0.87 at 0.4135 0.5084 0.0986 [ 2.01 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 2129 / 39027 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1315 -0.4466 0.8638 1.00000 0.05 0.79 1.37 N1 2.06 P1 2.40 O2 2.44 H3C Q2 1 0.8791 -0.0166 0.6793 1.00000 0.05 0.79 1.53 CL2 2.07 P2 2.36 H4B 2.42 H3A Q3 1 1.2808 -0.4163 1.0879 1.00000 0.05 0.78 1.53 H4B 1.79 H2 1.85 C4 2.13 O2 Q4 1 0.6863 -0.5821 0.8722 1.00000 0.05 0.78 1.27 CL4 2.44 H3C 2.68 N1 2.79 H3B Q5 1 0.9522 -0.6455 0.8786 1.00000 0.05 0.74 1.69 O1 1.88 P1 2.19 N3 2.32 N1 Q6 1 0.8935 0.0540 0.9681 1.00000 0.05 0.73 0.76 CL3 2.14 P3 2.51 H1B 2.78 N3 Q7 1 0.9975 -0.6207 1.0188 1.00000 0.05 0.72 1.24 H1B 1.66 N3 1.68 C1 1.68 O1 Q8 1 0.9405 -0.6496 0.9730 1.00000 0.05 0.71 1.65 N3 1.90 H1B 1.96 O1 2.17 P1 Q9 1 0.9373 -0.7377 0.9187 1.00000 0.05 0.68 1.78 O1 2.27 CL3 2.33 N3 2.36 P1 Q10 1 1.1532 -0.6648 0.8811 1.00000 0.05 0.64 2.01 O1 2.07 CL4 2.41 N1 2.55 P1 Shortest distances between peaks (including symmetry equivalents) 5 9 0.91 7 8 0.92 8 9 0.98 1 10 1.37 5 8 1.52 7 9 1.66 2 3 1.70 6 9 1.71 6 8 1.93 5 7 2.04 1 4 2.35 6 7 2.47 4 10 2.60 5 6 2.61 3 6 2.88 5 10 2.97 1 5 3.00 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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 0.01: Analyse other restraints etc. 0.45: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.42: Structure factors and derivatives 0.44: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0567 finished at 22:52:20 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++