+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0568r started at 14:54:08 on 16-May-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0568r in Pbca CELL 0.71073 12.3344 13.3334 15.9953 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0002 0.0004 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O P CL UNIT 32 64 24 16 24 32 V = 2630.58 F(000) = 1456.0 Mu = 1.25 mm-1 Cell Wt = 2918.75 Rho = 1.842 MERG 2 OMIT 4.00 180.00 FMAP 2 PLAN 20 BOND WGHT 0.05820 5.72480 L.S. 4 FVAR 0.10375 H4B 2 1.141500 0.099500 0.628000 11.00000 0.05000 H2A 2 1.042100 -0.108600 0.606200 11.00000 0.05000 H1A 2 1.085300 0.011900 0.759200 11.00000 0.05000 H1B 2 1.057700 -0.123800 0.754200 11.00000 0.05000 H4A 2 1.153300 0.024200 0.540300 11.00000 0.05000 H3C 2 1.190600 -0.185000 0.671200 11.00000 0.05000 H3A 2 1.241400 -0.065700 0.673800 11.00000 0.05000 H3B 2 1.219500 -0.130000 0.588500 11.00000 0.05000 MOLE 1 C1 1 1.050754 -0.051244 0.727213 11.00000 0.01369 0.03221 = 0.01984 0.00183 0.00168 0.00408 C2 1 1.092017 -0.062428 0.638279 11.00000 0.01453 0.02409 = 0.02129 -0.00066 -0.00035 0.00110 C3 1 1.195199 -0.118664 0.645345 11.00000 0.01715 0.02953 = 0.02815 -0.00117 -0.00193 0.00689 C4 1 1.109583 0.044034 0.590944 11.00000 0.01188 0.03442 = 0.02213 0.00389 0.00190 0.00465 N1 3 0.979361 0.178777 0.705901 11.00000 0.01249 0.02364 = 0.01347 0.00046 0.00061 -0.00166 N2 3 0.850075 0.191691 0.575259 11.00000 0.01104 0.03985 = 0.01689 0.00617 0.00059 -0.00040 N3 3 0.791157 0.100354 0.723071 11.00000 0.01163 0.03936 = 0.01771 0.00378 0.00157 -0.00271 O1 4 0.942742 -0.026209 0.728802 11.00000 0.01254 0.02787 = 0.02220 -0.00068 0.00237 -0.00258 O2 4 1.015066 0.091867 0.560030 11.00000 0.01682 0.03255 = 0.01561 -0.00249 -0.00128 0.00480 P1 5 0.906519 0.092081 0.747624 11.00000 0.01223 0.02412 = 0.01310 0.00080 0.00054 -0.00155 P2 5 0.962921 0.186939 0.607664 11.00000 0.01131 0.02272 = 0.01391 0.00101 0.00077 -0.00127 P3 5 0.763901 0.148039 0.634016 11.00000 0.01028 0.02889 = 0.01713 0.00125 0.00044 -0.00014 CL1 6 0.916795 0.109546 0.871167 11.00000 0.02033 0.03548 = 0.01266 0.00046 0.00008 0.00009 CL2 6 1.032637 0.321095 0.569935 11.00000 0.02257 0.02954 = 0.02401 0.00619 0.00290 -0.00794 CL3 6 0.685980 0.033937 0.572053 11.00000 0.01562 0.03529 = 0.02237 -0.00269 -0.00147 -0.00329 CL4 6 0.661475 0.264171 0.648312 11.00000 0.01769 0.03581 = 0.03388 -0.00100 0.00301 0.00678 HKLF 4 Covalent radii and connectivity table for 2006src0568r in Pbca C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3 C1 C4 C3 - C2 C4 - O2 C2 N1 - P2 P1 N2 - P2 P3 N3 - P1 P3 O1 - C1 P1 O2 - C4 P2 P1 - N3 N1 O1 Cl1 P3 P2 P2 - N2 N1 O2 Cl2 P3 P1 P3 - N2 N3 Cl4 Cl3 P2 P1 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 21295 Reflections read, of which 1466 rejected -15 =< h =< 17, -16 =< k =< 16, -20 =< l =< 17, Max. 2-theta = 59.34 0 Systematic absence violations 0 Inconsistent equivalents 3013 Unique reflections, of which 650 suppressed R(int) = 0.0447 R(sigma) = 0.0331 Friedel opposites merged Maximum memory for data reduction = 1469 / 30298 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1886 / 222040 wR2 = 0.0818 before cycle 1 for 2363 data and 177 / 177 parameters GooF = S = 0.854; Restrained GooF = 0.854 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0582 * P )^2 + 5.72 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10341 0.00019 -1.803 OSF 5 0.00001 0.01194 -4.211 U11 H4B Mean shift/esd = 0.607 Maximum = -4.211 for U11 H4B Max. shift = 0.087 A for H3A Max. dU =-0.050 for H4B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1886 / 222040 wR2 = 0.0786 before cycle 2 for 2363 data and 177 / 177 parameters GooF = S = 0.822; Restrained GooF = 0.822 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0582 * P )^2 + 5.72 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10330 0.00018 -0.561 OSF Mean shift/esd = 0.179 Maximum = -0.924 for U23 C4 Max. shift = 0.033 A for H3B Max. dU =-0.005 for H1B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1886 / 222040 wR2 = 0.0784 before cycle 3 for 2363 data and 177 / 177 parameters GooF = S = 0.821; Restrained GooF = 0.821 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0582 * P )^2 + 5.72 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10330 0.00018 -0.002 OSF Mean shift/esd = 0.014 Maximum = 0.205 for z H2A Max. shift = 0.007 A for H2A Max. dU = 0.001 for H4B Least-squares cycle 4 Maximum vector length = 511 Memory required = 1886 / 222040 wR2 = 0.0784 before cycle 4 for 2363 data and 177 / 177 parameters GooF = S = 0.821; Restrained GooF = 0.821 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0582 * P )^2 + 5.72 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10330 0.00018 0.003 OSF Mean shift/esd = 0.004 Maximum = 0.031 for U11 H3A Max. shift = 0.001 A for H2A Max. dU = 0.000 for H3A No correlation matrix elements larger than 0.500 2006src0568r in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H4B 1.13899 0.09499 0.62537 1.00000 0.00183 0.04751 0.00199 0.00203 0.00160 0.00000 0.00591 H2A 1.04651 -0.10702 0.60546 1.00000 0.01854 0.05330 0.00231 0.00231 0.00193 0.00000 0.00736 H1A 1.08280 0.00798 0.75989 1.00000 0.02559 0.05686 0.00241 0.00245 0.00199 0.00000 0.00816 H1B 1.05525 -0.11917 0.75303 1.00000 0.02608 0.05373 0.00241 0.00245 0.00209 0.00000 0.00825 H4A 1.14852 0.02566 0.53884 1.00000 0.02934 0.05560 0.00251 0.00246 0.00215 0.00000 0.00858 H3C 1.18854 -0.18413 0.67297 1.00000 0.03451 0.05916 0.00268 0.00282 0.00219 0.00000 0.00933 H3A 1.23680 -0.07141 0.67186 1.00000 0.02721 0.05998 0.00265 0.00252 0.00199 0.00000 0.00831 H3B 1.21858 -0.13651 0.59365 1.00000 0.04429 0.06587 0.00305 0.00284 0.00245 0.00000 0.01059 C1 1.05078 -0.05137 0.72678 1.00000 0.01485 0.02651 0.02050 0.00197 0.00114 0.00302 0.02062 0.00508 0.00019 0.00024 0.00018 0.00000 0.00110 0.00165 0.00142 0.00127 0.00092 0.00107 0.00058 C2 1.09233 -0.06199 0.63832 1.00000 0.01387 0.02490 0.02012 -0.00328 -0.00177 -0.00053 0.01963 0.00474 0.00019 0.00023 0.00017 0.00000 0.00105 0.00153 0.00139 0.00116 0.00092 0.00107 0.00056 C3 1.19463 -0.11848 0.64547 1.00000 0.01820 0.02622 0.02558 -0.00228 -0.00132 0.00401 0.02333 0.00532 0.00022 0.00025 0.00019 0.00000 0.00120 0.00173 0.00159 0.00136 0.00106 0.00117 0.00062 C4 1.10947 0.04329 0.59112 1.00000 0.01186 0.03348 0.01969 -0.00030 0.00158 0.00385 0.02167 0.00515 0.00019 0.00024 0.00018 0.00000 0.00105 0.00179 0.00140 0.00129 0.00097 0.00109 0.00060 N1 0.97956 0.17861 0.70591 1.00000 0.01158 0.02315 0.01365 0.00025 0.00045 -0.00179 0.01613 0.00361 0.00015 0.00017 0.00013 0.00000 0.00086 0.00131 0.00107 0.00092 0.00074 0.00083 0.00046 N2 0.85026 0.19182 0.57517 1.00000 0.01083 0.04061 0.01649 0.00616 0.00043 -0.00060 0.02264 0.00410 0.00016 0.00020 0.00014 0.00000 0.00089 0.00157 0.00115 0.00104 0.00077 0.00093 0.00054 N3 0.79114 0.10033 0.72318 1.00000 0.01117 0.03986 0.01707 0.00459 0.00127 -0.00294 0.02270 0.00396 0.00016 0.00019 0.00014 0.00000 0.00092 0.00153 0.00114 0.00106 0.00076 0.00094 0.00053 O1 0.94279 -0.02621 0.72882 1.00000 0.01229 0.02689 0.02156 -0.00084 0.00231 -0.00235 0.02025 0.00318 0.00013 0.00014 0.00012 0.00000 0.00073 0.00111 0.00101 0.00084 0.00066 0.00073 0.00042 O2 1.01509 0.09184 0.56007 1.00000 0.01551 0.03166 0.01566 -0.00162 -0.00113 0.00533 0.02094 0.00325 0.00014 0.00016 0.00011 0.00000 0.00081 0.00116 0.00094 0.00082 0.00066 0.00077 0.00042 P1 0.90653 0.09213 0.74761 1.00000 0.01188 0.02418 0.01297 0.00071 0.00054 -0.00159 0.01634 0.00114 0.00005 0.00005 0.00004 0.00000 0.00026 0.00039 0.00031 0.00028 0.00022 0.00025 0.00016 P2 0.96294 0.18696 0.60767 1.00000 0.01095 0.02228 0.01377 0.00109 0.00088 -0.00142 0.01567 0.00113 0.00005 0.00005 0.00004 0.00000 0.00026 0.00040 0.00033 0.00028 0.00022 0.00024 0.00016 P3 0.76392 0.14808 0.63405 1.00000 0.00998 0.02876 0.01680 0.00133 0.00042 -0.00013 0.01851 0.00119 0.00005 0.00006 0.00004 0.00000 0.00027 0.00042 0.00034 0.00029 0.00023 0.00026 0.00017 Cl1 0.91677 0.10959 0.87120 1.00000 0.02019 0.03528 0.01249 0.00060 -0.00002 0.00013 0.02265 0.00116 0.00005 0.00006 0.00004 0.00000 0.00028 0.00042 0.00030 0.00028 0.00022 0.00027 0.00016 Cl2 1.03264 0.32108 0.56989 1.00000 0.02210 0.02935 0.02375 0.00589 0.00293 -0.00783 0.02506 0.00121 0.00005 0.00006 0.00004 0.00000 0.00030 0.00042 0.00037 0.00029 0.00024 0.00027 0.00017 Cl3 0.68599 0.03391 0.57205 1.00000 0.01522 0.03513 0.02218 -0.00279 -0.00140 -0.00334 0.02418 0.00112 0.00005 0.00006 0.00004 0.00000 0.00026 0.00043 0.00036 0.00029 0.00023 0.00026 0.00017 Cl4 0.66146 0.26413 0.64829 1.00000 0.01723 0.03577 0.03374 -0.00094 0.00305 0.00656 0.02891 0.00130 0.00005 0.00006 0.00005 0.00000 0.00028 0.00044 0.00041 0.00032 0.00025 0.00028 0.00018 Final Structure Factor Calculation for 2006src0568r in Pbca Total number of l.s. parameters = 177 Maximum vector length = 511 Memory required = 1709 / 25039 wR2 = 0.0923 before cycle 5 for 3013 data and 0 / 177 parameters GooF = S = 0.851; Restrained GooF = 0.851 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0582 * P )^2 + 5.72 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0330 for 2363 Fo > 4sig(Fo) and 0.0519 for all 3013 data wR2 = 0.0923, GooF = S = 0.851, Restrained GooF = 0.851 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0279 0.0199 0.0140 C1 0.0266 0.0191 0.0132 C2 0.0296 0.0239 0.0165 C3 0.0341 0.0200 0.0109 C4 0.0234 0.0137 0.0112 N1 0.0421 0.0151 0.0107 N2 0.0410 0.0167 0.0104 N3 0.0275 0.0218 0.0115 O1 0.0335 0.0157 0.0137 O2 0.0244 0.0132 0.0114 P1 0.0226 0.0140 0.0105 P2 0.0289 0.0167 0.0099 P3 0.0353 0.0202 0.0125 Cl1 0.0355 0.0260 0.0137 Cl2 0.0361 0.0222 0.0142 Cl3 0.0379 0.0343 0.0146 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.047 0.066 0.086 0.108 0.134 0.174 0.258 1.000 0.000 0.000 Number in group 314. 300. 294. 300. 306. 294. 301. 254. 0. 0. GooF 0.876 0.885 0.913 0.772 0.708 0.624 0.789 0.917 0.000 0.000 K 1.039 0.950 0.958 0.979 0.992 1.009 1.031 0.990 0.000 0.000 Resolution(A) 0.72 0.82 0.87 0.94 1.01 1.13 1.32 1.72 0.00 0.00 inf Number in group 307. 298. 302. 299. 300. 301. 303. 253. 0. 0. GooF 0.873 0.768 0.816 0.691 0.685 0.641 0.740 1.234 0.000 0.000 K 0.978 1.011 1.022 1.035 1.036 1.027 1.016 0.955 0.000 0.000 R1 0.054 0.044 0.041 0.032 0.028 0.022 0.021 0.035 0.000 0.000 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0390 1.8384 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 0 0 24268.22 32450.82 5.03 0.567 6.17 8 0 2 886.72 570.06 5.00 0.075 1.51 6 1 3 51.51 0.09 4.89 0.001 1.90 7 1 2 436.84 249.48 4.75 0.050 1.71 * 6 14 2 55.34 353.55 4.59 0.059 0.86 0 0 4 79033.97 99584.75 4.32 0.993 4.00 4 2 3 345.73 552.29 4.14 0.074 2.48 1 0 8 952.23 668.11 4.02 0.081 1.97 * 1 0 18 68.14 350.23 3.57 0.059 0.89 * 1 14 4 -82.17 288.19 3.52 0.053 0.92 5 2 4 182.85 306.17 3.48 0.055 2.00 10 12 5 403.04 844.61 3.36 0.091 0.80 * 6 11 8 -6.49 100.42 3.33 0.032 0.93 * 10 9 8 37.83 157.93 3.29 0.040 0.86 4 0 4 128.15 227.82 3.28 0.048 2.44 2 14 6 197.88 388.84 3.24 0.062 0.89 1 0 6 602.94 431.70 3.23 0.065 2.61 6 13 0 987.76 1470.64 3.22 0.121 0.92 * 3 1 15 -28.97 72.39 3.20 0.027 1.03 * 13 7 5 113.99 307.25 3.15 0.055 0.82 6 1 2 7318.72 6195.34 3.15 0.248 1.97 6 1 1 1438.17 1150.86 3.09 0.107 2.02 * 6 10 14 112.13 334.53 3.04 0.058 0.80 15 6 3 295.02 548.69 3.00 0.074 0.76 * 13 7 10 -63.64 168.34 3.00 0.041 0.75 9 6 12 1212.83 1643.09 2.99 0.128 0.88 6 3 0 350.38 509.22 2.97 0.071 1.87 * 11 1 16 119.24 686.69 2.96 0.082 0.75 4 3 2 593.15 439.71 2.94 0.066 2.42 13 7 9 593.36 912.50 2.91 0.095 0.77 * 0 2 18 31.71 217.28 2.84 0.046 0.88 * 6 13 2 -56.35 80.91 2.81 0.028 0.91 4 1 6 1482.78 1211.56 2.80 0.110 1.99 4 9 4 193.64 304.65 2.78 0.055 1.27 2 14 0 6835.94 5750.18 2.75 0.239 0.94 * 13 10 1 117.87 331.57 2.75 0.057 0.77 6 5 9 59.51 0.19 2.72 0.001 1.20 * 1 5 19 -36.69 158.22 2.71 0.040 0.80 12 4 14 252.20 434.47 2.71 0.066 0.74 12 8 7 346.41 554.44 2.70 0.074 0.82 3 1 4 602.98 775.74 2.70 0.088 2.80 6 3 2 252.92 172.21 2.69 0.041 1.82 * 3 12 8 7.37 109.30 2.66 0.033 0.95 4 10 14 158.26 0.70 2.65 0.003 0.84 * 9 5 5 -6.43 20.80 2.65 0.014 1.14 0 2 1 74413.27 85176.81 2.62 0.919 6.15 4 0 2 3201.91 3751.93 2.62 0.193 2.88 * 8 6 7 16.95 75.16 2.58 0.027 1.11 * 11 2 11 50.67 126.36 2.58 0.035 0.88 0 4 1 141.16 223.47 2.53 0.047 3.26 Bond lengths and angles C1 - Distance Angles O1 1.3740 (0.0028) C2 1.5115 (0.0038) 111.95 (0.22) C1 - O1 C2 - Distance Angles C3 1.4740 (0.0036) C1 1.5115 (0.0038) 105.39 (0.23) C4 1.6078 (0.0043) 111.72 (0.22) 113.73 (0.24) C2 - C3 C1 C3 - Distance Angles C2 1.4740 (0.0036) C3 - C4 - Distance Angles O2 1.4216 (0.0031) C2 1.6078 (0.0043) 117.00 (0.21) C4 - O2 N1 - Distance Angles P2 1.5887 (0.0022) P1 1.6081 (0.0022) 112.84 (0.13) N1 - P2 N2 - Distance Angles P2 1.4853 (0.0021) P3 1.5366 (0.0022) 114.67 (0.15) N2 - P2 N3 - Distance Angles P1 1.4800 (0.0021) P3 1.5971 (0.0024) 117.86 (0.14) N3 - P1 O1 - Distance Angles C1 1.3740 (0.0028) P1 1.6673 (0.0020) 119.70 (0.18) O1 - C1 O2 - Distance Angles C4 1.4216 (0.0031) P2 1.6130 (0.0020) 121.31 (0.17) O2 - C4 P1 - Distance Angles N3 1.4800 (0.0021) N1 1.6081 (0.0022) 112.10 (0.12) O1 1.6673 (0.0020) 106.28 (0.12) 116.97 (0.10) Cl1 1.9945 (0.0009) 108.30 (0.10) 106.97 (0.09) 105.79 (0.08) P3 2.6363 (0.0009) 32.39 (0.09) 83.40 (0.08) 108.82 (0.07) 133.80 (0.04) P2 2.6633 (0.0010) 89.67 (0.09) 33.35 (0.08) 103.16 (0.07) 139.56 (0.04) 57.38 (0.02) P1 - N3 N1 O1 Cl1 P3 P2 - Distance Angles N2 1.4853 (0.0021) N1 1.5887 (0.0022) 118.04 (0.11) O2 1.6130 (0.0020) 104.02 (0.12) 111.13 (0.11) Cl2 2.0742 (0.0010) 104.37 (0.11) 107.16 (0.09) 112.03 (0.08) P3 2.5441 (0.0008) 33.29 (0.09) 86.92 (0.08) 107.63 (0.07) 128.60 (0.04) P1 2.6633 (0.0010) 94.04 (0.09) 33.81 (0.08) 97.34 (0.08) 139.68 (0.04) 60.78 (0.02) P2 - N2 N1 O2 Cl2 P3 P3 - Distance Angles N2 1.5366 (0.0022) N3 1.5971 (0.0024) 123.56 (0.11) Cl4 2.0109 (0.0010) 102.30 (0.11) 109.74 (0.09) Cl3 2.0554 (0.0010) 108.03 (0.10) 103.52 (0.10) 109.31 (0.04) P2 2.5441 (0.0008) 32.04 (0.08) 91.52 (0.08) 117.93 (0.04) 121.48 (0.04) P1 2.6363 (0.0009) 93.86 (0.09) 29.76 (0.07) 123.99 (0.04) 115.78 (0.04) 61.85 (0.02) P3 - N2 N3 Cl4 Cl3 P2 Cl1 - Distance Angles P1 1.9945 (0.0009) Cl1 - Cl2 - Distance Angles P2 2.0742 (0.0010) Cl2 - Cl3 - Distance Angles P3 2.0554 (0.0010) Cl3 - Cl4 - Distance Angles P3 2.0109 (0.0010) Cl4 - FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 24 -2 1.563 1 2 R1 = 0.0331 for 2363 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.7047 0.0388 0.2925 [ 1.02 A from H3A ] Deepest hole -0.47 at 0.3768 0.0402 0.7463 [ 0.79 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2221 / 29399 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2953 -0.0388 0.7075 1.00000 0.05 0.32 1.02 H3A 1.91 C3 2.09 O1 2.16 N3 Q2 1 0.6802 -0.0701 0.6501 1.00000 0.05 0.29 1.87 CL3 2.14 H1A 2.28 H1B 2.55 C1 Q3 1 0.9603 -0.0607 0.5793 1.00000 0.05 0.28 1.30 H2A 1.88 C2 2.17 O2 2.29 O2 Q4 1 0.8981 0.0391 0.9191 1.00000 0.05 0.28 1.23 CL1 2.83 CL3 2.83 P1 2.87 H3A Q5 1 1.1106 -0.0005 0.6321 1.00000 0.05 0.28 0.86 C2 0.88 C4 1.32 H4B 1.60 H4A Q6 1 0.8350 0.0200 0.7436 1.00000 0.05 0.27 1.24 N3 1.31 P1 1.48 O1 2.19 H3A Q7 1 0.7829 0.0684 0.6977 1.00000 0.05 0.27 0.60 N3 1.49 P3 1.75 P1 2.38 CL3 Q8 1 0.9178 0.1100 0.9819 1.00000 0.05 0.27 1.77 CL1 2.20 CL2 2.72 CL3 3.15 N2 Q9 1 1.2574 -0.0601 0.5745 1.00000 0.05 0.27 1.17 H3B 1.58 C3 1.59 H3A 1.85 H4A Q10 1 0.7987 0.0386 0.6871 1.00000 0.05 0.26 1.01 N3 1.74 P3 1.79 P1 2.09 O1 Q11 1 0.9482 0.1812 0.7032 1.00000 0.05 0.26 0.39 N1 1.48 P1 1.54 P2 2.24 N3 Q12 1 0.9936 0.1279 0.7160 1.00000 0.05 0.26 0.72 N1 1.28 P1 1.94 P2 2.06 H1A Q13 1 0.6776 0.1980 0.6570 1.00000 0.05 0.26 0.91 CL4 1.31 P3 2.19 N3 2.50 N2 Q14 1 0.6851 0.1548 0.5030 1.00000 0.05 0.25 1.95 CL3 1.96 H3B 2.24 CL2 2.31 P3 Q15 1 1.3010 -0.1351 0.5534 1.00000 0.05 0.25 1.20 H3B 1.98 C3 2.15 CL2 2.22 H3A Q16 1 0.9840 0.1077 0.6919 1.00000 0.05 0.24 0.97 N1 1.32 P1 1.73 P2 1.95 O1 Q17 1 0.6792 0.1700 0.7562 1.00000 0.05 0.24 1.75 N3 2.15 CL4 2.20 H4B 2.24 P3 Q18 1 1.2335 0.1439 0.4963 1.00000 0.05 0.24 2.01 H4A 2.46 H4B 2.54 C4 2.76 CL4 Q19 1 0.9063 -0.0873 0.7153 1.00000 0.05 0.24 0.96 O1 1.85 C1 1.98 H1B 2.40 CL4 Q20 1 0.9573 0.0314 0.8619 1.00000 0.05 0.24 1.17 CL1 2.09 P1 2.27 O1 2.27 H1A Shortest distances between peaks (including symmetry equivalents) 7 10 0.47 12 16 0.48 11 12 0.93 14 15 0.95 6 10 1.04 11 16 1.09 6 7 1.17 4 20 1.18 9 15 1.18 1 6 1.21 4 8 1.40 13 17 1.63 6 19 1.74 9 14 1.91 1 19 1.95 1 10 1.98 7 17 2.09 1 7 2.09 2 10 2.14 5 9 2.18 4 9 2.18 10 19 2.19 3 5 2.19 1 9 2.20 8 20 2.24 7 13 2.26 3 19 2.30 6 16 2.33 5 16 2.33 8 18 2.34 2 7 2.36 12 17 2.40 6 20 2.42 10 16 2.47 6 12 2.47 1 20 2.47 13 14 2.53 7 11 2.53 7 16 2.54 10 17 2.54 7 19 2.59 1 4 2.60 5 12 2.61 1 5 2.63 6 11 2.64 10 13 2.64 4 15 2.65 10 11 2.66 16 17 2.68 12 20 2.70 2 6 2.71 1 2 2.72 10 12 2.72 7 12 2.73 14 18 2.75 2 18 2.75 1 15 2.78 6 17 2.78 16 19 2.80 4 18 2.81 3 16 2.89 19 20 2.90 3 18 2.90 16 20 2.92 4 6 2.92 11 17 2.93 9 20 2.93 3 10 2.95 2 19 2.99 2 8 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 4.86: 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 1.07: Structure factors and derivatives 0.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.32: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.04: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0568r finished at 14:54:19 Total CPU time: 7.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++