+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0194 started at 20:56:20 on 07-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0194 in P2(1)/c CELL 0.71073 6.0475 27.1376 10.4986 90.000 96.177 90.000 ZERR 4.00 0.0004 0.0015 0.0007 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F P CL UNIT 24 16 12 8 32 12 16 V = 1712.97 F(000) = 1048.0 Mu = 1.06 mm-1 Cell Wt = 2147.33 Rho = 2.082 MERG 2 OMIT -3.00 55.00 OMIT 0 3 1 OMIT 1 2 11 FMAP 2 PLAN 20 SIZE 0.02 0.06 0.10 ACTA BOND WGHT 0.02050 9.73780 L.S. 4 TEMP -153.00 FVAR 0.48998 C1 1 0.633403 0.697668 0.342022 11.00000 0.04504 0.03017 = 0.02746 -0.00480 0.00949 -0.00036 AFIX 23 H1A 2 0.504919 0.676196 0.353994 11.00000 -1.20000 H1B 2 0.610447 0.729759 0.383478 11.00000 -1.20000 AFIX 0 C2 1 0.846444 0.673977 0.403410 11.00000 0.03307 0.03993 = 0.02526 -0.00654 0.00786 -0.01240 C3 1 0.904587 0.620132 0.367884 11.00000 0.02102 0.04805 = 0.03033 -0.00296 0.00590 0.00026 C4 1 0.765346 0.579686 0.428035 11.00000 0.03343 0.04345 = 0.02992 0.00468 0.00800 0.00815 C5 1 0.748170 0.528363 0.358271 11.00000 0.03181 0.03185 = 0.04251 0.00544 0.00799 0.00825 C6 1 0.557080 0.520512 0.254025 11.00000 0.03967 0.02600 = 0.02692 0.00370 0.00794 0.00032 AFIX 23 H6A 2 0.531440 0.484748 0.241015 11.00000 -1.20000 H6B 2 0.419763 0.535156 0.281223 11.00000 -1.20000 AFIX 0 N1 3 0.407787 0.627444 0.145518 11.00000 0.02920 0.02221 = 0.02512 0.00152 0.00924 0.00020 N2 3 0.544515 0.589052 -0.071633 11.00000 0.03874 0.02513 = 0.02688 -0.00353 0.00953 0.00283 N3 3 0.563875 0.687892 -0.030975 11.00000 0.04811 0.02568 = 0.02954 0.00298 0.01578 -0.00322 O1 4 0.648460 0.704925 0.207037 11.00000 0.03962 0.02707 = 0.02953 -0.00389 0.00676 -0.00995 O2 4 0.603924 0.542492 0.136258 11.00000 0.03346 0.02623 = 0.03179 0.00234 0.01194 0.00565 F1 5 1.022324 0.701079 0.373547 11.00000 0.04214 0.06116 = 0.04350 -0.01059 0.00820 -0.02542 F2 5 0.843519 0.676506 0.531848 11.00000 0.04779 0.05463 = 0.03036 -0.00651 0.00693 -0.00778 F3 5 0.884498 0.615103 0.238739 11.00000 0.02909 0.04019 = 0.02961 0.00026 0.01103 0.00017 F4 5 1.119252 0.611456 0.411154 11.00000 0.02494 0.07471 = 0.04929 0.00260 0.00238 0.00207 F5 5 0.556576 0.596700 0.433934 11.00000 0.02612 0.03566 = 0.03848 0.00383 0.01372 0.00584 F6 5 0.855694 0.572981 0.549933 11.00000 0.04903 0.05794 = 0.02745 0.00389 0.00386 0.00917 F7 5 0.945995 0.517911 0.316318 11.00000 0.03710 0.04849 = 0.04557 0.00875 0.01335 0.01608 F8 5 0.717619 0.495235 0.451786 11.00000 0.05767 0.04277 = 0.03785 0.01121 0.00921 0.01342 P1 6 0.471373 0.681229 0.103531 11.00000 0.03387 0.01968 = 0.02829 0.00119 0.00941 -0.00071 P2 6 0.445859 0.581069 0.061078 11.00000 0.02736 0.02090 = 0.02748 -0.00025 0.00743 -0.00133 P3 6 0.596394 0.642294 -0.120098 11.00000 0.02846 0.02977 = 0.02586 0.00176 0.00892 -0.00091 CL1 7 0.206584 0.724532 0.108181 11.00000 0.04810 0.03140 = 0.04495 0.00381 0.01025 0.01377 CL2 7 0.157225 0.545642 0.031739 11.00000 0.03365 0.03187 = 0.04899 -0.00527 0.00674 -0.00991 CL3 7 0.418548 0.652857 -0.289538 11.00000 0.03165 0.05077 = 0.03066 0.00472 0.00680 0.00302 CL4 7 0.904528 0.644212 -0.169999 11.00000 0.02653 0.06198 = 0.03777 0.00604 0.00961 -0.00128 HKLF 4 Covalent radii and connectivity table for 2007src0194 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 CL 0.990 C1 - O1 C2 C2 - F2 F1 C1 C3 C3 - F4 F3 C2 C4 C4 - F6 F5 C3 C5 C5 - F7 F8 C6 C4 C6 - O2 C5 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C6 P2 F1 - C2 F2 - C2 F3 - C3 F4 - C3 F5 - C4 F6 - C4 F7 - C5 F8 - C5 P1 - O1 N1 N3 Cl1 P2 - N1 O2 N2 Cl2 P3 - N2 N3 Cl4 Cl3 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 h k l Fo^2 Sigma Why rejected -3 0 3 20.23 4.79 observed but should be systematically absent 4 0 3 11.09 2.72 observed but should be systematically absent 0 0 7 19.97 3.88 observed but should be systematically absent 0 0 7 27.28 6.32 observed but should be systematically absent 17520 Reflections read, of which 323 rejected -7 =< h =< 7, -35 =< k =< 35, -12 =< l =< 13, Max. 2-theta = 54.99 4 Systematic absence violations 0 Inconsistent equivalents 3849 Unique reflections, of which 0 suppressed R(int) = 0.0523 R(sigma) = 0.0441 Friedel opposites merged Maximum memory for data reduction = 1729 / 37970 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 = 2294 / 294431 wR2 = 0.1382 before cycle 1 for 3849 data and 235 / 235 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0205 * P )^2 + 9.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48999 0.00102 0.014 OSF Mean shift/esd = 0.006 Maximum = 0.022 for U22 F4 Max. shift = 0.000 A for C2 Max. dU = 0.000 for F4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2294 / 294431 wR2 = 0.1381 before cycle 2 for 3849 data and 235 / 235 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0205 * P )^2 + 9.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48999 0.00102 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.009 for U22 F4 Max. shift = 0.000 A for C2 Max. dU = 0.000 for F4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2294 / 294431 wR2 = 0.1381 before cycle 3 for 3849 data and 235 / 235 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0205 * P )^2 + 9.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49000 0.00102 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U22 F4 Max. shift = 0.000 A for N2 Max. dU = 0.000 for F4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2294 / 294431 wR2 = 0.1381 before cycle 4 for 3849 data and 235 / 235 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0205 * P )^2 + 9.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49000 0.00102 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y P2 Max. shift = 0.000 A for N3 Max. dU = 0.000 for F8 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5049 0.6762 0.3540 23 0.990 0.000 C1 O1 C2 H1B 0.6104 0.7298 0.3835 23 0.990 0.000 C1 O1 C2 H6A 0.5315 0.4847 0.2410 23 0.990 0.000 C6 O2 C5 H6B 0.4198 0.5352 0.2812 23 0.990 0.000 C6 O2 C5 2007src0194 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.63340 0.69767 0.34202 1.00000 0.04505 0.03017 0.02745 -0.00479 0.00951 -0.00037 0.03381 0.00931 0.00088 0.00018 0.00047 0.00000 0.00291 0.00243 0.00256 0.00194 0.00220 0.00211 0.00110 H1A 0.50492 0.67620 0.35399 1.00000 0.04058 0.00000 0.00000 H1B 0.61045 0.72976 0.38348 1.00000 0.04058 0.00000 0.00000 C2 0.84646 0.67398 0.40341 1.00000 0.03307 0.03994 0.02525 -0.00652 0.00785 -0.01241 0.03241 0.00855 0.00082 0.00019 0.00046 0.00000 0.00251 0.00269 0.00245 0.00201 0.00201 0.00207 0.00107 C3 0.90457 0.62013 0.36789 1.00000 0.02101 0.04809 0.03031 -0.00295 0.00589 0.00026 0.03291 0.00911 0.00077 0.00020 0.00048 0.00000 0.00216 0.00292 0.00264 0.00217 0.00195 0.00201 0.00108 C4 0.76535 0.57969 0.42803 1.00000 0.03340 0.04348 0.02994 0.00468 0.00799 0.00814 0.03527 0.01004 0.00084 0.00020 0.00049 0.00000 0.00257 0.00284 0.00261 0.00216 0.00211 0.00219 0.00112 C5 0.74818 0.52837 0.35827 1.00000 0.03180 0.03183 0.04253 0.00544 0.00799 0.00825 0.03510 0.00995 0.00083 0.00018 0.00052 0.00000 0.00251 0.00249 0.00302 0.00217 0.00223 0.00202 0.00112 C6 0.55708 0.52051 0.25402 1.00000 0.03965 0.02601 0.02691 0.00370 0.00792 0.00032 0.03054 0.00902 0.00084 0.00017 0.00045 0.00000 0.00266 0.00225 0.00245 0.00186 0.00208 0.00196 0.00102 H6A 0.53146 0.48475 0.24101 1.00000 0.03665 0.00000 0.00000 H6B 0.41976 0.53515 0.28122 1.00000 0.03665 0.00000 0.00000 N1 0.40780 0.62744 0.14551 1.00000 0.02916 0.02222 0.02509 0.00152 0.00920 0.00021 0.02504 0.00694 0.00063 0.00013 0.00036 0.00000 0.00194 0.00179 0.00198 0.00145 0.00161 0.00148 0.00080 N2 0.54452 0.58905 -0.07164 1.00000 0.03873 0.02514 0.02684 -0.00354 0.00951 0.00283 0.02980 0.00732 0.00069 0.00014 0.00038 0.00000 0.00223 0.00191 0.00207 0.00156 0.00175 0.00165 0.00087 N3 0.56386 0.68789 -0.03098 1.00000 0.04807 0.02569 0.02953 0.00300 0.01575 -0.00321 0.03359 0.00791 0.00075 0.00014 0.00039 0.00000 0.00252 0.00197 0.00222 0.00162 0.00192 0.00176 0.00095 O1 0.64846 0.70493 0.20704 1.00000 0.03959 0.02708 0.02950 -0.00389 0.00673 -0.00995 0.03184 0.00583 0.00057 0.00012 0.00032 0.00000 0.00190 0.00163 0.00181 0.00136 0.00150 0.00143 0.00075 O2 0.60392 0.54249 0.13626 1.00000 0.03346 0.02623 0.03180 0.00236 0.01194 0.00566 0.02988 0.00621 0.00054 0.00011 0.00032 0.00000 0.00172 0.00159 0.00182 0.00134 0.00144 0.00135 0.00072 F1 1.02233 0.70108 0.37355 1.00000 0.04212 0.06121 0.04346 -0.01061 0.00818 -0.02543 0.04867 0.00543 0.00053 0.00013 0.00031 0.00000 0.00176 0.00209 0.00192 0.00158 0.00148 0.00157 0.00084 F2 0.84352 0.67651 0.53185 1.00000 0.04777 0.05467 0.03034 -0.00650 0.00694 -0.00778 0.04406 0.00555 0.00053 0.00012 0.00029 0.00000 0.00184 0.00191 0.00162 0.00140 0.00140 0.00152 0.00075 F3 0.88450 0.61510 0.23874 1.00000 0.02907 0.04023 0.02957 0.00026 0.01101 0.00016 0.03238 0.00513 0.00044 0.00010 0.00026 0.00000 0.00140 0.00154 0.00149 0.00119 0.00117 0.00116 0.00062 F4 1.11925 0.61146 0.41115 1.00000 0.02491 0.07479 0.04929 0.00260 0.00236 0.00209 0.04978 0.00619 0.00049 0.00014 0.00033 0.00000 0.00148 0.00236 0.00203 0.00173 0.00139 0.00150 0.00085 F5 0.55658 0.59670 0.43393 1.00000 0.02610 0.03567 0.03848 0.00383 0.01373 0.00585 0.03268 0.00529 0.00044 0.00010 0.00027 0.00000 0.00134 0.00145 0.00159 0.00122 0.00120 0.00113 0.00063 F6 0.85570 0.57298 0.54994 1.00000 0.04901 0.05799 0.02744 0.00389 0.00385 0.00918 0.04483 0.00604 0.00054 0.00012 0.00028 0.00000 0.00185 0.00198 0.00158 0.00141 0.00138 0.00155 0.00077 F7 0.94599 0.51791 0.31631 1.00000 0.03710 0.04853 0.04556 0.00874 0.01335 0.01609 0.04308 0.00621 0.00050 0.00012 0.00030 0.00000 0.00163 0.00182 0.00187 0.00146 0.00142 0.00138 0.00076 F8 0.71761 0.49523 0.45178 1.00000 0.05765 0.04280 0.03784 0.01122 0.00920 0.01342 0.04580 0.00637 0.00057 0.00012 0.00030 0.00000 0.00201 0.00173 0.00178 0.00140 0.00153 0.00151 0.00079 P1 0.47137 0.68123 0.10353 1.00000 0.03387 0.01969 0.02829 0.00118 0.00941 -0.00071 0.02684 0.00227 0.00021 0.00004 0.00012 0.00000 0.00063 0.00053 0.00063 0.00045 0.00051 0.00046 0.00027 P2 0.44586 0.58107 0.06108 1.00000 0.02736 0.02091 0.02748 -0.00025 0.00743 -0.00133 0.02492 0.00217 0.00020 0.00004 0.00012 0.00000 0.00057 0.00052 0.00060 0.00044 0.00047 0.00044 0.00025 P3 0.59639 0.64229 -0.12010 1.00000 0.02845 0.02978 0.02585 0.00176 0.00891 -0.00091 0.02759 0.00230 0.00020 0.00004 0.00012 0.00000 0.00059 0.00060 0.00062 0.00047 0.00049 0.00047 0.00027 Cl1 0.20658 0.72453 0.10818 1.00000 0.04810 0.03141 0.04494 0.00381 0.01024 0.01378 0.04110 0.00267 0.00023 0.00005 0.00013 0.00000 0.00075 0.00061 0.00075 0.00053 0.00060 0.00055 0.00032 Cl2 0.15722 0.54564 0.03174 1.00000 0.03365 0.03187 0.04898 -0.00527 0.00673 -0.00991 0.03800 0.00225 0.00021 0.00004 0.00013 0.00000 0.00061 0.00060 0.00078 0.00053 0.00054 0.00049 0.00030 Cl3 0.41855 0.65286 -0.28954 1.00000 0.03164 0.05078 0.03066 0.00472 0.00679 0.00301 0.03744 0.00245 0.00021 0.00005 0.00012 0.00000 0.00060 0.00074 0.00064 0.00053 0.00050 0.00052 0.00030 Cl4 0.90453 0.64421 -0.17000 1.00000 0.02652 0.06200 0.03776 0.00605 0.00960 -0.00128 0.04165 0.00256 0.00020 0.00006 0.00013 0.00000 0.00058 0.00085 0.00072 0.00060 0.00052 0.00055 0.00032 Final Structure Factor Calculation for 2007src0194 in P2(1)/c Total number of l.s. parameters = 235 Maximum vector length = 511 Memory required = 2059 / 26061 wR2 = 0.1381 before cycle 5 for 3849 data and 0 / 235 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0205 * P )^2 + 9.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0633 for 3270 Fo > 4sig(Fo) and 0.0771 for all 3849 data wR2 = 0.1381, GooF = S = 1.100, Restrained GooF = 1.100 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0463 0.0327 0.0224 C1 0.0511 0.0237 0.0225 C2 0.0486 0.0305 0.0196 C3 0.0495 0.0302 0.0261 C4 0.0474 0.0343 0.0236 C5 0.0407 0.0290 0.0220 C6 0.0332 0.0226 0.0193 N1 0.0408 0.0289 0.0197 N2 0.0526 0.0287 0.0195 N3 0.0458 0.0283 0.0213 O1 0.0422 0.0259 0.0216 O2 0.0808 0.0409 0.0244 F1 0.0608 0.0429 0.0285 F2 0.0402 0.0364 0.0205 F3 0.0751 0.0494 0.0248 F4 0.0465 0.0330 0.0184 F5 0.0638 0.0437 0.0269 F6 0.0657 0.0387 0.0249 F7 0.0675 0.0417 0.0282 F8 0.0372 0.0241 0.0192 P1 0.0316 0.0227 0.0205 P2 0.0327 0.0302 0.0199 P3 0.0581 0.0416 0.0236 Cl1 0.0515 0.0397 0.0228 Cl2 0.0523 0.0329 0.0271 Cl3 0.0634 0.0388 0.0227 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.042 0.057 0.076 0.098 0.124 0.161 0.233 1.000 Number in group 399. 372. 393. 379. 389. 386. 376. 384. 385. 386. GooF 1.317 1.241 1.085 1.087 1.040 0.945 1.050 1.089 0.963 1.128 K 5.470 1.723 1.211 1.044 1.014 0.996 1.002 1.002 1.003 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 394. 377. 396. 386. 376. 383. 390. 377. 382. 388. GooF 1.256 1.181 1.214 1.152 1.158 1.047 0.994 0.960 0.919 1.059 K 1.079 1.034 1.041 1.026 1.004 1.014 1.000 1.004 1.008 1.004 R1 0.203 0.164 0.136 0.118 0.100 0.084 0.066 0.044 0.038 0.030 Recommended weighting scheme: WGHT 0.0203 9.7486 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) 2 6 10 2058.42 4979.01 7.33 0.349 0.93 4 0 10 30.28 503.07 6.84 0.111 0.82 3 18 2 2308.08 3665.95 5.28 0.300 1.16 1 13 5 1245.33 2182.09 4.72 0.231 1.41 -1 10 1 4893.60 6402.63 4.29 0.396 2.43 1 12 11 280.85 762.18 4.22 0.137 0.85 3 4 7 2893.38 4169.92 4.04 0.320 1.12 3 3 10 147.11 0.57 4.02 0.004 0.88 4 4 9 211.58 32.16 3.91 0.028 0.87 6 14 0 751.16 1299.39 3.82 0.178 0.89 -1 3 11 168.74 37.03 3.69 0.030 0.95 2 4 12 -15.20 136.31 3.62 0.058 0.81 1 13 1 361.94 673.94 3.61 0.129 1.93 2 16 9 1653.57 1102.35 3.57 0.164 0.89 1 15 5 470.88 823.83 3.45 0.142 1.31 1 3 13 391.80 108.35 3.45 0.052 0.78 2 1 8 140.80 24.30 3.44 0.024 1.15 3 7 7 246.48 504.88 3.40 0.111 1.09 -1 1 12 101.53 12.00 3.32 0.017 0.87 0 7 11 290.62 21.96 3.25 0.023 0.92 -3 3 9 63.65 0.00 3.17 0.000 1.05 -1 9 13 181.08 34.39 3.16 0.029 0.78 1 13 9 364.02 656.73 3.16 0.127 0.98 -4 7 4 78.27 12.28 3.14 0.017 1.29 0 25 9 1305.08 874.89 3.14 0.146 0.79 -1 8 13 1261.83 837.07 3.13 0.143 0.79 0 9 12 -14.91 103.83 3.12 0.050 0.84 -2 6 13 94.77 9.49 3.10 0.015 0.79 1 9 12 85.53 0.47 3.10 0.003 0.82 5 11 5 330.49 630.72 3.10 0.124 0.92 2 5 10 244.03 65.46 3.06 0.040 0.94 1 4 13 275.76 578.34 3.05 0.119 0.78 1 9 7 2180.03 2868.60 3.02 0.265 1.28 0 4 12 70.32 0.40 3.01 0.003 0.86 6 0 6 -48.86 77.49 3.00 0.044 0.83 0 2 6 75.87 0.14 2.99 0.002 1.73 1 1 13 112.37 0.87 2.98 0.005 0.78 7 11 3 256.51 486.64 2.96 0.109 0.77 4 6 9 1023.42 606.01 2.96 0.122 0.86 4 2 5 83.83 8.53 2.95 0.014 1.16 -2 23 6 -11.15 72.85 2.95 0.042 0.95 -3 21 6 68.05 3.11 2.92 0.009 0.95 4 10 8 155.73 12.32 2.91 0.017 0.89 -3 3 2 42.07 1.70 2.88 0.006 1.90 0 16 11 1197.45 798.41 2.87 0.140 0.83 4 0 2 11805.68 10122.61 2.83 0.498 1.40 2 7 0 411.11 244.27 2.82 0.077 2.38 -5 12 3 63.95 7.73 2.81 0.014 1.04 0 10 11 5.51 82.50 2.80 0.045 0.90 4 9 7 142.28 30.13 2.79 0.027 0.95 Bond lengths and angles C1 - Distance Angles O1 1.4433 (0.0057) C2 1.5200 (0.0074) 109.50 (0.39) C1 - O1 C2 - Distance Angles F2 1.3522 (0.0054) F1 1.3572 (0.0053) 107.31 (0.38) C1 1.5200 (0.0074) 107.45 (0.39) 108.81 (0.42) C3 1.5575 (0.0071) 108.30 (0.42) 104.51 (0.38) 119.88 (0.40) C2 - F2 F1 C1 C3 - Distance Angles F4 1.3492 (0.0055) F3 1.3551 (0.0056) 107.38 (0.36) C2 1.5575 (0.0071) 108.47 (0.41) 109.62 (0.41) C4 1.5577 (0.0071) 106.44 (0.42) 109.91 (0.41) 114.72 (0.38) C3 - F4 F3 C2 C4 - Distance Angles F6 1.3488 (0.0059) F5 1.3520 (0.0054) 106.71 (0.38) C3 1.5577 (0.0071) 107.35 (0.43) 109.03 (0.40) C5 1.5718 (0.0073) 108.80 (0.41) 107.98 (0.42) 116.55 (0.40) C4 - F6 F5 C3 C5 - Distance Angles F7 1.3487 (0.0055) F8 1.3584 (0.0057) 106.93 (0.38) C6 1.5187 (0.0074) 111.59 (0.43) 106.01 (0.41) C4 1.5718 (0.0073) 108.79 (0.41) 104.90 (0.41) 117.85 (0.40) C5 - F7 F8 C6 C6 - Distance Angles O2 1.4283 (0.0053) C5 1.5187 (0.0075) 111.03 (0.39) C6 - O2 N1 - Distance Angles P2 1.5705 (0.0037) P1 1.5840 (0.0037) 121.78 (0.23) N1 - P2 N2 - Distance Angles P3 1.5745 (0.0040) P2 1.5885 (0.0039) 121.01 (0.24) N2 - P3 N3 - Distance Angles P3 1.5764 (0.0041) P1 1.5842 (0.0039) 121.20 (0.25) N3 - P3 O1 - Distance Angles C1 1.4433 (0.0057) P1 1.5783 (0.0035) 120.71 (0.30) O1 - C1 O2 - Distance Angles C6 1.4283 (0.0053) P2 1.5717 (0.0034) 123.12 (0.29) O2 - C6 F1 - Distance Angles C2 1.3572 (0.0053) F1 - F2 - Distance Angles C2 1.3522 (0.0054) F2 - F3 - Distance Angles C3 1.3551 (0.0056) F3 - F4 - Distance Angles C3 1.3492 (0.0056) F4 - F5 - Distance Angles C4 1.3520 (0.0054) F5 - F6 - Distance Angles C4 1.3488 (0.0059) F6 - F7 - Distance Angles C5 1.3487 (0.0055) F7 - F8 - Distance Angles C5 1.3584 (0.0057) F8 - P1 - Distance Angles O1 1.5783 (0.0036) N1 1.5840 (0.0037) 110.54 (0.20) N3 1.5842 (0.0040) 106.78 (0.21) 118.22 (0.21) Cl1 1.9911 (0.0017) 103.33 (0.14) 108.49 (0.15) 108.45 (0.18) P1 - O1 N1 N3 P2 - Distance Angles N1 1.5705 (0.0037) O2 1.5717 (0.0034) 111.62 (0.20) N2 1.5885 (0.0039) 118.52 (0.20) 105.41 (0.19) Cl2 1.9876 (0.0017) 107.19 (0.15) 103.42 (0.14) 109.67 (0.17) P2 - N1 O2 N2 P3 - Distance Angles N2 1.5745 (0.0040) N3 1.5764 (0.0041) 119.12 (0.21) Cl4 1.9899 (0.0017) 109.50 (0.16) 108.42 (0.18) Cl3 1.9979 (0.0018) 108.21 (0.17) 109.04 (0.18) 101.04 (0.07) P3 - N2 N3 Cl4 Cl1 - Distance Angles P1 1.9911 (0.0017) Cl1 - Cl2 - Distance Angles P2 1.9876 (0.0017) Cl2 - Cl3 - Distance Angles P3 1.9979 (0.0018) Cl3 - Cl4 - Distance Angles P3 1.9899 (0.0017) Cl4 - FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 24 -2 3.846 1 2 R1 = 0.0768 for 3849 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.77 at 0.1108 0.5763 0.3805 [ 1.01 A from F4 ] Deepest hole -0.51 at 0.4237 0.4126 0.8767 [ 0.98 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 2716 / 32357 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1108 0.5763 0.3805 1.00000 0.05 0.77 1.01 F4 1.72 C3 1.95 F7 2.18 F3 Q2 1 0.8913 0.6081 0.5622 1.00000 0.05 0.64 0.98 F6 1.71 C4 1.90 F2 2.08 C3 Q3 1 0.7885 0.6172 0.4377 1.00000 0.05 0.54 1.03 C4 1.07 C3 1.51 F5 1.63 C2 Q4 1 0.4696 0.6496 0.1439 1.00000 0.05 0.51 0.71 N1 0.96 P1 1.93 O1 2.05 P2 Q5 1 0.5725 0.6094 -0.1123 1.00000 0.05 0.50 0.73 N2 0.91 P3 2.19 P2 2.30 N3 Q6 1 0.8828 0.5793 0.3154 1.00000 0.05 0.49 1.24 C3 1.26 F3 1.44 C4 1.69 C5 Q7 1 0.4301 0.6108 0.1063 1.00000 0.05 0.49 0.63 N1 0.95 P2 1.93 P1 2.14 O2 Q8 1 0.2118 0.6481 -0.2984 1.00000 0.05 0.46 1.25 CL3 2.41 CL4 2.81 F2 2.83 P3 Q9 1 0.7662 0.7077 0.5441 1.00000 0.05 0.44 0.98 F2 1.85 C2 1.94 H1B 2.20 C1 Q10 1 0.5046 0.6445 0.1248 1.00000 0.05 0.44 0.79 N1 1.04 P1 1.87 P2 2.01 O1 Q11 1 0.1563 0.5768 0.0783 1.00000 0.05 0.44 0.98 CL2 1.78 P2 2.11 N1 2.69 F3 Q12 1 0.9164 0.6088 -0.1704 1.00000 0.05 0.43 0.96 CL4 2.25 P3 2.63 N2 2.98 CL2 Q13 1 0.4834 0.6394 0.2578 1.00000 0.05 0.42 1.26 N1 1.42 H1A 1.97 P1 1.98 C1 Q14 1 1.1240 0.5366 0.3191 1.00000 0.05 0.42 1.19 F7 1.87 H6B 2.25 F4 2.36 C5 Q15 1 0.2718 0.6894 0.1002 1.00000 0.05 0.41 1.04 CL1 1.22 P1 1.91 N1 2.35 N3 Q16 1 0.5978 0.6691 -0.0626 1.00000 0.05 0.41 0.65 N3 0.95 P3 2.01 P1 2.20 N2 Q17 1 0.2361 0.6006 -0.2636 1.00000 0.05 0.41 1.84 CL3 2.61 CL4 2.61 N2 2.71 H6A Q18 1 0.1886 0.6376 -0.4020 1.00000 0.05 0.40 1.77 CL3 2.09 F4 2.38 F2 2.68 F6 Q19 1 0.4192 0.6004 -0.1027 1.00000 0.05 0.40 0.85 N2 1.59 P3 1.79 P2 2.42 CL3 Q20 1 0.7334 0.6789 0.3605 1.00000 0.05 0.40 0.79 C2 0.80 C1 1.38 H1A 1.60 H1B Shortest distances between peaks (including symmetry equivalents) 4 10 0.34 5 19 0.97 7 10 1.03 8 18 1.12 4 7 1.14 4 13 1.22 1 14 1.26 8 17 1.34 2 3 1.41 10 13 1.42 1 6 1.47 4 15 1.64 5 16 1.70 17 18 1.76 7 13 1.77 3 6 1.79 6 14 1.86 10 15 1.86 3 20 1.87 7 11 1.89 17 19 1.92 2 18 1.97 13 20 2.06 9 20 2.07 16 19 2.17 7 19 2.21 10 16 2.21 5 12 2.23 12 17 2.27 7 15 2.34 1 3 2.38 13 15 2.40 4 16 2.44 5 17 2.45 5 7 2.54 2 8 2.54 3 13 2.57 8 12 2.58 1 2 2.59 2 17 2.63 8 19 2.63 7 16 2.66 10 19 2.67 11 19 2.68 2 6 2.70 3 9 2.71 5 10 2.74 4 20 2.75 4 11 2.77 11 14 2.78 2 12 2.79 10 11 2.80 15 16 2.80 2 9 2.81 1 18 2.82 3 18 2.85 12 16 2.85 10 20 2.86 4 19 2.90 6 20 2.91 6 13 2.92 2 20 2.94 5 8 2.96 11 12 2.98 Time profile in seconds ----------------------- 0.05: 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 0.01: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 4.04: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.35: Structure factors and derivatives 2.32: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.21: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.10: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0194 finished at 20:56:30 Total CPU time: 8.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++