+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0702 started at 22:44:35 on 13-Jun-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006SRC0702 in P2(1)/c CELL 0.71073 15.9483 12.1905 16.5233 90.000 99.189 90.000 ZERR 8.00 0.0005 0.0003 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL UNIT 56 112 24 16 24 32 V = 3171.20 F(000) = 1648.0 Mu = 1.05 mm-1 Cell Wt = 3255.38 Rho = 1.705 MERG 2 OMIT -3.00 55.00 OMIT -1 1 2 OMIT 1 0 0 OMIT 0 1 2 OMIT -1 1 1 OMIT 0 2 0 OMIT 3 3 5 OMIT -5 2 7 OMIT 3 0 0 OMIT -3 5 5 OMIT 1 1 0 FMAP 2 PLAN 20 SIZE 0.20 0.20 0.35 ACTA BOND WGHT 0.03990 1.79460 L.S. 4 TEMP -153.00 FVAR 0.24798 MOLE 1 C1 1 0.114633 0.009770 0.330342 11.00000 0.02163 0.01740 = 0.02437 0.00057 0.00200 -0.00230 AFIX 23 H1A 2 0.155205 -0.007547 0.292639 11.00000 -1.20000 H1B 2 0.069607 -0.046914 0.322772 11.00000 -1.20000 AFIX 0 C2 1 0.161510 0.004882 0.419229 11.00000 0.01873 0.01866 = 0.02063 0.00113 0.00316 -0.00050 C3 1 0.250399 0.056524 0.429814 11.00000 0.01980 0.01636 = 0.02354 0.00357 0.00261 0.00335 AFIX 23 H3A 2 0.284273 0.028509 0.481089 11.00000 -1.20000 H3B 2 0.278931 0.033137 0.383685 11.00000 -1.20000 AFIX 0 C4 1 0.180001 -0.119017 0.437491 11.00000 0.02728 0.02083 = 0.02602 0.00317 0.00280 0.00125 AFIX 23 H4A 2 0.210525 -0.148455 0.394527 11.00000 -1.20000 H4B 2 0.218823 -0.124770 0.490417 11.00000 -1.20000 AFIX 0 C5 1 0.103288 -0.191942 0.441712 11.00000 0.03756 0.02334 = 0.04550 0.00669 0.00287 -0.00617 AFIX 137 H5A 2 0.075223 -0.168391 0.487393 11.00000 -1.50000 H5B 2 0.121920 -0.268269 0.450195 11.00000 -1.50000 H5C 2 0.063356 -0.186094 0.390264 11.00000 -1.50000 AFIX 0 C6 1 0.106296 0.057440 0.476657 11.00000 0.02158 0.02317 = 0.02186 0.00041 0.00516 0.00060 AFIX 23 H6A 2 0.098910 0.136092 0.462359 11.00000 -1.20000 H6B 2 0.049416 0.022889 0.466219 11.00000 -1.20000 AFIX 0 C7 1 0.140519 0.048557 0.568138 11.00000 0.03751 0.03041 = 0.01840 0.00034 0.00591 0.00671 AFIX 137 H7A 2 0.148862 -0.028868 0.583264 11.00000 -1.50000 H7B 2 0.099784 0.081446 0.599575 11.00000 -1.50000 H7C 2 0.194878 0.087391 0.580294 11.00000 -1.50000 AFIX 0 C8 1 0.271831 0.508251 0.596137 11.00000 0.02181 0.01754 = 0.02134 -0.00396 -0.00055 0.00009 AFIX 23 H8A 2 0.241641 0.470246 0.547028 11.00000 -1.20000 H8B 2 0.252900 0.475126 0.644864 11.00000 -1.20000 AFIX 0 C9 1 0.367871 0.488978 0.601258 11.00000 0.01832 0.01660 = 0.01867 -0.00262 0.00121 0.00083 C10 1 0.417244 0.488800 0.689260 11.00000 0.02139 0.01729 = 0.02248 -0.00315 0.00035 0.00325 AFIX 23 H10A 2 0.380759 0.456718 0.726311 11.00000 -1.20000 H10B 2 0.467760 0.441093 0.691193 11.00000 -1.20000 AFIX 0 C11 1 0.407541 0.572050 0.548702 11.00000 0.02544 0.02069 = 0.02417 -0.00043 0.00295 -0.00395 AFIX 23 H11A 2 0.468557 0.554263 0.551965 11.00000 -1.20000 H11B 2 0.403761 0.645881 0.572814 11.00000 -1.20000 AFIX 0 C12 1 0.367335 0.576944 0.457891 11.00000 0.04096 0.02861 = 0.02439 0.00350 0.00653 -0.00743 AFIX 137 H12A 2 0.370897 0.504532 0.432905 11.00000 -1.50000 H12B 2 0.397832 0.630691 0.429410 11.00000 -1.50000 H12C 2 0.307624 0.598734 0.453413 11.00000 -1.50000 AFIX 0 C13 1 0.378312 0.371266 0.568191 11.00000 0.02608 0.01835 = 0.02038 -0.00339 0.00416 -0.00038 AFIX 23 H13A 2 0.345996 0.366978 0.511909 11.00000 -1.20000 H13B 2 0.438999 0.360235 0.564127 11.00000 -1.20000 AFIX 0 C14 1 0.350055 0.276744 0.617659 11.00000 0.03849 0.01859 = 0.02732 -0.00154 0.00864 -0.00100 AFIX 137 H14A 2 0.383901 0.276545 0.672652 11.00000 -1.50000 H14B 2 0.358207 0.207216 0.590174 11.00000 -1.50000 H14C 2 0.289861 0.285611 0.622002 11.00000 -1.50000 AFIX 0 N1 3 0.219956 0.188167 0.273248 11.00000 0.01717 0.01969 = 0.01851 -0.00071 0.00217 0.00126 N2 3 0.228325 0.367530 0.371191 11.00000 0.01948 0.01887 = 0.02330 -0.00162 -0.00077 -0.00011 N3 3 0.080942 0.318829 0.269147 11.00000 0.01674 0.02353 = 0.02086 -0.00086 -0.00122 0.00254 N4 3 0.292784 0.640995 0.749876 11.00000 0.01777 0.01758 = 0.01838 0.00063 0.00183 -0.00012 N5 3 0.416395 0.795814 0.755808 11.00000 0.01790 0.01783 = 0.02253 -0.00101 -0.00154 -0.00217 N6 3 0.268289 0.818414 0.649658 11.00000 0.01955 0.01987 = 0.02501 0.00375 -0.00322 -0.00017 O1 4 0.076028 0.117528 0.308443 11.00000 0.01863 0.02384 = 0.02185 0.00467 0.00184 -0.00027 O2 4 0.249242 0.176461 0.432822 11.00000 0.02139 0.01937 = 0.01711 -0.00066 0.00203 -0.00316 O3 4 0.247776 0.624990 0.591761 11.00000 0.02569 0.02221 = 0.01914 -0.00187 -0.00264 0.00634 O4 4 0.445150 0.598396 0.719774 11.00000 0.01778 0.02232 = 0.02418 -0.00727 0.00289 -0.00091 P1 5 0.119389 0.200625 0.255816 11.00000 0.01674 0.01999 = 0.01530 0.00015 0.00019 0.00051 P2 5 0.260931 0.246988 0.355963 11.00000 0.01442 0.01810 = 0.01776 0.00084 0.00108 -0.00023 P3 5 0.133840 0.398117 0.334005 11.00000 0.01756 0.01936 = 0.01906 0.00018 0.00176 0.00130 P4 5 0.242539 0.696718 0.669168 11.00000 0.01473 0.01746 = 0.01953 0.00032 0.00025 0.00017 P5 5 0.390595 0.671837 0.769063 11.00000 0.01704 0.01666 = 0.01529 -0.00055 -0.00004 0.00065 P6 5 0.357351 0.865728 0.689104 11.00000 0.01721 0.01632 = 0.01928 0.00045 0.00098 -0.00084 CL1 6 0.082422 0.156294 0.139508 11.00000 0.02692 0.03104 = 0.01695 -0.00356 -0.00286 0.00301 CL2 6 0.385889 0.253122 0.356646 11.00000 0.01481 0.02801 = 0.02748 -0.00020 0.00269 -0.00071 CL3 6 0.069155 0.421479 0.427970 11.00000 0.02423 0.03995 = 0.02277 -0.00305 0.00602 0.00134 CL4 6 0.131000 0.548352 0.286878 11.00000 0.03123 0.02033 = 0.03387 0.00516 0.00363 0.00369 CL5 6 0.119698 0.699247 0.678757 11.00000 0.01499 0.02797 = 0.03637 0.00353 0.00343 0.00048 CL6 6 0.430535 0.635202 0.886597 11.00000 0.03069 0.02583 = 0.01720 0.00208 -0.00358 0.00000 CL7 6 0.343266 1.014288 0.734452 11.00000 0.02874 0.01848 = 0.03218 -0.00475 0.00184 0.00196 CL8 6 0.422522 0.902660 0.597691 11.00000 0.02591 0.03206 = 0.02638 0.00473 0.00832 -0.00069 HKLF 4 Covalent radii and connectivity table for 2006SRC0702 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C6 C3 C1 C4 C3 - O2 C2 C4 - C5 C2 C5 - C4 C6 - C7 C2 C7 - C6 C8 - O3 C9 C9 - C11 C8 C10 C13 C10 - O4 C9 C11 - C9 C12 C12 - C11 C13 - C14 C9 C14 - C13 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 N4 - P5 P4 N5 - P6 P5 N6 - P6 P4 O1 - C1 P1 O2 - C3 P2 O3 - C8 P4 O4 - C10 P5 P1 - O1 N1 N3 Cl1 P2 P2 - O2 N1 N2 Cl2 P1 P3 - N2 N3 Cl4 Cl3 P4 - O3 N6 N4 Cl5 P5 P5 - O4 N4 N5 Cl6 P4 P6 - N6 N5 Cl7 Cl8 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 Cl5 - P4 Cl6 - P5 Cl7 - P6 Cl8 - P6 h k l Fo^2 Sigma Why rejected 0 3 0 2.52 0.62 observed but should be systematically absent 0 3 0 4.47 0.79 observed but should be systematically absent 42429 Reflections read, of which 1327 rejected -20 =< h =< 20, -15 =< k =< 15, -21 =< l =< 21, Max. 2-theta = 54.99 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 10 7 0.24 0.12 6 1.39 4 8 11 -0.55 0.62 6 3.59 -4 9 13 21.45 1.00 4 9.14 3 Inconsistent equivalents 7260 Unique reflections, of which 0 suppressed R(int) = 0.0477 R(sigma) = 0.0396 Friedel opposites merged Maximum memory for data reduction = 3135 / 71998 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 = 4076 / 440745 wR2 = 0.0852 before cycle 1 for 7260 data and 347 / 347 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0399 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24793 0.00027 -0.182 OSF Mean shift/esd = 0.046 Maximum = -0.182 for OSF Max. shift = 0.001 A for H12A Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4076 / 440745 wR2 = 0.0851 before cycle 2 for 7260 data and 347 / 347 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0399 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24792 0.00027 -0.043 OSF Mean shift/esd = 0.015 Maximum = 0.053 for y C1 Max. shift = 0.000 A for H12A Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4076 / 440745 wR2 = 0.0851 before cycle 3 for 7260 data and 347 / 347 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0399 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24792 0.00027 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.004 for tors H7A Max. shift = 0.000 A for H5C Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4076 / 440745 wR2 = 0.0851 before cycle 4 for 7260 data and 347 / 347 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0399 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24792 0.00027 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cl8 Max. shift = 0.000 A for H5B Max. dU = 0.000 for N6 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 0.1552 -0.0075 0.2926 23 0.990 0.000 C1 O1 C2 H1B 0.0696 -0.0469 0.3228 23 0.990 0.000 C1 O1 C2 H3A 0.2843 0.0285 0.4811 23 0.990 0.000 C3 O2 C2 H3B 0.2789 0.0332 0.3837 23 0.990 0.000 C3 O2 C2 H4A 0.2105 -0.1484 0.3945 23 0.990 0.000 C4 C5 C2 H4B 0.2188 -0.1248 0.4904 23 0.990 0.000 C4 C5 C2 H5A 0.0753 -0.1685 0.4874 137 0.980 0.000 C5 C4 H5A H5B 0.1219 -0.2683 0.4502 137 0.980 0.000 C5 C4 H5A H5C 0.0633 -0.1861 0.3903 137 0.980 0.000 C5 C4 H5A H6A 0.0989 0.1361 0.4623 23 0.990 0.000 C6 C7 C2 H6B 0.0494 0.0229 0.4662 23 0.990 0.000 C6 C7 C2 H7A 0.1488 -0.0289 0.5833 137 0.980 0.000 C7 C6 H7A H7B 0.0998 0.0815 0.5995 137 0.980 0.000 C7 C6 H7A H7C 0.1949 0.0873 0.5803 137 0.980 0.000 C7 C6 H7A H8A 0.2416 0.4702 0.5470 23 0.990 0.000 C8 O3 C9 H8B 0.2529 0.4751 0.6449 23 0.990 0.000 C8 O3 C9 H10A 0.3808 0.4567 0.7263 23 0.990 0.000 C10 O4 C9 H10B 0.4678 0.4411 0.6912 23 0.990 0.000 C10 O4 C9 H11A 0.4686 0.5542 0.5520 23 0.990 0.000 C11 C9 C12 H11B 0.4038 0.6459 0.5728 23 0.990 0.000 C11 C9 C12 H12A 0.3708 0.5045 0.4329 137 0.980 0.000 C12 C11 H12A H12B 0.3979 0.6306 0.4294 137 0.980 0.000 C12 C11 H12A H12C 0.3076 0.5988 0.4534 137 0.980 0.000 C12 C11 H12A H13A 0.3460 0.3670 0.5119 23 0.990 0.000 C13 C14 C9 H13B 0.4390 0.3602 0.5641 23 0.990 0.000 C13 C14 C9 H14A 0.3838 0.2766 0.6727 137 0.980 0.000 C14 C13 H14A H14B 0.3583 0.2072 0.5902 137 0.980 0.000 C14 C13 H14A H14C 0.2898 0.2856 0.6219 137 0.980 0.000 C14 C13 H14A 2006SRC0702 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.11462 0.00981 0.33034 1.00000 0.02169 0.01728 0.02440 0.00055 0.00204 -0.00233 0.02130 0.00416 0.00015 0.00019 0.00014 0.00000 0.00124 0.00115 0.00119 0.00094 0.00096 0.00094 0.00049 H1A 0.15519 -0.00751 0.29264 1.00000 0.02556 0.00000 0.00000 H1B 0.06959 -0.04687 0.32277 1.00000 0.02556 0.00000 0.00000 C2 0.16151 0.00489 0.41924 1.00000 0.01854 0.01865 0.02060 0.00121 0.00304 -0.00049 0.01927 0.00413 0.00014 0.00018 0.00014 0.00000 0.00118 0.00116 0.00112 0.00090 0.00091 0.00092 0.00047 C3 0.25039 0.05656 0.42982 1.00000 0.01997 0.01629 0.02348 0.00361 0.00260 0.00336 0.02001 0.00414 0.00014 0.00018 0.00014 0.00000 0.00119 0.00113 0.00117 0.00091 0.00094 0.00093 0.00048 H3A 0.28427 0.02855 0.48109 1.00000 0.02401 0.00000 0.00000 H3B 0.27892 0.03316 0.38369 1.00000 0.02401 0.00000 0.00000 C4 0.18000 -0.11900 0.43749 1.00000 0.02712 0.02099 0.02597 0.00313 0.00284 0.00132 0.02485 0.00452 0.00016 0.00019 0.00015 0.00000 0.00133 0.00124 0.00126 0.00098 0.00102 0.00102 0.00053 H4A 0.21052 -0.14843 0.39452 1.00000 0.02982 0.00000 0.00000 H4B 0.21883 -0.12476 0.49041 1.00000 0.02982 0.00000 0.00000 C5 0.10330 -0.19196 0.44171 1.00000 0.03757 0.02320 0.04551 0.00671 0.00288 -0.00608 0.03584 0.00501 0.00018 0.00021 0.00018 0.00000 0.00163 0.00135 0.00164 0.00120 0.00129 0.00118 0.00065 H5A 0.07526 -0.16846 0.48742 1.00000 0.05376 0.00000 0.00000 H5B 0.12194 -0.26829 0.45015 1.00000 0.05376 0.00000 0.00000 H5C 0.06334 -0.18608 0.39028 1.00000 0.05376 0.00000 0.00000 C6 0.10631 0.05742 0.47665 1.00000 0.02149 0.02314 0.02186 0.00039 0.00519 0.00050 0.02197 0.00428 0.00015 0.00019 0.00013 0.00000 0.00124 0.00123 0.00118 0.00096 0.00096 0.00099 0.00050 H6A 0.09891 0.13606 0.46234 1.00000 0.02637 0.00000 0.00000 H6B 0.04943 0.02285 0.46620 1.00000 0.02637 0.00000 0.00000 C7 0.14051 0.04856 0.56813 1.00000 0.03748 0.03030 0.01851 0.00039 0.00603 0.00675 0.02859 0.00476 0.00017 0.00021 0.00014 0.00000 0.00152 0.00138 0.00118 0.00101 0.00106 0.00116 0.00057 H7A 0.14879 -0.02886 0.58328 1.00000 0.04289 0.00000 0.00000 H7B 0.09979 0.08153 0.59955 1.00000 0.04289 0.00000 0.00000 H7C 0.19489 0.08734 0.58028 1.00000 0.04289 0.00000 0.00000 C8 0.27183 0.50824 0.59614 1.00000 0.02196 0.01732 0.02140 -0.00393 -0.00056 0.00006 0.02067 0.00410 0.00015 0.00018 0.00014 0.00000 0.00123 0.00113 0.00114 0.00092 0.00093 0.00094 0.00049 H8A 0.24164 0.47022 0.54704 1.00000 0.02480 0.00000 0.00000 H8B 0.25292 0.47512 0.64488 1.00000 0.02480 0.00000 0.00000 C9 0.36787 0.48899 0.60124 1.00000 0.01826 0.01661 0.01871 -0.00256 0.00122 0.00068 0.01805 0.00393 0.00014 0.00018 0.00013 0.00000 0.00117 0.00112 0.00111 0.00088 0.00090 0.00091 0.00047 C10 0.41725 0.48880 0.68926 1.00000 0.02146 0.01716 0.02246 -0.00328 0.00037 0.00314 0.02070 0.00405 0.00015 0.00018 0.00014 0.00000 0.00122 0.00114 0.00115 0.00092 0.00094 0.00094 0.00049 H10A 0.38076 0.45671 0.72630 1.00000 0.02484 0.00000 0.00000 H10B 0.46777 0.44110 0.69119 1.00000 0.02484 0.00000 0.00000 C11 0.40754 0.57202 0.54872 1.00000 0.02543 0.02071 0.02407 -0.00045 0.00291 -0.00395 0.02351 0.00429 0.00016 0.00020 0.00014 0.00000 0.00130 0.00121 0.00121 0.00097 0.00100 0.00100 0.00051 H11A 0.46855 0.55423 0.55198 1.00000 0.02822 0.00000 0.00000 H11B 0.40376 0.64585 0.57283 1.00000 0.02822 0.00000 0.00000 C12 0.36732 0.57693 0.45787 1.00000 0.04102 0.02855 0.02431 0.00352 0.00651 -0.00735 0.03115 0.00476 0.00018 0.00022 0.00015 0.00000 0.00160 0.00138 0.00127 0.00108 0.00113 0.00120 0.00059 H12A 0.37082 0.50450 0.43290 1.00000 0.04673 0.00000 0.00000 H12B 0.39786 0.63061 0.42938 1.00000 0.04673 0.00000 0.00000 H12C 0.30763 0.59881 0.45339 1.00000 0.04673 0.00000 0.00000 C13 0.37831 0.37127 0.56820 1.00000 0.02592 0.01830 0.02049 -0.00344 0.00419 -0.00041 0.02152 0.00423 0.00016 0.00018 0.00014 0.00000 0.00130 0.00116 0.00115 0.00093 0.00098 0.00097 0.00050 H13A 0.34601 0.36698 0.51191 1.00000 0.02582 0.00000 0.00000 H13B 0.43900 0.36024 0.56415 1.00000 0.02582 0.00000 0.00000 C14 0.35005 0.27675 0.61765 1.00000 0.03834 0.01860 0.02737 -0.00151 0.00858 -0.00091 0.02774 0.00469 0.00017 0.00019 0.00015 0.00000 0.00155 0.00119 0.00131 0.00100 0.00113 0.00108 0.00056 H14A 0.38385 0.27659 0.67267 1.00000 0.04161 0.00000 0.00000 H14B 0.35826 0.20722 0.59019 1.00000 0.04161 0.00000 0.00000 H14C 0.28984 0.28558 0.62194 1.00000 0.04161 0.00000 0.00000 N1 0.21997 0.18819 0.27326 1.00000 0.01719 0.01959 0.01843 -0.00073 0.00227 0.00125 0.01847 0.00334 0.00012 0.00015 0.00011 0.00000 0.00099 0.00098 0.00095 0.00077 0.00076 0.00078 0.00040 N2 0.22832 0.36754 0.37119 1.00000 0.01936 0.01885 0.02326 -0.00162 -0.00074 -0.00013 0.02094 0.00340 0.00012 0.00015 0.00012 0.00000 0.00103 0.00099 0.00100 0.00080 0.00081 0.00080 0.00042 N3 0.08095 0.31883 0.26915 1.00000 0.01670 0.02343 0.02092 -0.00092 -0.00120 0.00251 0.02081 0.00343 0.00012 0.00016 0.00011 0.00000 0.00099 0.00103 0.00098 0.00081 0.00078 0.00082 0.00042 N4 0.29278 0.64099 0.74987 1.00000 0.01769 0.01751 0.01834 0.00068 0.00183 -0.00006 0.01796 0.00334 0.00012 0.00015 0.00011 0.00000 0.00098 0.00095 0.00093 0.00075 0.00077 0.00077 0.00040 N5 0.41638 0.79581 0.75581 1.00000 0.01785 0.01788 0.02251 -0.00096 -0.00154 -0.00214 0.01993 0.00331 0.00012 0.00015 0.00011 0.00000 0.00099 0.00097 0.00100 0.00078 0.00078 0.00078 0.00041 N6 0.26830 0.81838 0.64966 1.00000 0.01957 0.01983 0.02487 0.00380 -0.00320 -0.00014 0.02216 0.00348 0.00012 0.00016 0.00012 0.00000 0.00103 0.00101 0.00105 0.00082 0.00081 0.00082 0.00043 O1 0.07603 0.11754 0.30844 1.00000 0.01855 0.02375 0.02180 0.00468 0.00177 -0.00028 0.02152 0.00289 0.00010 0.00013 0.00009 0.00000 0.00084 0.00086 0.00082 0.00067 0.00066 0.00068 0.00035 O2 0.24925 0.17646 0.43282 1.00000 0.02134 0.01930 0.01712 -0.00065 0.00204 -0.00318 0.01937 0.00274 0.00010 0.00013 0.00009 0.00000 0.00085 0.00080 0.00078 0.00063 0.00064 0.00066 0.00034 O3 0.24776 0.62498 0.59175 1.00000 0.02561 0.02219 0.01900 -0.00184 -0.00263 0.00629 0.02294 0.00286 0.00010 0.00013 0.00009 0.00000 0.00091 0.00086 0.00080 0.00067 0.00068 0.00070 0.00036 O4 0.44515 0.59840 0.71979 1.00000 0.01768 0.02225 0.02423 -0.00725 0.00294 -0.00092 0.02143 0.00275 0.00010 0.00013 0.00009 0.00000 0.00084 0.00085 0.00084 0.00067 0.00066 0.00067 0.00035 P1 0.11939 0.20062 0.25582 1.00000 0.01672 0.02002 0.01527 0.00014 0.00019 0.00050 0.01760 0.00105 0.00004 0.00005 0.00003 0.00000 0.00030 0.00030 0.00028 0.00022 0.00022 0.00023 0.00013 P2 0.26093 0.24698 0.35596 1.00000 0.01437 0.01813 0.01777 0.00085 0.00109 -0.00025 0.01692 0.00105 0.00004 0.00005 0.00003 0.00000 0.00029 0.00030 0.00029 0.00022 0.00023 0.00023 0.00013 P3 0.13384 0.39811 0.33400 1.00000 0.01754 0.01938 0.01905 0.00021 0.00175 0.00132 0.01879 0.00107 0.00004 0.00005 0.00004 0.00000 0.00031 0.00030 0.00029 0.00023 0.00023 0.00024 0.00013 P4 0.24254 0.69672 0.66917 1.00000 0.01468 0.01747 0.01950 0.00030 0.00022 0.00018 0.01749 0.00104 0.00004 0.00005 0.00004 0.00000 0.00029 0.00030 0.00029 0.00023 0.00023 0.00023 0.00013 P5 0.39059 0.67184 0.76906 1.00000 0.01702 0.01671 0.01527 -0.00055 -0.00003 0.00063 0.01662 0.00103 0.00004 0.00005 0.00003 0.00000 0.00030 0.00029 0.00027 0.00022 0.00022 0.00023 0.00013 P6 0.35735 0.86573 0.68910 1.00000 0.01721 0.01629 0.01926 0.00044 0.00101 -0.00083 0.01780 0.00105 0.00004 0.00005 0.00004 0.00000 0.00030 0.00028 0.00029 0.00023 0.00023 0.00023 0.00013 Cl1 0.08242 0.15630 0.13951 1.00000 0.02689 0.03106 0.01693 -0.00355 -0.00285 0.00303 0.02565 0.00105 0.00004 0.00005 0.00003 0.00000 0.00032 0.00032 0.00027 0.00023 0.00023 0.00025 0.00014 Cl2 0.38589 0.25312 0.35665 1.00000 0.01479 0.02800 0.02743 -0.00019 0.00268 -0.00071 0.02348 0.00104 0.00004 0.00005 0.00004 0.00000 0.00028 0.00031 0.00030 0.00024 0.00023 0.00023 0.00013 Cl3 0.06916 0.42147 0.42797 1.00000 0.02420 0.03992 0.02279 -0.00306 0.00602 0.00137 0.02872 0.00113 0.00004 0.00005 0.00004 0.00000 0.00032 0.00036 0.00030 0.00026 0.00024 0.00027 0.00014 Cl4 0.13100 0.54835 0.28688 1.00000 0.03119 0.02032 0.03386 0.00517 0.00362 0.00370 0.02863 0.00115 0.00004 0.00005 0.00004 0.00000 0.00034 0.00029 0.00033 0.00025 0.00026 0.00025 0.00014 Cl5 0.11970 0.69925 0.67876 1.00000 0.01499 0.02800 0.03636 0.00351 0.00343 0.00049 0.02652 0.00111 0.00004 0.00005 0.00004 0.00000 0.00028 0.00032 0.00034 0.00026 0.00024 0.00024 0.00014 Cl6 0.43053 0.63521 0.88660 1.00000 0.03064 0.02583 0.01718 0.00209 -0.00357 -0.00001 0.02536 0.00105 0.00004 0.00005 0.00003 0.00000 0.00033 0.00030 0.00027 0.00023 0.00023 0.00025 0.00014 Cl7 0.34327 1.01429 0.73445 1.00000 0.02870 0.01848 0.03217 -0.00474 0.00184 0.00196 0.02678 0.00106 0.00004 0.00005 0.00004 0.00000 0.00033 0.00028 0.00032 0.00024 0.00025 0.00024 0.00014 Cl8 0.42252 0.90266 0.59769 1.00000 0.02588 0.03208 0.02636 0.00474 0.00830 -0.00069 0.02766 0.00115 0.00004 0.00005 0.00004 0.00000 0.00032 0.00033 0.00030 0.00025 0.00024 0.00026 0.00014 Final Structure Factor Calculation for 2006SRC0702 in P2(1)/c Total number of l.s. parameters = 347 Maximum vector length = 511 Memory required = 3729 / 25039 wR2 = 0.0851 before cycle 5 for 7260 data and 0 / 347 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0399 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0347 for 5579 Fo > 4sig(Fo) and 0.0561 for all 7260 data wR2 = 0.0851, GooF = S = 1.057, Restrained GooF = 1.057 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0259 0.0218 0.0163 C1 0.0213 0.0188 0.0177 C2 0.0250 0.0216 0.0134 C3 0.0285 0.0268 0.0193 C4 0.0509 0.0371 0.0195 C5 0.0237 0.0226 0.0196 C6 0.0415 0.0263 0.0179 C7 0.0274 0.0200 0.0146 C8 0.0219 0.0174 0.0149 C9 0.0280 0.0192 0.0149 C10 0.0280 0.0241 0.0184 C11 0.0446 0.0287 0.0201 C12 0.0260 0.0229 0.0157 C13 0.0389 0.0260 0.0183 C14 0.0207 0.0181 0.0167 N1 0.0269 0.0190 0.0169 N2 0.0263 0.0217 0.0144 N3 0.0195 0.0175 0.0169 N4 0.0264 0.0192 0.0142 N5 0.0318 0.0196 0.0151 N6 0.0280 0.0191 0.0176 O1 0.0238 0.0181 0.0162 O2 0.0343 0.0189 0.0156 O3 0.0306 0.0179 0.0158 O4 0.0201 0.0188 0.0138 P1 0.0193 0.0174 0.0140 P2 0.0204 0.0194 0.0165 P3 0.0211 0.0175 0.0139 P4 0.0197 0.0164 0.0137 P5 0.0209 0.0167 0.0157 P6 0.0359 0.0266 0.0145 Cl1 0.0281 0.0276 0.0147 Cl2 0.0406 0.0255 0.0200 Cl3 0.0358 0.0323 0.0178 Cl4 0.0379 0.0268 0.0149 Cl5 0.0354 0.0260 0.0146 Cl6 0.0362 0.0274 0.0168 Cl7 0.0348 0.0284 0.0197 Cl8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.033 0.045 0.059 0.075 0.095 0.121 0.167 1.000 Number in group 760. 728. 715. 729. 728. 702. 719. 734. 725. 720. GooF 0.915 1.001 1.104 1.112 1.163 1.030 1.036 0.936 1.030 1.213 K 0.545 0.834 0.885 0.909 0.938 0.963 0.975 0.998 1.025 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 734. 721. 730. 725. 734. 717. 728. 721. 721. 729. GooF 0.991 0.952 1.041 1.008 1.025 1.064 1.041 0.960 0.905 1.474 K 0.949 1.014 1.015 1.009 1.003 1.025 1.025 1.030 1.020 0.978 R1 0.163 0.113 0.090 0.077 0.062 0.051 0.039 0.029 0.022 0.028 Recommended weighting scheme: WGHT 0.0399 1.7639 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 4 1 130.46 50.48 5.41 0.017 2.96 1 3 20 2973.79 4252.01 4.95 0.158 0.79 3 2 3 268.50 153.77 4.76 0.030 3.04 3 1 7 598.58 408.16 4.75 0.049 1.99 0 6 0 4366.83 3410.99 4.74 0.141 2.03 4 4 0 370.57 224.09 4.68 0.036 2.41 2 1 1 77.14 235.56 4.52 0.037 5.86 -6 3 2 1657.89 1293.84 4.35 0.087 2.20 1 2 7 7.85 70.75 4.32 0.020 2.11 -3 5 3 312.61 198.65 4.27 0.034 2.10 4 3 13 313.88 488.68 4.18 0.053 1.10 5 2 3 1257.10 1618.88 4.18 0.097 2.36 3 4 3 9.06 80.84 4.00 0.022 2.30 1 1 7 195.60 114.87 3.97 0.026 2.22 7 2 3 1735.84 1389.61 3.90 0.090 1.87 -3 3 1 1353.01 1698.20 3.90 0.100 3.21 8 1 0 6711.66 5609.67 3.88 0.181 1.94 0 5 2 6390.23 7711.12 3.85 0.212 2.34 6 1 0 4905.43 4106.97 3.74 0.155 2.57 -5 4 5 902.61 703.45 3.71 0.064 1.92 14 0 0 948.60 1275.67 3.71 0.086 1.12 -6 10 13 381.00 566.69 3.64 0.058 0.86 -1 13 6 10183.35 8401.34 3.58 0.222 0.89 3 3 4 713.66 549.95 3.56 0.057 2.41 2 15 3 8271.50 6699.12 3.53 0.198 0.80 -9 6 15 350.31 118.15 3.52 0.026 0.90 7 1 1 545.52 408.01 3.47 0.049 2.15 -2 1 16 301.29 184.17 3.43 0.033 1.03 0 2 2 19936.67 23476.13 3.35 0.371 4.88 7 0 4 599.30 441.67 3.34 0.051 1.85 -14 7 11 109.31 573.05 3.26 0.058 0.85 -5 2 1 2345.05 2781.12 3.24 0.128 2.82 3 5 1 1604.09 1926.30 3.20 0.106 2.17 5 4 2 462.19 350.28 3.20 0.045 2.06 -18 7 5 634.92 968.34 3.19 0.075 0.79 17 3 4 331.55 547.96 3.19 0.057 0.85 -4 9 10 166.49 290.08 3.16 0.041 1.03 7 9 8 124.97 220.00 3.09 0.036 0.97 0 2 7 1238.86 1030.83 3.07 0.078 2.18 14 1 11 66.36 371.67 3.05 0.047 0.83 -4 9 15 200.84 336.29 3.04 0.044 0.85 4 7 0 541.04 418.01 3.01 0.049 1.59 -1 1 7 196.54 273.55 2.99 0.040 2.32 -2 6 1 211.19 144.80 2.99 0.029 1.96 14 2 10 79.85 291.64 2.98 0.041 0.86 -6 0 18 209.22 28.50 2.98 0.013 0.90 -5 1 3 471.34 368.43 2.98 0.046 2.85 0 1 3 3345.63 3905.17 2.97 0.151 4.97 -6 2 6 982.48 1187.03 2.97 0.083 1.95 -1 1 19 269.10 20.69 2.96 0.011 0.86 Bond lengths and angles C1 - Distance Angles O1 1.4708 (0.0027) C2 1.5394 (0.0031) 112.96 (0.18) C1 - O1 C2 - Distance Angles C6 1.5335 (0.0031) C3 1.5353 (0.0031) 111.66 (0.19) C1 1.5394 (0.0031) 109.55 (0.19) 113.05 (0.19) C4 1.5589 (0.0031) 113.23 (0.19) 103.46 (0.18) 105.69 (0.19) C2 - C6 C3 C1 C3 - Distance Angles O2 1.4627 (0.0026) C2 1.5353 (0.0031) 113.43 (0.18) C3 - O2 C4 - Distance Angles C5 1.5230 (0.0035) C2 1.5589 (0.0031) 116.50 (0.21) C4 - C5 C5 - Distance Angles C4 1.5230 (0.0035) C5 - C6 - Distance Angles C7 1.5266 (0.0031) C2 1.5335 (0.0031) 115.68 (0.20) C6 - C7 C7 - Distance Angles C6 1.5266 (0.0031) C7 - C8 - Distance Angles O3 1.4728 (0.0026) C9 1.5385 (0.0031) 113.55 (0.18) C8 - O3 C9 - Distance Angles C11 1.5341 (0.0032) C8 1.5385 (0.0031) 111.42 (0.19) C10 1.5392 (0.0030) 109.91 (0.19) 113.99 (0.18) C13 1.5537 (0.0030) 109.49 (0.18) 106.45 (0.18) 105.27 (0.18) C9 - C11 C8 C10 C10 - Distance Angles O4 1.4717 (0.0027) C9 1.5392 (0.0030) 113.80 (0.18) C10 - O4 C11 - Distance Angles C9 1.5341 (0.0032) C12 1.5365 (0.0032) 115.65 (0.20) C11 - C9 C12 - Distance Angles C11 1.5365 (0.0032) C12 - C13 - Distance Angles C14 1.5219 (0.0032) C9 1.5537 (0.0030) 116.94 (0.19) C13 - C14 C14 - Distance Angles C13 1.5219 (0.0032) C14 - N1 - Distance Angles P2 1.5883 (0.0019) P1 1.5909 (0.0019) 112.16 (0.11) N1 - P2 N2 - Distance Angles P3 1.5783 (0.0020) P2 1.5924 (0.0020) 118.16 (0.12) N2 - P3 N3 - Distance Angles P3 1.5828 (0.0020) P1 1.5950 (0.0020) 118.04 (0.12) N3 - P3 N4 - Distance Angles P5 1.5866 (0.0019) P4 1.5940 (0.0019) 114.39 (0.11) N4 - P5 N5 - Distance Angles P6 1.5800 (0.0019) P5 1.5905 (0.0019) 118.05 (0.12) N5 - P6 N6 - Distance Angles P6 1.5746 (0.0020) P4 1.5858 (0.0020) 120.30 (0.12) N6 - P6 O1 - Distance Angles C1 1.4708 (0.0027) P1 1.5659 (0.0016) 120.64 (0.14) O1 - C1 O2 - Distance Angles C3 1.4627 (0.0026) P2 1.5691 (0.0016) 121.09 (0.14) O2 - C3 O3 - Distance Angles C8 1.4728 (0.0026) P4 1.5627 (0.0016) 123.23 (0.14) O3 - C8 O4 - Distance Angles C10 1.4717 (0.0027) P5 1.5646 (0.0016) 122.34 (0.14) O4 - C10 P1 - Distance Angles O1 1.5659 (0.0016) N1 1.5909 (0.0019) 111.08 (0.09) N3 1.5950 (0.0020) 107.10 (0.10) 117.37 (0.10) Cl1 1.9927 (0.0008) 105.74 (0.07) 106.46 (0.07) 108.49 (0.07) P2 2.6382 (0.0008) 101.52 (0.06) 33.89 (0.07) 91.67 (0.07) 139.00 (0.04) P1 - O1 N1 N3 Cl1 P2 - Distance Angles O2 1.5691 (0.0016) N1 1.5883 (0.0019) 111.31 (0.09) N2 1.5924 (0.0020) 107.08 (0.10) 116.91 (0.10) Cl2 1.9924 (0.0008) 105.30 (0.07) 107.19 (0.07) 108.43 (0.08) P1 2.6382 (0.0008) 100.95 (0.06) 33.95 (0.07) 91.63 (0.07) 140.04 (0.03) P2 - O2 N1 N2 Cl2 P3 - Distance Angles N2 1.5783 (0.0020) N3 1.5828 (0.0020) 119.46 (0.10) Cl4 1.9879 (0.0008) 109.31 (0.08) 108.73 (0.08) Cl3 2.0169 (0.0008) 107.91 (0.08) 108.94 (0.08) 100.89 (0.04) P3 - N2 N3 Cl4 P4 - Distance Angles O3 1.5627 (0.0016) N6 1.5858 (0.0020) 107.92 (0.10) N4 1.5940 (0.0019) 111.16 (0.09) 117.18 (0.10) Cl5 1.9908 (0.0008) 104.81 (0.07) 106.97 (0.08) 108.04 (0.08) P5 2.6733 (0.0008) 106.54 (0.06) 89.98 (0.07) 32.72 (0.07) 137.39 (0.03) P4 - O3 N6 N4 Cl5 P5 - Distance Angles O4 1.5646 (0.0016) N4 1.5866 (0.0019) 111.78 (0.09) N5 1.5905 (0.0019) 107.13 (0.10) 117.74 (0.10) Cl6 1.9955 (0.0008) 105.11 (0.07) 107.00 (0.07) 107.29 (0.07) P4 2.6733 (0.0008) 104.68 (0.06) 32.89 (0.07) 91.70 (0.07) 137.69 (0.04) P5 - O4 N4 N5 Cl6 P6 - Distance Angles N6 1.5746 (0.0020) N5 1.5800 (0.0019) 119.25 (0.10) Cl7 1.9863 (0.0008) 109.97 (0.08) 108.62 (0.08) Cl8 2.0163 (0.0008) 108.09 (0.08) 108.79 (0.08) 100.48 (0.04) P6 - N6 N5 Cl7 Cl1 - Distance Angles P1 1.9927 (0.0008) Cl1 - Cl2 - Distance Angles P2 1.9924 (0.0008) Cl2 - Cl3 - Distance Angles P3 2.0169 (0.0008) Cl3 - Cl4 - Distance Angles P3 1.9879 (0.0008) Cl4 - Cl5 - Distance Angles P4 1.9908 (0.0008) Cl5 - Cl6 - Distance Angles P5 1.9955 (0.0008) Cl6 - Cl7 - Distance Angles P6 1.9863 (0.0008) Cl7 - Cl8 - Distance Angles P6 2.0163 (0.0008) Cl8 - FMAP and GRID set by program FMAP 2 1 37 GRID -1.471 -2 -1 1.471 2 1 R1 = 0.0558 for 7260 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.2741 0.8351 0.2799 [ 0.68 A from N4 ] Deepest hole -0.50 at 0.2804 0.1975 0.3378 [ 0.76 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3806 / 47105 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2741 0.6649 0.7799 1.00000 0.05 0.36 0.68 N4 1.86 P4 1.90 P5 2.30 H4A Q2 1 0.2288 0.1977 0.2493 1.00000 0.05 0.36 0.46 N1 1.77 P1 1.85 P2 2.46 H14C Q3 1 0.2470 0.4977 0.5421 1.00000 0.05 0.34 0.36 H8A 0.93 C8 1.71 H8B 1.75 O3 Q4 1 0.5313 0.6041 0.9251 1.00000 0.05 0.33 1.68 CL6 2.21 H14B 2.61 CL8 2.99 C14 Q5 1 0.0599 -0.0051 0.3336 1.00000 0.05 0.33 0.57 H1B 0.90 C1 1.58 O1 1.76 H1A Q6 1 0.2648 0.3636 0.3818 1.00000 0.05 0.32 0.58 N2 1.48 P2 2.15 P3 2.33 H13A Q7 1 0.1716 -0.0444 0.4341 1.00000 0.05 0.31 0.66 C2 0.92 C4 1.47 H4B 1.60 H4A Q8 1 0.3946 0.4868 0.6473 1.00000 0.05 0.31 0.73 C10 0.81 C9 1.39 H10B 1.41 H10A Q9 1 0.2482 0.1115 0.5920 1.00000 0.05 0.30 0.89 H7C 1.86 C7 2.11 H14B 2.25 H3A Q10 1 0.5535 0.4632 0.6341 1.00000 0.05 0.30 1.80 H10B 1.81 H12A 1.81 H12B 2.08 H11A Q11 1 0.2547 -0.2318 0.5492 1.00000 0.05 0.30 1.67 H4B 1.75 N6 1.89 O3 2.20 P4 Q12 1 0.1901 -0.0016 0.2599 1.00000 0.05 0.30 0.84 H1A 1.81 C1 2.31 H8B 2.33 H3B Q13 1 0.3648 0.9377 0.6995 1.00000 0.05 0.30 0.90 P6 1.18 CL7 2.07 N5 2.09 CL8 Q14 1 0.1946 0.2925 0.4404 1.00000 0.05 0.30 1.62 N2 1.68 O2 1.96 P2 2.27 P3 Q15 1 0.1300 0.2960 0.2686 1.00000 0.05 0.29 0.83 N3 1.19 P1 1.64 P3 1.94 N1 Q16 1 0.0741 0.4416 0.3784 1.00000 0.05 0.29 0.87 CL3 1.40 P3 2.29 CL4 2.36 N3 Q17 1 0.4557 0.1646 0.3232 1.00000 0.05 0.29 1.70 CL2 2.31 CL8 2.36 H10A 2.57 H10B Q18 1 0.0106 0.2526 0.4158 1.00000 0.05 0.29 2.06 H6A 2.26 CL3 2.46 CL5 2.49 H5A Q19 1 0.2471 0.6206 0.6212 1.00000 0.05 0.28 0.49 O3 1.23 P4 1.50 C8 1.81 H8B Q20 1 0.0171 0.1869 0.0711 1.00000 0.05 0.28 1.46 CL1 2.17 H5C 2.26 H5B 2.40 H5A Shortest distances between peaks (including symmetry equivalents) 6 14 1.81 3 19 1.99 2 15 2.04 11 19 2.17 5 7 2.28 1 12 2.39 2 12 2.52 5 12 2.57 8 10 2.59 16 18 2.63 1 19 2.64 18 20 2.66 3 8 2.70 14 16 2.72 6 15 2.74 15 16 2.78 8 19 2.84 14 15 2.86 10 13 2.87 14 18 2.94 2 6 2.97 12 19 2.97 7 12 2.98 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.01: 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 0.02: Analyse other restraints etc. 9.06: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.79: Structure factors and derivatives 8.65: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.91: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.12: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.08: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0702 finished at 22:45:09 Total CPU time: 24.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++