+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0700 started at 22:35:22 on 02-Jun-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0700 in Pbca CELL 0.71073 13.0288 12.2797 18.0331 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0004 0.0005 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 BR UNIT 24 32 32 32 24 32 8 V = 2885.11 F(000) = 1840.0 Mu = 3.93 mm-1 Cell Wt = 3797.78 Rho = 2.186 MERG 2 OMIT -3.00 55.00 OMIT 0 2 1 OMIT 1 1 1 OMIT 2 0 0 OMIT 0 8 20 FMAP 2 PLAN 20 SIZE 0.10 0.25 0.50 ACTA BOND WGHT 0.04610 5.36240 L.S. 4 TEMP -153.00 FVAR 0.19892 MOLE 1 C1 1 0.220035 0.067271 0.323063 11.00000 0.02047 0.02260 = 0.01369 0.00143 -0.00297 -0.00331 AFIX 23 H1A 2 0.147322 0.047292 0.331366 11.00000 -1.20000 H1B 2 0.241060 0.039091 0.273921 11.00000 -1.20000 AFIX 0 C2 1 0.231808 0.190776 0.324915 11.00000 0.01527 0.01887 = 0.01233 -0.00054 -0.00520 0.00144 C3 1 0.207376 0.237754 0.400563 11.00000 0.02658 0.01998 = 0.01438 0.00289 -0.00313 0.00496 AFIX 23 H3A 2 0.218456 0.317511 0.400110 11.00000 -1.20000 H3B 2 0.134530 0.223785 0.412950 11.00000 -1.20000 AFIX 0 N1 3 0.370368 0.025576 0.506261 11.00000 0.01550 0.03430 = 0.02105 0.01251 0.00111 -0.00234 N2 3 0.254578 -0.054504 0.619793 11.00000 0.01368 0.03036 = 0.01442 0.00759 0.00164 0.00223 N3 3 0.163140 0.019827 0.494610 11.00000 0.01720 0.03399 = 0.01539 0.00597 -0.00397 -0.00263 N4 3 0.340571 0.222854 0.302244 11.00000 0.02154 0.02764 = 0.01379 0.00574 -0.00230 -0.00386 O1 4 0.272931 0.187911 0.455523 11.00000 0.03053 0.01815 = 0.01294 0.00086 -0.00623 -0.00086 O2 4 0.283564 0.019686 0.380327 11.00000 0.02797 0.01299 = 0.01542 0.00104 0.00143 0.00386 O3 4 0.389838 0.157324 0.265720 11.00000 0.02261 0.04303 = 0.03292 0.00042 0.00977 -0.00012 O4 4 0.369960 0.313519 0.320121 11.00000 0.03675 0.02745 = 0.05082 0.00355 -0.00287 -0.01768 P1 5 0.270630 0.059640 0.463030 11.00000 0.01831 0.01799 = 0.01271 0.00327 -0.00025 -0.00122 P2 5 0.364015 -0.035191 0.583137 11.00000 0.01212 0.02043 = 0.01503 0.00466 0.00037 -0.00004 P3 5 0.153543 -0.036069 0.572831 11.00000 0.01233 0.01763 = 0.01502 0.00047 0.00042 -0.00116 CL1 6 0.437003 -0.177689 0.573259 11.00000 0.02466 0.02399 = 0.02261 0.00274 0.00604 0.00554 CL2 6 0.450536 0.042935 0.656748 11.00000 0.02318 0.03161 = 0.02864 -0.00265 -0.00737 -0.00365 CL3 6 0.080745 -0.178340 0.562269 11.00000 0.02419 0.02025 = 0.03552 -0.00895 0.00697 -0.00529 CL4 6 0.053805 0.046485 0.635204 11.00000 0.01671 0.02114 = 0.02504 -0.00567 0.00232 0.00120 BR1 7 0.141260 0.255789 0.253864 11.00000 0.03126 0.04169 = 0.01958 -0.00013 -0.01071 0.01519 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 2006src0700 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 BR 1.140 C1 - O2 C2 C2 - C3 C1 N4 Br1 C3 - O1 C2 N1 - P1 P2 N2 - P3 P2 N3 - P3 P1 N4 - O4 O3 C2 O1 - C3 P1 O2 - C1 P1 O3 - N4 O4 - N4 P1 - N1 O2 O1 N3 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl4 Cl3 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Br1 - C2 h k l Fo^2 Sigma Why rejected 3 1 0 4.27 1.05 observed but should be systematically absent 25767 Reflections read, of which 1865 rejected -16 =< h =< 14, -15 =< k =< 14, -19 =< l =< 23, Max. 2-theta = 55.00 1 Systematic absence violations 0 Inconsistent equivalents 3290 Unique reflections, of which 0 suppressed R(int) = 0.0570 R(sigma) = 0.0368 Friedel opposites merged Maximum memory for data reduction = 1428 / 32613 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 = 1840 / 217067 wR2 = 0.0981 before cycle 1 for 3290 data and 172 / 172 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0461 * P )^2 + 5.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19892 0.00038 -0.004 OSF Mean shift/esd = 0.003 Maximum = -0.018 for U11 Br1 Max. shift = 0.000 A for O4 Max. dU = 0.000 for O4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1840 / 217067 wR2 = 0.0981 before cycle 2 for 3290 data and 172 / 172 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0461 * P )^2 + 5.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19892 0.00038 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U11 Br1 Max. shift = 0.000 A for O4 Max. dU = 0.000 for Cl4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1840 / 217067 wR2 = 0.0981 before cycle 3 for 3290 data and 172 / 172 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0461 * P )^2 + 5.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19892 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z P3 Max. shift = 0.000 A for N1 Max. dU = 0.000 for N4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1840 / 217067 wR2 = 0.0981 before cycle 4 for 3290 data and 172 / 172 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0461 * P )^2 + 5.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19892 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z P3 Max. shift = 0.000 A for N3 Max. dU = 0.000 for N3 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 0.1473 0.0473 0.3314 23 0.990 0.000 C1 O2 C2 H1B 0.2411 0.0391 0.2739 23 0.990 0.000 C1 O2 C2 H3A 0.2185 0.3175 0.4001 23 0.990 0.000 C3 O1 C2 H3B 0.1345 0.2238 0.4129 23 0.990 0.000 C3 O1 C2 2006src0700 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.22004 0.06727 0.32306 1.00000 0.02047 0.02260 0.01369 0.00143 -0.00297 -0.00331 0.01892 0.00590 0.00027 0.00030 0.00018 0.00000 0.00176 0.00183 0.00156 0.00134 0.00136 0.00150 0.00072 H1A 0.14732 0.04729 0.33137 1.00000 0.02270 0.00000 0.00000 H1B 0.24106 0.03909 0.27392 1.00000 0.02270 0.00000 0.00000 C2 0.23181 0.19078 0.32492 1.00000 0.01527 0.01887 0.01233 -0.00054 -0.00520 0.00144 0.01549 0.00567 0.00025 0.00028 0.00018 0.00000 0.00170 0.00176 0.00151 0.00125 0.00127 0.00137 0.00070 C3 0.20738 0.23775 0.40056 1.00000 0.02658 0.01998 0.01438 0.00289 -0.00314 0.00495 0.02031 0.00639 0.00030 0.00030 0.00018 0.00000 0.00189 0.00184 0.00160 0.00136 0.00143 0.00153 0.00075 H3A 0.21846 0.31751 0.40011 1.00000 0.02438 0.00000 0.00000 H3B 0.13453 0.22378 0.41295 1.00000 0.02438 0.00000 0.00000 N1 0.37037 0.02558 0.50626 1.00000 0.01550 0.03430 0.02105 0.01251 0.00112 -0.00234 0.02362 0.00572 0.00023 0.00029 0.00017 0.00000 0.00151 0.00193 0.00154 0.00135 0.00119 0.00134 0.00072 N2 0.25458 -0.05450 0.61979 1.00000 0.01368 0.03036 0.01442 0.00759 0.00164 0.00223 0.01949 0.00531 0.00021 0.00026 0.00016 0.00000 0.00140 0.00174 0.00136 0.00120 0.00111 0.00127 0.00064 N3 0.16314 0.01983 0.49461 1.00000 0.01720 0.03399 0.01539 0.00597 -0.00397 -0.00263 0.02219 0.00540 0.00023 0.00028 0.00016 0.00000 0.00155 0.00184 0.00141 0.00124 0.00115 0.00139 0.00068 N4 0.34057 0.22285 0.30224 1.00000 0.02154 0.02764 0.01379 0.00574 -0.00230 -0.00386 0.02099 0.00532 0.00023 0.00026 0.00016 0.00000 0.00162 0.00172 0.00137 0.00123 0.00123 0.00139 0.00066 O1 0.27293 0.18791 0.45552 1.00000 0.03053 0.01815 0.01294 0.00086 -0.00622 -0.00086 0.02054 0.00410 0.00020 0.00020 0.00013 0.00000 0.00144 0.00132 0.00110 0.00094 0.00102 0.00108 0.00055 O2 0.28356 0.01969 0.38033 1.00000 0.02797 0.01299 0.01542 0.00104 0.00143 0.00386 0.01879 0.00425 0.00019 0.00019 0.00013 0.00000 0.00132 0.00120 0.00117 0.00092 0.00102 0.00104 0.00052 O3 0.38984 0.15732 0.26572 1.00000 0.02261 0.04304 0.03292 0.00042 0.00977 -0.00012 0.03286 0.00526 0.00021 0.00026 0.00016 0.00000 0.00145 0.00180 0.00155 0.00136 0.00121 0.00133 0.00068 O4 0.36996 0.31352 0.32012 1.00000 0.03675 0.02744 0.05081 0.00355 -0.00287 -0.01768 0.03834 0.00513 0.00023 0.00024 0.00018 0.00000 0.00169 0.00165 0.00191 0.00141 0.00145 0.00133 0.00075 P1 0.27063 0.05964 0.46303 1.00000 0.01831 0.01798 0.01271 0.00327 -0.00025 -0.00122 0.01633 0.00154 0.00007 0.00007 0.00005 0.00000 0.00045 0.00046 0.00040 0.00032 0.00034 0.00036 0.00020 P2 0.36401 -0.03519 0.58314 1.00000 0.01212 0.02043 0.01503 0.00466 0.00037 -0.00004 0.01586 0.00154 0.00006 0.00008 0.00005 0.00000 0.00042 0.00048 0.00041 0.00034 0.00033 0.00035 0.00020 P3 0.15354 -0.03607 0.57283 1.00000 0.01233 0.01763 0.01502 0.00047 0.00042 -0.00116 0.01499 0.00149 0.00007 0.00007 0.00005 0.00000 0.00041 0.00046 0.00040 0.00033 0.00032 0.00035 0.00019 Cl1 0.43700 -0.17769 0.57326 1.00000 0.02466 0.02399 0.02261 0.00274 0.00604 0.00554 0.02375 0.00165 0.00007 0.00008 0.00005 0.00000 0.00047 0.00047 0.00043 0.00035 0.00035 0.00037 0.00021 Cl2 0.45054 0.04293 0.65675 1.00000 0.02318 0.03161 0.02864 -0.00265 -0.00737 -0.00365 0.02781 0.00154 0.00007 0.00008 0.00005 0.00000 0.00046 0.00054 0.00046 0.00039 0.00038 0.00040 0.00022 Cl3 0.08075 -0.17834 0.56227 1.00000 0.02419 0.02025 0.03552 -0.00895 0.00697 -0.00529 0.02665 0.00158 0.00007 0.00008 0.00005 0.00000 0.00047 0.00046 0.00051 0.00038 0.00039 0.00038 0.00022 Cl4 0.05381 0.04648 0.63520 1.00000 0.01671 0.02114 0.02504 -0.00567 0.00232 0.00120 0.02097 0.00146 0.00006 0.00007 0.00005 0.00000 0.00041 0.00045 0.00042 0.00034 0.00033 0.00035 0.00020 Br1 0.14126 0.25579 0.25386 1.00000 0.03125 0.04168 0.01958 -0.00013 -0.01071 0.01519 0.03084 0.00072 0.00003 0.00004 0.00002 0.00000 0.00023 0.00026 0.00020 0.00016 0.00016 0.00018 0.00014 Final Structure Factor Calculation for 2006src0700 in Pbca Total number of l.s. parameters = 172 Maximum vector length = 511 Memory required = 1668 / 26061 wR2 = 0.0981 before cycle 5 for 3290 data and 0 / 172 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0461 * P )^2 + 5.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0384 for 2642 Fo > 4sig(Fo) and 0.0559 for all 3290 data wR2 = 0.0981, GooF = S = 1.083, Restrained GooF = 1.083 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0257 0.0185 0.0126 C1 0.0205 0.0176 0.0084 C2 0.0294 0.0201 0.0115 C3 0.0419 0.0168 0.0121 N1 0.0338 0.0135 0.0112 N2 0.0364 0.0184 0.0117 N3 0.0316 0.0197 0.0116 N4 0.0326 0.0181 0.0109 O1 0.0291 0.0154 0.0119 O2 0.0431 0.0388 0.0167 O3 0.0551 0.0462 0.0138 O4 0.0203 0.0176 0.0111 P1 0.0231 0.0126 0.0119 P2 0.0179 0.0151 0.0120 P3 0.0336 0.0207 0.0170 Cl1 0.0338 0.0330 0.0167 Cl2 0.0435 0.0210 0.0155 Cl3 0.0292 0.0192 0.0145 Cl4 0.0538 0.0279 0.0108 Br1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.035 0.049 0.062 0.078 0.099 0.131 0.186 1.000 Number in group 352. 308. 357. 312. 325. 327. 331. 324. 327. 327. GooF 1.105 1.196 1.152 1.075 0.976 1.024 1.093 0.972 0.984 1.217 K 1.494 1.071 0.964 0.991 0.981 0.986 0.983 1.002 1.013 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 330. 337. 338. 315. 331. 324. 328. 332. 326. 329. GooF 1.022 0.919 0.940 0.912 0.939 1.009 0.983 1.121 1.130 1.652 K 0.956 0.996 1.009 1.020 1.014 1.012 1.022 1.021 1.013 0.978 R1 0.131 0.096 0.081 0.067 0.059 0.051 0.039 0.035 0.031 0.039 Recommended weighting scheme: WGHT 0.0461 5.3605 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) 4 6 1 356.84 109.00 5.33 0.020 1.72 1 1 2 1247.97 2409.52 5.23 0.095 6.35 0 2 8 906.10 517.24 4.96 0.044 2.12 0 2 23 1143.59 2136.52 4.76 0.089 0.78 0 4 3 5058.96 3767.10 4.48 0.119 2.73 0 6 1 533.58 236.99 4.38 0.030 2.03 2 1 2 22789.35 29341.19 4.28 0.331 4.85 3 2 13 489.07 272.99 3.87 0.032 1.29 6 4 7 531.94 293.31 3.78 0.033 1.46 2 1 0 10077.93 12619.71 3.75 0.217 5.75 2 1 4 12493.96 15417.14 3.71 0.240 3.55 1 4 2 93.10 11.60 3.65 0.007 2.84 0 6 0 2518.02 1858.21 3.59 0.083 2.05 9 4 12 471.76 56.85 3.52 0.015 0.99 6 8 5 377.52 179.00 3.44 0.026 1.18 5 4 2 923.51 635.12 3.44 0.049 1.94 4 13 7 419.80 822.67 3.21 0.055 0.86 2 4 7 88.81 13.48 3.19 0.007 1.89 2 4 2 1002.68 735.50 3.14 0.052 2.65 4 1 6 2555.89 3188.36 3.13 0.109 2.17 0 6 11 291.60 106.40 3.10 0.020 1.28 1 5 2 181.37 83.23 3.07 0.018 2.33 2 3 0 34280.63 40555.98 3.03 0.389 3.47 3 7 9 181.50 53.07 3.02 0.014 1.26 13 2 5 297.29 83.02 3.01 0.018 0.95 16 2 7 14.26 1128.03 3.00 0.065 0.77 4 1 4 5365.63 6450.29 2.91 0.155 2.58 1 10 17 770.90 1130.10 2.90 0.065 0.80 4 1 0 3221.42 3923.60 2.89 0.121 3.15 1 6 1 1712.69 1343.20 2.88 0.071 2.01 6 0 4 27191.43 23296.58 2.86 0.295 1.96 1 4 8 420.56 244.35 2.85 0.030 1.80 1 7 4 233.99 105.11 2.84 0.020 1.62 3 1 4 4606.36 5497.09 2.82 0.143 3.03 0 8 1 3587.93 2933.07 2.81 0.105 1.53 8 1 2 767.27 1026.75 2.78 0.062 1.59 8 0 10 381.31 196.85 2.78 0.027 1.21 2 3 8 24247.86 28166.06 2.76 0.324 1.89 15 2 10 1628.96 2452.02 2.76 0.096 0.78 7 5 11 -42.66 101.20 2.75 0.019 1.10 2 3 3 4498.46 5346.74 2.71 0.141 3.00 2 1 6 51286.93 59246.17 2.71 0.471 2.66 2 3 1 1689.72 2094.44 2.70 0.088 3.40 3 7 8 116.27 6.04 2.70 0.005 1.32 6 1 15 92.93 257.89 2.66 0.031 1.05 7 11 2 240.35 0.59 2.64 0.001 0.95 10 9 10 200.23 571.56 2.60 0.046 0.84 3 7 6 96.14 9.23 2.57 0.006 1.43 4 2 6 7097.73 6101.95 2.57 0.151 2.08 2 1 5 5772.23 6744.86 2.55 0.159 3.06 Bond lengths and angles C1 - Distance Angles O2 1.4467 (0.0041) C2 1.5247 (0.0049) 109.18 (0.26) C1 - O2 C2 - Distance Angles C3 1.5149 (0.0046) C1 1.5247 (0.0049) 112.17 (0.28) N4 1.5265 (0.0044) 109.75 (0.28) 110.13 (0.28) Br1 1.9159 (0.0032) 108.31 (0.23) 109.75 (0.22) 106.56 (0.21) C2 - C3 C1 N4 C3 - Distance Angles O1 1.4444 (0.0041) C2 1.5149 (0.0046) 109.41 (0.28) C3 - O1 N1 - Distance Angles P1 1.5721 (0.0031) P2 1.5766 (0.0030) 121.24 (0.19) N1 - P1 N2 - Distance Angles P3 1.5815 (0.0029) P2 1.5894 (0.0029) 120.17 (0.18) N2 - P3 N3 - Distance Angles P3 1.5737 (0.0029) P1 1.5889 (0.0031) 121.70 (0.19) N3 - P3 N4 - Distance Angles O4 1.2207 (0.0043) O3 1.2220 (0.0042) 125.32 (0.33) C2 1.5265 (0.0044) 117.12 (0.31) 117.52 (0.30) N4 - O4 O3 O1 - Distance Angles C3 1.4444 (0.0041) P1 1.5812 (0.0026) 118.01 (0.22) O1 - C3 O2 - Distance Angles C1 1.4467 (0.0041) P1 1.5790 (0.0024) 119.18 (0.21) O2 - C1 O3 - Distance Angles N4 1.2220 (0.0042) O3 - O4 - Distance Angles N4 1.2207 (0.0043) O4 - P1 - Distance Angles N1 1.5721 (0.0031) O2 1.5790 (0.0024) 107.31 (0.16) O1 1.5812 (0.0026) 106.97 (0.17) 103.10 (0.13) N3 1.5889 (0.0031) 117.97 (0.16) 109.69 (0.15) 110.73 (0.17) P1 - N1 O2 O1 P2 - Distance Angles N1 1.5766 (0.0030) N2 1.5894 (0.0029) 118.91 (0.16) Cl2 1.9883 (0.0013) 109.20 (0.13) 107.63 (0.12) Cl1 1.9995 (0.0013) 108.11 (0.14) 109.46 (0.13) 102.25 (0.05) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5737 (0.0029) N2 1.5815 (0.0029) 118.44 (0.16) Cl4 1.9953 (0.0012) 109.60 (0.13) 108.24 (0.12) Cl3 1.9970 (0.0013) 109.50 (0.13) 108.73 (0.13) 100.89 (0.05) P3 - N3 N2 Cl4 Cl1 - Distance Angles P2 1.9995 (0.0013) Cl1 - Cl2 - Distance Angles P2 1.9883 (0.0013) Cl2 - Cl3 - Distance Angles P3 1.9970 (0.0013) Cl3 - Cl4 - Distance Angles P3 1.9953 (0.0012) Cl4 - Br1 - Distance Angles C2 1.9159 (0.0032) Br1 - FMAP and GRID set by program FMAP 2 1 17 GRID -1.786 -2 -1 1.786 2 1 R1 = 0.0538 for 3290 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.35 at 0.1484 0.7618 0.2505 [ 1.06 A from N4 ] Deepest hole -0.85 at 0.1091 0.2322 0.2550 [ 0.51 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 2179 / 27978 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3516 0.2618 0.2505 1.00000 0.05 2.35 1.06 N4 1.40 O3 1.43 O4 2.24 C2 Q2 1 0.2106 0.0571 0.4636 1.00000 0.05 0.86 0.78 P1 0.95 N3 1.81 O1 1.84 O2 Q3 1 0.4492 0.0444 0.6217 1.00000 0.05 0.60 0.63 CL2 1.63 P2 2.33 N1 2.81 N2 Q4 1 0.0912 0.1328 0.2659 1.00000 0.05 0.46 1.66 BR1 1.74 H1A 2.13 C1 2.23 C2 Q5 1 0.2070 0.1924 0.4460 1.00000 0.05 0.46 0.88 O1 0.99 C3 1.18 H3B 1.75 H3A Q6 1 0.1228 0.3004 0.3271 1.00000 0.05 0.46 1.45 BR1 1.82 H3B 1.83 H3A 1.89 C3 Q7 1 0.2186 0.0189 0.3799 1.00000 0.05 0.44 0.85 O2 1.19 C1 1.32 H1A 1.72 P1 Q8 1 0.3223 0.0419 0.5018 1.00000 0.05 0.41 0.66 N1 0.99 P1 1.83 P2 2.08 O1 Q9 1 0.2181 0.3624 0.1883 1.00000 0.05 0.40 2.03 BR1 2.60 CL4 2.71 N2 2.72 H1B Q10 1 0.2230 0.2088 0.3615 1.00000 0.05 0.39 0.71 C2 0.82 C3 1.49 H3B 1.51 H3A Q11 1 0.2963 0.0761 0.3204 1.00000 0.05 0.38 1.00 C1 1.19 H1B 1.29 O2 1.64 C2 Q12 1 0.4140 0.0613 0.6725 1.00000 0.05 0.37 0.60 CL2 2.10 P2 2.69 N2 2.99 H1B Q13 1 0.0561 0.2911 0.4307 1.00000 0.05 0.36 1.35 H3B 2.15 C3 2.21 H3A 2.26 CL3 Q14 1 0.5348 0.1780 0.6654 1.00000 0.05 0.36 2.00 CL2 2.17 BR1 2.27 H3B 2.67 H3A Q15 1 0.0029 -0.3056 0.5983 1.00000 0.05 0.36 1.97 CL3 2.06 H3B 2.22 CL2 2.86 C3 Q16 1 0.0545 0.3031 0.3689 1.00000 0.05 0.36 1.63 H3B 2.22 H3A 2.22 C3 2.37 CL2 Q17 1 0.5155 -0.0969 0.6386 1.00000 0.05 0.35 1.85 CL1 1.94 CL2 2.25 O3 2.34 P2 Q18 1 0.1821 0.2117 0.3077 1.00000 0.05 0.34 0.76 C2 1.23 BR1 1.74 C3 1.86 C1 Q19 1 0.0522 -0.1774 0.5863 1.00000 0.05 0.34 0.57 CL3 2.19 P3 2.50 H3B 2.89 CL4 Q20 1 0.2324 0.1385 0.3207 1.00000 0.05 0.33 0.65 C2 0.89 C1 1.49 H1B 1.59 H1A Shortest distances between peaks (including symmetry equivalents) 14 16 0.71 13 15 0.95 15 16 0.95 3 12 1.04 10 18 1.11 13 16 1.12 11 20 1.13 18 20 1.14 10 20 1.14 6 16 1.17 6 14 1.18 14 15 1.32 6 18 1.38 5 10 1.55 2 7 1.58 2 8 1.62 7 11 1.63 2 5 1.69 4 18 1.70 15 19 1.71 13 14 1.79 7 20 1.82 6 10 1.83 3 17 1.96 3 15 1.99 13 19 2.01 10 11 2.03 6 13 2.06 4 20 2.09 6 15 2.12 12 14 2.13 3 14 2.13 16 19 2.23 11 18 2.24 16 18 2.29 5 13 2.33 3 16 2.33 7 10 2.36 4 6 2.37 12 15 2.37 5 20 2.38 14 18 2.40 1 9 2.41 12 17 2.43 5 7 2.45 6 20 2.45 10 16 2.49 1 20 2.51 1 18 2.51 5 18 2.53 14 19 2.54 11 17 2.57 12 16 2.58 5 8 2.59 7 8 2.59 4 10 2.61 2 10 2.62 3 13 2.63 1 10 2.69 1 11 2.70 10 13 2.70 1 12 2.71 4 17 2.72 3 8 2.72 4 14 2.73 9 12 2.73 7 18 2.74 5 6 2.75 2 20 2.78 5 16 2.78 2 11 2.82 4 16 2.84 10 14 2.86 9 18 2.88 6 9 2.89 4 12 2.92 5 11 2.92 13 18 2.93 4 11 2.93 1 14 2.93 4 7 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.01: 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. 4.94: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.28: Structure factors and derivatives 1.24: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.03: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0700 finished at 22:35:35 Total CPU time: 8.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++