+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0699 started at 20:52:40 on 05-Jun-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0699 in Pna2(1) CELL 0.71073 23.2125 9.1684 7.6006 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0002 0.0002 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O P CL UNIT 36 40 12 8 12 16 V = 1617.57 F(000) = 856.0 Mu = 1.03 mm-1 Cell Wt = 1707.64 Rho = 1.753 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 OMIT 1 1 0 OMIT 2 1 0 OMIT 12 3 -3 FMAP 2 PLAN 20 SIZE 0.02 0.20 0.24 ACTA BOND WGHT 0.02330 0.68970 L.S. 4 TEMP -153.00 FVAR 0.41194 C1 1 0.244980 0.394939 0.398800 11.00000 0.01809 0.01928 = 0.01528 0.00070 0.00314 -0.00008 AFIX 23 H1A 2 0.219615 0.481600 0.404863 11.00000 -1.20000 H1B 2 0.272701 0.400146 0.497587 11.00000 -1.20000 AFIX 0 C2 1 0.208953 0.256661 0.414428 11.00000 0.01194 0.02143 = 0.01240 0.00236 0.00235 0.00077 AFIX 13 H2 2 0.182056 0.253337 0.311731 11.00000 -1.20000 AFIX 0 C3 1 0.248159 0.123364 0.403950 11.00000 0.01792 0.01905 = 0.01571 0.00295 0.00364 -0.00223 AFIX 23 H3A 2 0.276346 0.125611 0.501663 11.00000 -1.20000 H3B 2 0.224912 0.033314 0.415182 11.00000 -1.20000 AFIX 0 C4 1 0.173067 0.256915 0.580343 11.00000 0.01495 0.01612 = 0.01716 0.00074 0.00225 0.00008 C5 1 0.113141 0.256521 0.569706 11.00000 0.01508 0.02950 = 0.02177 -0.00196 0.00101 -0.00037 AFIX 43 H5 2 0.094975 0.255022 0.457718 11.00000 -1.20000 AFIX 0 C6 1 0.079847 0.258292 0.720612 11.00000 0.01647 0.03736 = 0.03587 0.00099 0.01180 0.00052 AFIX 43 H6 2 0.039027 0.257567 0.711675 11.00000 -1.20000 AFIX 0 C7 1 0.105726 0.261111 0.884384 11.00000 0.03519 0.03894 = 0.02297 -0.00077 0.01655 -0.00188 AFIX 43 H7 2 0.082827 0.262870 0.987956 11.00000 -1.20000 AFIX 0 C8 1 0.165013 0.261352 0.896410 11.00000 0.03930 0.03932 = 0.01454 -0.00102 0.00106 -0.00068 AFIX 43 H8 2 0.182963 0.262937 1.008720 11.00000 -1.20000 AFIX 0 C9 1 0.198585 0.259294 0.745391 11.00000 0.01996 0.03098 = 0.01855 0.00145 -0.00128 -0.00006 AFIX 43 H9 2 0.239388 0.259514 0.755083 11.00000 -1.20000 AFIX 0 N1 3 0.372684 0.264962 0.301404 11.00000 0.01354 0.03442 = 0.01226 0.00020 -0.00150 -0.00200 N2 3 0.440420 0.284180 0.011395 11.00000 0.01277 0.06597 = 0.01446 0.00246 0.00050 -0.00287 N3 3 0.323846 0.258880 -0.021859 11.00000 0.00986 0.02849 = 0.01411 0.00017 -0.00023 0.00019 O1 4 0.276233 0.394314 0.231114 11.00000 0.01848 0.01734 = 0.01827 0.00321 0.00489 0.00018 O2 4 0.278599 0.123345 0.235116 11.00000 0.01743 0.01510 = 0.01736 -0.00229 0.00346 -0.00065 P1 5 0.315604 0.260422 0.186343 11.00000 0.00995 0.01998 = 0.01235 -0.00008 0.00061 -0.00043 P2 5 0.434436 0.269720 0.218714 11.00000 0.01031 0.03061 = 0.01457 0.00037 -0.00128 -0.00031 P3 5 0.384997 0.270248 -0.108624 11.00000 0.01163 0.03393 = 0.01156 0.00015 0.00095 0.00068 CL1 6 0.480154 0.428632 0.328526 11.00000 0.02294 0.03359 = 0.03421 -0.00154 -0.00177 -0.01020 CL2 6 0.480110 0.096632 0.296289 11.00000 0.02838 0.03192 = 0.04336 -0.00025 -0.00189 0.01096 CL3 6 0.394484 0.101678 -0.273743 11.00000 0.03213 0.03761 = 0.02245 -0.00493 0.00281 0.01476 CL4 6 0.384203 0.436123 -0.279791 11.00000 0.02483 0.03447 = 0.01902 0.00389 0.00109 -0.00819 HKLF 4 1.0 0.00 -1.00 0.00 0.00 0.00 -1.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2006src0699 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C4 C1 C3 C3 - O2 C2 C4 - C9 C5 C2 C5 - C6 C4 C6 - C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C4 C8 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C3 P1 P1 - O2 O1 N1 N3 P2 - N1 N2 Cl1 Cl2 P3 - N3 N2 Cl4 Cl3 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 0 -7 35.81 8.35 observed but should be systematically absent 23 0 0 14.98 3.44 observed but should be systematically absent 0 7 0 51.53 10.71 observed but should be systematically absent 16235 Reflections read, of which 1167 rejected -30 =< h =< 20, -11 =< k =< 10, -9 =< l =< 9, Max. 2-theta = 54.99 3 Systematic absence violations 0 Inconsistent equivalents 3611 Unique reflections, of which 0 suppressed R(int) = 0.0443 R(sigma) = 0.0447 Friedel opposites not merged Maximum memory for data reduction = 1704 / 35716 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 = 2194 / 237744 wR2 = 0.0685 before cycle 1 for 3611 data and 190 / 190 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41204 0.00052 0.197 OSF Mean shift/esd = 0.046 Maximum = 0.201 for x C2 Max. shift = 0.001 A for C2 Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2194 / 237744 wR2 = 0.0684 before cycle 2 for 3611 data and 190 / 190 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41208 0.00052 0.069 OSF Mean shift/esd = 0.016 Maximum = 0.069 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2194 / 237744 wR2 = 0.0685 before cycle 3 for 3611 data and 190 / 190 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41208 0.00052 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U22 C2 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2194 / 237744 wR2 = 0.0685 before cycle 4 for 3611 data and 190 / 190 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41208 0.00052 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U22 N2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for N2 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 0.2196 0.4816 0.4048 23 0.990 0.000 C1 O1 C2 H1B 0.2727 0.4002 0.4976 23 0.990 0.000 C1 O1 C2 H2 0.1821 0.2533 0.3117 13 1.000 0.000 C2 C4 C1 C3 H3A 0.2763 0.1256 0.5016 23 0.990 0.000 C3 O2 C2 H3B 0.2249 0.0333 0.4151 23 0.990 0.000 C3 O2 C2 H5 0.0950 0.2550 0.4577 43 0.950 0.000 C5 C6 C4 H6 0.0390 0.2576 0.7117 43 0.950 0.000 C6 C7 C5 H7 0.0828 0.2628 0.9880 43 0.950 0.000 C7 C8 C6 H8 0.1829 0.2630 1.0087 43 0.950 0.000 C8 C7 C9 H9 0.2394 0.2595 0.7551 43 0.950 0.000 C9 C4 C8 2006src0699 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.24498 0.39492 0.39878 1.00000 0.01810 0.01938 0.01525 0.00061 0.00321 0.00004 0.01758 0.00444 0.00010 0.00025 0.00037 0.00000 0.00120 0.00116 0.00131 0.00110 0.00112 0.00094 0.00051 H1A 0.21960 0.48156 0.40483 1.00000 0.02109 0.00000 0.00000 H1B 0.27270 0.40017 0.49757 1.00000 0.02109 0.00000 0.00000 C2 0.20898 0.25665 0.41445 1.00000 0.01204 0.02146 0.01231 0.00234 0.00240 0.00076 0.01527 0.00445 0.00011 0.00023 0.00035 0.00000 0.00117 0.00121 0.00132 0.00101 0.00106 0.00087 0.00052 H2 0.18209 0.25333 0.31175 1.00000 0.01833 0.00000 0.00000 C3 0.24815 0.12337 0.40392 1.00000 0.01799 0.01907 0.01565 0.00293 0.00373 -0.00235 0.01757 0.00447 0.00010 0.00024 0.00036 0.00000 0.00122 0.00117 0.00132 0.00108 0.00111 0.00095 0.00052 H3A 0.27634 0.12557 0.50164 1.00000 0.02109 0.00000 0.00000 H3B 0.22489 0.03335 0.41513 1.00000 0.02109 0.00000 0.00000 C4 0.17306 0.25690 0.58038 1.00000 0.01508 0.01610 0.01700 0.00079 0.00237 0.00012 0.01606 0.00449 0.00011 0.00024 0.00039 0.00000 0.00125 0.00109 0.00137 0.00109 0.00113 0.00090 0.00052 C5 0.11314 0.25651 0.56973 1.00000 0.01523 0.02946 0.02164 -0.00199 0.00096 -0.00032 0.02211 0.00480 0.00011 0.00027 0.00043 0.00000 0.00134 0.00141 0.00164 0.00121 0.00120 0.00105 0.00061 H5 0.09497 0.25502 0.45774 1.00000 0.02653 0.00000 0.00000 C6 0.07984 0.25829 0.72062 1.00000 0.01665 0.03716 0.03576 0.00095 0.01179 0.00052 0.02986 0.00551 0.00012 0.00026 0.00050 0.00000 0.00127 0.00146 0.00185 0.00152 0.00148 0.00096 0.00067 H6 0.03902 0.25758 0.71169 1.00000 0.03583 0.00000 0.00000 C7 0.10573 0.26109 0.88438 1.00000 0.03524 0.03866 0.02286 -0.00079 0.01638 -0.00194 0.03225 0.00576 0.00014 0.00030 0.00046 0.00000 0.00176 0.00171 0.00180 0.00141 0.00150 0.00121 0.00075 H7 0.08283 0.26283 0.98796 1.00000 0.03871 0.00000 0.00000 C8 0.16499 0.26136 0.89638 1.00000 0.03954 0.03930 0.01446 -0.00107 0.00109 -0.00063 0.03110 0.00557 0.00014 0.00030 0.00043 0.00000 0.00178 0.00166 0.00145 0.00134 0.00144 0.00123 0.00069 H8 0.18294 0.26296 1.00869 1.00000 0.03732 0.00000 0.00000 C9 0.19858 0.25929 0.74542 1.00000 0.01997 0.03104 0.01854 0.00142 -0.00129 -0.00013 0.02318 0.00472 0.00012 0.00025 0.00040 0.00000 0.00132 0.00138 0.00152 0.00117 0.00119 0.00097 0.00060 H9 0.23938 0.25952 0.75513 1.00000 0.02782 0.00000 0.00000 N1 0.37268 0.26493 0.30143 1.00000 0.01366 0.03433 0.01232 0.00021 -0.00152 -0.00209 0.02010 0.00372 0.00009 0.00022 0.00032 0.00000 0.00104 0.00125 0.00122 0.00093 0.00091 0.00081 0.00049 N2 0.44041 0.28412 0.01139 1.00000 0.01262 0.06589 0.01447 0.00253 0.00049 -0.00277 0.03099 0.00445 0.00010 0.00029 0.00034 0.00000 0.00117 0.00171 0.00119 0.00124 0.00093 0.00108 0.00059 N3 0.32386 0.25886 -0.02183 1.00000 0.00996 0.02851 0.01398 0.00012 -0.00013 0.00020 0.01748 0.00379 0.00009 0.00022 0.00030 0.00000 0.00105 0.00117 0.00120 0.00091 0.00093 0.00082 0.00048 O1 0.27623 0.39432 0.23112 1.00000 0.01854 0.01736 0.01820 0.00321 0.00495 0.00019 0.01803 0.00293 0.00006 0.00016 0.00026 0.00000 0.00080 0.00075 0.00098 0.00079 0.00085 0.00058 0.00036 O2 0.27859 0.12333 0.23510 1.00000 0.01742 0.01509 0.01740 -0.00233 0.00346 -0.00060 0.01664 0.00283 0.00006 0.00016 0.00025 0.00000 0.00078 0.00073 0.00096 0.00076 0.00081 0.00058 0.00035 P1 0.31560 0.26042 0.18635 1.00000 0.01002 0.02001 0.01237 -0.00008 0.00060 -0.00042 0.01413 0.00103 0.00002 0.00006 0.00009 0.00000 0.00028 0.00030 0.00037 0.00029 0.00026 0.00021 0.00015 P2 0.43444 0.26972 0.21871 1.00000 0.01033 0.03063 0.01460 0.00036 -0.00131 -0.00031 0.01852 0.00111 0.00003 0.00007 0.00010 0.00000 0.00028 0.00032 0.00037 0.00036 0.00028 0.00022 0.00015 P3 0.38500 0.27025 -0.10863 1.00000 0.01161 0.03401 0.01159 0.00015 0.00095 0.00068 0.01907 0.00118 0.00003 0.00007 0.00009 0.00000 0.00030 0.00037 0.00035 0.00035 0.00028 0.00025 0.00015 Cl1 0.48016 0.42863 0.32852 1.00000 0.02292 0.03362 0.03428 -0.00153 -0.00176 -0.01019 0.03027 0.00118 0.00003 0.00007 0.00011 0.00000 0.00034 0.00035 0.00048 0.00033 0.00030 0.00026 0.00018 Cl2 0.48011 0.09663 0.29628 1.00000 0.02842 0.03196 0.04340 -0.00024 -0.00190 0.01097 0.03459 0.00128 0.00003 0.00007 0.00011 0.00000 0.00037 0.00035 0.00056 0.00037 0.00033 0.00027 0.00021 Cl3 0.39448 0.10167 -0.27374 1.00000 0.03214 0.03760 0.02248 -0.00493 0.00279 0.01473 0.03074 0.00126 0.00003 0.00007 0.00010 0.00000 0.00034 0.00035 0.00037 0.00038 0.00036 0.00026 0.00016 Cl4 0.38421 0.43611 -0.27978 1.00000 0.02485 0.03446 0.01904 0.00388 0.00110 -0.00818 0.02611 0.00111 0.00003 0.00007 0.00010 0.00000 0.00030 0.00032 0.00035 0.00036 0.00033 0.00024 0.00015 Final Structure Factor Calculation for 2006src0699 in Pna2(1) Total number of l.s. parameters = 190 Maximum vector length = 511 Memory required = 2006 / 27090 wR2 = 0.0684 before cycle 5 for 3611 data and 2 / 190 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0309 for 3272 Fo > 4sig(Fo) and 0.0373 for all 3611 data wR2 = 0.0684, GooF = S = 1.033, Restrained GooF = 1.033 for all data Flack x parameter = -0.0136 with esd 0.0664 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 = 21.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0203 0.0193 0.0131 C1 0.0222 0.0139 0.0097 C2 0.0209 0.0206 0.0111 C3 0.0188 0.0160 0.0134 C4 0.0300 0.0213 0.0151 C5 0.0416 0.0369 0.0110 C6 0.0471 0.0382 0.0115 C7 0.0402 0.0388 0.0144 C8 0.0312 0.0207 0.0177 C9 0.0345 0.0145 0.0113 N1 0.0662 0.0145 0.0123 N2 0.0285 0.0140 0.0100 N3 0.0242 0.0175 0.0124 O1 0.0216 0.0154 0.0130 O2 0.0200 0.0125 0.0099 P1 0.0306 0.0150 0.0100 P2 0.0340 0.0125 0.0106 P3 0.0398 0.0345 0.0165 Cl1 0.0442 0.0406 0.0190 Cl2 0.0500 0.0265 0.0157 Cl3 0.0395 0.0224 0.0164 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.039 0.053 0.065 0.079 0.095 0.115 0.146 0.204 1.000 Number in group 373. 349. 388. 342. 375. 347. 360. 360. 353. 364. GooF 1.037 0.967 1.018 0.998 1.054 1.036 0.991 1.133 1.104 0.979 K 1.283 0.996 0.998 1.017 1.002 1.006 1.007 1.008 0.998 1.009 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.05 1.16 1.32 1.67 inf Number in group 365. 377. 356. 352. 370. 349. 361. 358. 360. 363. GooF 1.078 0.941 0.999 1.056 0.966 0.928 0.956 0.924 0.984 1.406 K 0.964 1.005 1.022 1.030 1.024 0.993 0.991 1.001 1.001 1.017 R1 0.095 0.068 0.056 0.054 0.038 0.034 0.027 0.019 0.018 0.022 Recommended weighting scheme: WGHT 0.0230 0.6856 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) 6 2 -1 1362.17 1056.52 6.51 0.135 2.76 6 6 0 228.09 157.02 5.01 0.052 1.42 6 2 1 1339.06 1087.35 4.93 0.137 2.76 6 4 -1 1278.96 1055.57 4.90 0.135 1.91 14 7 0 100.78 43.42 4.60 0.027 1.03 6 3 0 512.62 264.77 4.52 0.068 2.40 6 1 -3 1694.40 1436.16 4.03 0.158 2.07 10 2 0 225.92 164.16 3.98 0.053 2.07 12 9 3 127.73 7.99 3.96 0.012 0.85 6 4 1 1250.06 1067.19 3.88 0.136 1.91 6 1 3 1657.21 1424.89 3.83 0.157 2.07 12 3 3 190.60 3.53 3.76 0.008 1.37 0 2 2 2053.84 1735.82 3.70 0.174 2.93 12 1 1 182.39 244.98 3.65 0.065 1.84 9 9 -2 1949.25 1619.69 3.58 0.168 0.92 7 7 0 28.72 8.46 3.55 0.012 1.22 8 3 0 1007.88 858.61 3.54 0.122 2.10 0 1 -5 270.54 356.38 3.52 0.079 1.50 12 0 -2 1843.63 1607.99 3.47 0.167 1.72 26 0 0 268.12 131.66 3.36 0.048 0.89 15 8 -1 84.54 151.30 3.28 0.051 0.91 12 1 -1 200.03 251.41 3.27 0.066 1.84 12 1 0 1360.47 1565.14 3.24 0.165 1.89 28 0 -3 389.43 587.13 3.19 0.101 0.79 0 2 -2 2163.35 1773.48 3.18 0.175 2.93 12 10 -3 80.09 207.89 3.12 0.060 0.79 0 10 0 305.22 412.80 3.07 0.085 0.92 28 0 -2 680.77 492.02 2.94 0.092 0.81 25 6 1 677.57 527.00 2.93 0.096 0.79 6 9 6 243.32 351.60 2.91 0.078 0.78 12 9 0 603.40 711.32 2.91 0.111 0.90 8 1 3 1808.77 2020.28 2.90 0.187 1.87 8 0 -3 4339.24 3847.85 2.90 0.258 1.91 6 1 -6 1356.66 1569.24 2.88 0.165 1.19 5 1 3 16.42 3.43 2.86 0.008 2.16 4 4 1 453.66 386.98 2.84 0.082 2.05 6 2 0 48.60 70.74 2.84 0.035 2.96 4 3 0 423.62 496.26 2.75 0.093 2.70 18 9 1 196.75 273.98 2.69 0.069 0.79 1 5 -2 1204.78 1341.53 2.68 0.153 1.65 2 1 -5 3344.04 3027.56 2.66 0.229 1.49 8 11 0 487.64 376.04 2.66 0.081 0.80 6 9 0 30.90 0.70 2.65 0.003 0.99 6 10 0 292.86 225.57 2.65 0.063 0.89 24 2 0 60.28 28.08 2.63 0.022 0.95 14 0 6 931.38 1094.04 2.61 0.138 1.01 7 1 8 229.43 157.56 2.60 0.052 0.91 15 10 -1 -33.21 51.07 2.59 0.030 0.78 2 4 1 12493.92 11512.49 2.58 0.447 2.16 14 0 -6 873.09 1096.88 2.57 0.138 1.01 Bond lengths and angles C1 - Distance Angles O1 1.4663 (0.0031) C2 1.5230 (0.0031) 109.65 (0.19) C1 - O1 C2 - Distance Angles C4 1.5119 (0.0037) C1 1.5230 (0.0031) 111.50 (0.19) C3 1.5252 (0.0031) 111.95 (0.19) 109.62 (0.20) C2 - C4 C1 C3 - Distance Angles O2 1.4649 (0.0031) C2 1.5252 (0.0031) 109.49 (0.19) C3 - O2 C4 - Distance Angles C9 1.3874 (0.0040) C5 1.3933 (0.0036) 118.61 (0.27) C2 1.5119 (0.0037) 121.25 (0.22) 120.14 (0.26) C4 - C9 C5 C5 - Distance Angles C6 1.3831 (0.0043) C4 1.3933 (0.0036) 120.64 (0.29) C5 - C6 C6 - Distance Angles C7 1.3823 (0.0049) C5 1.3831 (0.0043) 120.26 (0.25) C6 - C7 C7 - Distance Angles C8 1.3788 (0.0046) C6 1.3823 (0.0049) 119.56 (0.27) C7 - C8 C8 - Distance Angles C7 1.3788 (0.0046) C9 1.3873 (0.0042) 120.40 (0.30) C8 - C7 C9 - Distance Angles C4 1.3874 (0.0040) C8 1.3873 (0.0042) 120.53 (0.26) C9 - C4 N1 - Distance Angles P2 1.5659 (0.0022) P1 1.5882 (0.0022) 122.91 (0.16) N1 - P2 N2 - Distance Angles P3 1.5821 (0.0025) P2 1.5873 (0.0027) 119.65 (0.15) N2 - P3 N3 - Distance Angles P3 1.5685 (0.0022) P1 1.5939 (0.0023) 121.72 (0.15) N3 - P3 O1 - Distance Angles C1 1.4663 (0.0031) P1 1.5679 (0.0016) 118.68 (0.14) O1 - C1 O2 - Distance Angles C3 1.4649 (0.0031) P1 1.5669 (0.0016) 118.13 (0.14) O2 - C3 P1 - Distance Angles O2 1.5669 (0.0016) O1 1.5679 (0.0016) 104.90 (0.09) N1 1.5882 (0.0022) 110.37 (0.10) 110.27 (0.11) N3 1.5939 (0.0023) 107.07 (0.11) 107.01 (0.11) 116.53 (0.12) P1 - O2 O1 N1 P2 - Distance Angles N1 1.5659 (0.0022) N2 1.5873 (0.0027) 118.75 (0.13) Cl1 1.9864 (0.0009) 109.93 (0.09) 108.02 (0.10) Cl2 1.9975 (0.0009) 110.19 (0.09) 108.22 (0.10) 100.09 (0.04) P2 - N1 N2 Cl1 P3 - Distance Angles N3 1.5685 (0.0022) N2 1.5821 (0.0025) 119.90 (0.13) Cl4 2.0012 (0.0009) 108.40 (0.09) 108.74 (0.10) Cl3 2.0031 (0.0010) 108.16 (0.09) 109.50 (0.10) 100.37 (0.04) P3 - N3 N2 Cl4 Cl1 - Distance Angles P2 1.9864 (0.0009) Cl1 - Cl2 - Distance Angles P2 1.9975 (0.0009) Cl2 - Cl3 - Distance Angles P3 2.0031 (0.0010) Cl3 - Cl4 - Distance Angles P3 2.0012 (0.0009) Cl4 - FMAP and GRID set by program FMAP 2 3 19 GRID -3.125 -1 -2 3.125 1 2 R1 = 0.0315 for 1983 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.0996 0.8671 0.2724 [ 0.84 A from CL4 ] Deepest hole -0.29 at 0.1302 0.0071 0.1859 [ 0.78 A from CL4 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2428 / 29306 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4004 0.3671 -0.2276 1.00000 0.05 0.32 0.84 CL4 1.32 P3 2.18 N2 2.46 CL3 Q2 1 0.4568 0.0641 0.2412 1.00000 0.05 0.31 0.75 CL2 1.96 P2 2.70 N2 2.72 N1 Q3 1 0.5001 0.4239 0.2278 1.00000 0.05 0.27 0.90 CL1 2.08 P2 2.50 N2 2.98 CL4 Q4 1 0.3873 0.2119 -0.1867 1.00000 0.05 0.27 0.80 P3 1.22 CL3 1.98 N3 2.06 N2 Q5 1 0.2574 0.1044 0.7410 1.00000 0.05 0.25 1.49 H9 1.76 H1A 1.88 H3A 1.97 C9 Q6 1 0.2903 0.2023 0.2232 1.00000 0.05 0.24 0.78 O2 0.84 P1 1.79 O1 1.83 C3 Q7 1 0.4396 0.2041 0.0608 1.00000 0.05 0.24 0.82 N2 1.35 P2 1.91 P3 2.25 CL2 Q8 1 0.2227 0.3241 0.3999 1.00000 0.05 0.23 0.70 C2 0.83 C1 1.33 H2 1.45 H1A Q9 1 0.3971 0.3010 0.2307 1.00000 0.05 0.23 0.85 N1 0.92 P2 1.95 N2 1.96 P1 Q10 1 0.3978 0.1789 -0.1637 1.00000 0.05 0.23 0.98 P3 1.10 CL3 1.92 N2 2.16 N3 Q11 1 0.0276 0.2896 0.6177 1.00000 0.05 0.23 0.82 H6 1.47 C6 2.01 H5 2.04 C5 Q12 1 0.1786 0.2417 0.8199 1.00000 0.05 0.23 0.69 C8 0.75 C9 1.45 H8 1.50 H9 Q13 1 0.1433 0.2210 0.5750 1.00000 0.05 0.23 0.77 C4 0.77 C5 1.47 H5 1.86 C9 Q14 1 0.0288 0.3413 0.5056 1.00000 0.05 0.22 1.76 H6 1.77 H5 2.03 CL2 2.16 C6 Q15 1 0.3721 0.2396 0.4021 1.00000 0.05 0.22 0.80 N1 2.03 P2 2.11 P1 2.57 H3A Q16 1 0.4112 0.3845 -0.3302 1.00000 0.05 0.22 0.87 CL4 2.07 P3 2.66 CL3 2.84 N2 Q17 1 0.1812 0.2496 0.6773 1.00000 0.05 0.22 0.66 C9 0.76 C4 1.48 H9 1.71 C8 Q18 1 0.0992 0.2400 0.6525 1.00000 0.05 0.22 0.71 C6 0.72 C5 1.48 H6 1.49 H5 Q19 1 0.3378 0.2647 0.2487 1.00000 0.05 0.21 0.70 P1 0.90 N1 1.86 O1 1.89 O2 Q20 1 -0.0062 0.2283 0.6714 1.00000 0.05 0.21 1.13 H6 2.05 C6 2.81 CL3 2.87 H5 Shortest distances between peaks (including symmetry equivalents) 4 10 0.42 1 16 0.83 11 14 0.98 11 20 1.05 12 17 1.09 13 18 1.19 13 17 1.20 6 19 1.26 9 19 1.42 15 19 1.43 1 4 1.49 9 15 1.53 11 18 1.74 1 10 1.79 14 20 1.82 7 9 1.85 17 18 1.91 2 7 1.92 7 10 1.98 4 16 2.00 12 13 2.04 16 20 2.18 14 18 2.19 12 18 2.24 4 7 2.24 5 17 2.27 10 16 2.29 5 12 2.30 6 8 2.35 6 15 2.36 8 17 2.42 18 20 2.45 1 20 2.46 8 13 2.46 2 9 2.58 15 16 2.59 6 9 2.64 3 9 2.64 10 20 2.69 2 11 2.71 2 14 2.74 3 16 2.74 2 14 2.75 4 20 2.75 3 7 2.77 11 13 2.78 1 7 2.80 7 19 2.82 2 15 2.82 3 20 2.83 5 8 2.88 13 14 2.93 8 19 2.96 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.02: 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. 2.96: 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 1.70: Structure factors and derivatives 1.43: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.32: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0699 finished at 20:52:50 Total CPU time: 6.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++