+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005sjc0007 started at 19:44:08 on 17-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005sjc0007 in Pna2(1) CELL 0.71073 13.4804 10.6442 8.8479 90.000 90.000 90.000 ZERR 4.00 0.0014 0.0009 0.0007 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 P CL O UNIT 12 24 12 12 16 8 V = 1269.57 F(000) = 696.0 Mu = 1.29 mm-1 Cell Wt = 1403.27 Rho = 1.835 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 OMIT 4 0 0 OMIT 1 1 -1 OMIT 2 0 2 OMIT 1 1 2 OMIT 1 1 -2 OMIT 3 1 0 OMIT 1 1 1 EXTI 0.00554 FMAP 2 PLAN 20 SIZE 0.10 0.12 0.45 ACTA BOND WGHT 0.04810 0.42630 L.S. 4 TEMP 1.00 FVAR 0.88336 C1 1 0.522120 0.866573 0.314673 11.00000 0.05864 0.08935 = 0.04491 -0.00614 -0.00832 0.03331 AFIX 23 H1A 2 0.557348 0.788799 0.295079 11.00000 -1.20000 H1B 2 0.507582 0.870790 0.421923 11.00000 -1.20000 AFIX 0 C2 1 0.584855 0.975475 0.269931 11.00000 0.03031 0.15854 = 0.03594 -0.00552 -0.00132 0.00831 AFIX 23 H2A 2 0.600108 0.969911 0.163001 11.00000 -1.20000 H2B 2 0.646872 0.972816 0.325435 11.00000 -1.20000 AFIX 0 C3 1 0.532710 1.098355 0.301598 11.00000 0.05590 0.09968 = 0.05185 0.00937 -0.01469 -0.03420 AFIX 23 H3A 2 0.521462 1.106968 0.409384 11.00000 -1.20000 H3B 2 0.574041 1.167789 0.268793 11.00000 -1.20000 AFIX 0 N1 3 0.291628 0.990220 0.099491 11.00000 0.03520 0.09369 = 0.03055 0.00413 -0.00151 -0.00216 N2 3 0.129375 0.973238 0.279556 11.00000 0.03216 0.10320 = 0.04528 -0.00450 0.00008 -0.00463 N3 3 0.313027 0.996261 0.402288 11.00000 0.03068 0.07171 = 0.03118 -0.00701 -0.00013 -0.00067 O2 6 0.437040 1.102102 0.220890 11.00000 0.04455 0.05831 = 0.05922 0.01444 -0.00493 -0.01394 P1 4 0.363919 0.989807 0.239841 11.00000 0.02803 0.04692 = 0.02962 0.00110 -0.00054 -0.00011 P2 4 0.175992 0.981239 0.116746 11.00000 0.03241 0.06525 = 0.03560 0.00107 -0.00668 -0.00047 P3 4 0.198205 0.985990 0.424371 11.00000 0.03193 0.05237 = 0.03354 -0.00355 0.00293 -0.00090 CL1 5 0.126726 0.835237 -0.003592 11.00000 0.07024 0.09162 = 0.06496 -0.02066 -0.00885 -0.01713 CL2 5 0.114093 1.122696 0.003312 11.00000 0.07482 0.09069 = 0.08880 0.02458 -0.02406 0.01613 CL3 5 0.151017 1.130037 0.549152 11.00000 0.05998 0.07202 = 0.07889 -0.02678 0.00890 0.01282 CL4 5 0.166619 0.842526 0.561090 11.00000 0.07028 0.07047 = 0.06890 0.01980 0.00291 -0.01637 O1 6 0.429562 0.869051 0.228059 11.00000 0.04921 0.05485 = 0.05121 -0.01052 -0.00419 0.01256 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2005sjc0007 in Pna2(1) C 0.770 H 0.320 N 0.700 P 1.100 CL 0.990 O 0.660 C1 - O1 C2 C2 - C1 C3 C3 - O2 C2 N1 - P2 P1 N2 - P2 P3 N3 - P3 P1 O2 - C3 P1 P1 - O2 O1 N1 N3 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl3 Cl4 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 O1 - C1 P1 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 1 -4 15.30 3.57 observed but should be systematically absent 0 4 -7 11.94 2.84 observed but should be systematically absent 0 5 0 28.02 6.38 observed but should be systematically absent 0 6 1 17.51 4.34 observed but should be systematically absent 16478 Reflections read, of which 838 rejected -17 =< h =< 17, -13 =< k =< 13, -11 =< l =< 10, Max. 2-theta = 54.95 4 Systematic absence violations 0 Inconsistent equivalents 2801 Unique reflections, of which 0 suppressed R(int) = 0.0401 R(sigma) = 0.0313 Friedel opposites not merged Maximum memory for data reduction = 1298 / 27812 Default effective X-H distances for T = 1.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 1627 / 174780 wR2 = 0.0905 before cycle 1 for 2801 data and 137 / 137 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0481 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88335 0.00229 -0.004 OSF 2 0.00554 0.00204 0.000 EXTI Mean shift/esd = 0.005 Maximum = 0.016 for y Cl4 Max. shift = 0.000 A for C3 Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1627 / 174780 wR2 = 0.0905 before cycle 2 for 2801 data and 137 / 137 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0481 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88334 0.00229 -0.005 OSF 2 0.00554 0.00204 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.005 for U12 P1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1627 / 174780 wR2 = 0.0905 before cycle 3 for 2801 data and 137 / 137 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0481 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88334 0.00229 0.000 OSF 2 0.00554 0.00204 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U22 C2 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1627 / 174780 wR2 = 0.0905 before cycle 4 for 2801 data and 137 / 137 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0481 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88334 0.00229 0.000 OSF 2 0.00554 0.00204 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y P2 Max. shift = 0.000 A for P2 Max. dU = 0.000 for N2 Largest correlation matrix elements 0.626 EXTI / OSF 0.556 U23 P2 / U23 P1 0.586 U23 P3 / U23 P2 0.546 U23 P3 / U23 P1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5573 0.7888 0.2951 23 0.970 0.000 C1 O1 C2 H1B 0.5076 0.8708 0.4219 23 0.970 0.000 C1 O1 C2 H2A 0.6001 0.9699 0.1630 23 0.970 0.000 C2 C1 C3 H2B 0.6469 0.9728 0.3254 23 0.970 0.000 C2 C1 C3 H3A 0.5215 1.1070 0.4094 23 0.970 0.000 C3 O2 C2 H3B 0.5740 1.1678 0.2688 23 0.970 0.000 C3 O2 C2 2005sjc0007 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.52212 0.86657 0.31467 1.00000 0.05863 0.08935 0.04492 -0.00614 -0.00831 0.03331 0.06430 0.00691 0.00027 0.00038 0.00040 0.00000 0.00200 0.00252 0.00179 0.00161 0.00152 0.00188 0.00097 H1A 0.55735 0.78880 0.29508 1.00000 0.07716 0.00000 0.00000 H1B 0.50758 0.87079 0.42192 1.00000 0.07716 0.00000 0.00000 C2 0.58485 0.97547 0.26993 1.00000 0.03030 0.15853 0.03594 -0.00552 -0.00132 0.00831 0.07492 0.00693 0.00025 0.00041 0.00047 0.00000 0.00164 0.00389 0.00181 0.00206 0.00133 0.00196 0.00119 H2A 0.60011 0.96990 0.16300 1.00000 0.08991 0.00000 0.00000 H2B 0.64687 0.97281 0.32544 1.00000 0.08991 0.00000 0.00000 C3 0.53272 1.09835 0.30160 1.00000 0.05589 0.09967 0.05185 0.00939 -0.01470 -0.03421 0.06914 0.00604 0.00028 0.00041 0.00043 0.00000 0.00210 0.00274 0.00189 0.00190 0.00157 0.00204 0.00105 H3A 0.52147 1.10697 0.40938 1.00000 0.08297 0.00000 0.00000 H3B 0.57405 1.16778 0.26879 1.00000 0.08297 0.00000 0.00000 N1 0.29163 0.99022 0.09949 1.00000 0.03519 0.09368 0.03055 0.00414 -0.00151 -0.00215 0.05314 0.00501 0.00021 0.00027 0.00033 0.00000 0.00130 0.00214 0.00142 0.00114 0.00113 0.00114 0.00072 N2 0.12938 0.97324 0.27955 1.00000 0.03215 0.10319 0.04526 -0.00450 0.00007 -0.00463 0.06020 0.00539 0.00021 0.00030 0.00039 0.00000 0.00136 0.00215 0.00171 0.00150 0.00111 0.00133 0.00076 N3 0.31303 0.99626 0.40229 1.00000 0.03068 0.07172 0.03117 -0.00701 -0.00013 -0.00067 0.04452 0.00435 0.00019 0.00023 0.00030 0.00000 0.00120 0.00168 0.00156 0.00100 0.00100 0.00095 0.00064 O2 0.43704 1.10210 0.22089 1.00000 0.04455 0.05830 0.05922 0.01444 -0.00494 -0.01394 0.05402 0.00380 0.00016 0.00020 0.00026 0.00000 0.00121 0.00117 0.00137 0.00106 0.00101 0.00092 0.00056 P1 0.36392 0.98981 0.23984 1.00000 0.02803 0.04691 0.02962 0.00110 -0.00054 -0.00012 0.03485 0.00121 0.00005 0.00006 0.00009 0.00000 0.00033 0.00036 0.00037 0.00033 0.00027 0.00024 0.00018 P2 0.17599 0.98124 0.11675 1.00000 0.03241 0.06524 0.03560 0.00107 -0.00668 -0.00047 0.04442 0.00134 0.00006 0.00008 0.00009 0.00000 0.00036 0.00049 0.00039 0.00045 0.00033 0.00029 0.00021 P3 0.19821 0.98599 0.42437 1.00000 0.03193 0.05237 0.03353 -0.00355 0.00293 -0.00090 0.03928 0.00130 0.00005 0.00007 0.00009 0.00000 0.00035 0.00040 0.00037 0.00040 0.00030 0.00026 0.00019 Cl1 0.12673 0.83524 -0.00359 1.00000 0.07023 0.09161 0.06496 -0.02066 -0.00884 -0.01713 0.07560 0.00162 0.00008 0.00012 0.00013 0.00000 0.00058 0.00075 0.00056 0.00056 0.00047 0.00050 0.00031 Cl2 0.11409 1.12270 0.00331 1.00000 0.07481 0.09069 0.08880 0.02458 -0.02405 0.01614 0.08477 0.00218 0.00008 0.00012 0.00014 0.00000 0.00063 0.00079 0.00075 0.00068 0.00059 0.00055 0.00035 Cl3 0.15102 1.13004 0.54915 1.00000 0.05998 0.07201 0.07888 -0.02678 0.00890 0.01282 0.07029 0.00178 0.00007 0.00010 0.00012 0.00000 0.00049 0.00058 0.00063 0.00054 0.00048 0.00042 0.00028 Cl4 0.16662 0.84253 0.56109 1.00000 0.07027 0.07047 0.06890 0.01979 0.00291 -0.01636 0.06988 0.00182 0.00008 0.00010 0.00011 0.00000 0.00054 0.00056 0.00059 0.00049 0.00047 0.00045 0.00028 O1 0.42956 0.86905 0.22806 1.00000 0.04921 0.05485 0.05120 -0.01052 -0.00420 0.01257 0.05175 0.00367 0.00016 0.00019 0.00025 0.00000 0.00120 0.00113 0.00127 0.00097 0.00100 0.00092 0.00053 Final Structure Factor Calculation for 2005sjc0007 in Pna2(1) Total number of l.s. parameters = 137 Maximum vector length = 511 Memory required = 1492 / 27090 wR2 = 0.0905 before cycle 5 for 2801 data and 2 / 137 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0481 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0334 for 2568 Fo > 4sig(Fo) and 0.0380 for all 2801 data wR2 = 0.0905, GooF = S = 1.047, Restrained GooF = 1.047 for all data Flack x parameter = 0.2267 with esd 0.1049 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 = 15.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.1121 0.0452 0.0356 C1 0.1593 0.0358 0.0296 C2 0.1218 0.0528 0.0328 C3 0.0940 0.0355 0.0299 N1 0.1038 0.0449 0.0318 N2 0.0729 0.0307 0.0299 N3 0.0786 0.0483 0.0352 O2 0.0470 0.0297 0.0279 P1 0.0653 0.0408 0.0271 P2 0.0531 0.0351 0.0296 P3 0.1066 0.0768 0.0434 Cl1 0.1154 0.0980 0.0409 Cl2 0.1025 0.0707 0.0377 Cl3 0.0943 0.0726 0.0428 Cl4 0.0710 0.0464 0.0379 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.042 0.055 0.070 0.087 0.110 0.140 0.179 0.269 1.000 Number in group 284. 287. 270. 287. 286. 265. 288. 273. 280. 281. GooF 0.927 1.127 1.204 1.006 0.999 0.972 1.029 1.155 1.033 0.989 K 1.178 0.952 0.953 0.965 0.988 0.994 1.009 1.017 1.014 1.008 Resolution(A) 0.77 0.80 0.84 0.87 0.92 0.98 1.05 1.15 1.33 1.65 inf Number in group 289. 282. 269. 289. 280. 276. 276. 285. 273. 282. GooF 0.979 0.982 1.081 1.030 1.062 1.055 0.924 0.903 0.879 1.454 K 0.983 1.011 1.014 1.004 1.032 1.019 1.014 1.020 1.016 0.998 R1 0.114 0.082 0.069 0.049 0.046 0.038 0.027 0.022 0.020 0.029 Recommended weighting scheme: WGHT 0.0481 0.4260 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 4 -2 8490.68 13240.40 6.29 1.000 1.89 3 9 0 51.82 23.80 5.25 0.042 1.14 0 1 1 239.82 354.98 4.83 0.164 6.80 1 5 2 289.66 214.80 4.43 0.127 1.90 0 1 -1 256.59 350.71 3.96 0.163 6.80 2 10 1 66.62 41.47 3.85 0.056 1.04 6 2 -1 468.23 592.90 3.81 0.212 2.02 2 2 3 2106.46 2599.92 3.76 0.443 2.41 2 1 1 13.62 26.66 3.69 0.045 4.79 6 3 -9 2.33 16.86 3.66 0.036 0.87 1 5 -2 282.58 218.05 3.64 0.128 1.90 2 2 -3 2135.03 2616.93 3.63 0.445 2.41 9 7 6 41.59 67.06 3.58 0.071 0.86 4 2 -1 207.66 266.16 3.49 0.142 2.71 2 1 -1 13.89 25.94 3.41 0.044 4.79 1 13 0 16.09 0.44 3.41 0.006 0.82 6 2 1 491.22 604.53 3.39 0.214 2.02 4 12 2 17.13 36.56 3.22 0.053 0.84 2 12 1 26.54 9.87 3.19 0.027 0.88 0 10 -2 268.99 341.55 3.13 0.161 1.03 2 10 5 9.46 21.23 3.08 0.040 0.90 2 8 7 266.99 331.56 3.03 0.158 0.91 12 0 -3 56.12 30.41 3.02 0.048 1.05 4 2 1 208.93 258.04 3.01 0.140 2.71 14 2 -1 504.23 414.20 2.95 0.177 0.94 3 5 0 446.42 373.54 2.93 0.168 1.92 10 3 -6 1.70 9.82 2.91 0.027 0.96 8 12 1 2.24 18.09 2.88 0.037 0.78 0 3 -3 722.56 863.15 2.88 0.255 2.27 8 10 0 10.19 23.87 2.86 0.042 0.90 2 10 -1 60.36 42.96 2.82 0.057 1.04 4 2 -4 424.49 357.20 2.82 0.164 1.75 1 11 0 33.84 52.13 2.80 0.063 0.97 1 6 -1 63.54 44.92 2.79 0.058 1.73 1 2 -3 4.21 9.92 2.79 0.027 2.53 4 2 0 809.13 692.16 2.74 0.229 2.85 1 6 1 64.13 46.68 2.74 0.059 1.73 10 0 0 51.86 33.57 2.73 0.050 1.35 13 1 -4 336.77 272.30 2.73 0.143 0.94 8 5 -7 40.91 57.95 2.68 0.066 0.91 5 1 0 584.80 687.00 2.67 0.228 2.61 2 0 -8 15.11 25.53 2.67 0.044 1.09 5 9 0 34.70 49.82 2.66 0.061 1.08 3 11 -4 57.90 81.89 2.63 0.079 0.87 6 8 4 150.03 185.96 2.61 0.119 1.02 2 6 -3 344.90 292.15 2.56 0.149 1.48 4 8 -8 47.53 69.61 2.56 0.073 0.82 0 10 2 279.56 340.44 2.55 0.160 1.03 4 2 4 426.32 364.46 2.54 0.166 1.75 13 5 -4 16.86 30.54 2.53 0.048 0.86 Bond lengths and angles C1 - Distance Angles O1 1.4645 (0.0040) C2 1.4884 (0.0055) 109.32 (0.29) C1 - O1 C2 - Distance Angles C1 1.4884 (0.0055) C3 1.5111 (0.0059) 111.13 (0.30) C2 - C1 C3 - Distance Angles O2 1.4748 (0.0040) C2 1.5111 (0.0059) 109.90 (0.29) C3 - O2 N1 - Distance Angles P2 1.5692 (0.0029) P1 1.5785 (0.0029) 122.45 (0.19) N1 - P2 N2 - Distance Angles P2 1.5739 (0.0034) P3 1.5878 (0.0034) 120.04 (0.18) N2 - P2 N3 - Distance Angles P3 1.5639 (0.0028) P1 1.5941 (0.0026) 122.38 (0.17) N3 - P3 O2 - Distance Angles C3 1.4748 (0.0041) P1 1.5583 (0.0021) 118.70 (0.21) O2 - C3 P1 - Distance Angles O2 1.5583 (0.0021) O1 1.5640 (0.0020) 105.39 (0.14) N1 1.5785 (0.0029) 107.68 (0.14) 107.41 (0.14) N3 1.5941 (0.0026) 109.64 (0.13) 109.82 (0.13) 116.33 (0.14) P1 - O2 O1 N1 P2 - Distance Angles N1 1.5692 (0.0029) N2 1.5739 (0.0034) 119.27 (0.16) Cl2 1.9927 (0.0013) 108.72 (0.12) 109.55 (0.13) Cl1 1.9975 (0.0013) 109.02 (0.12) 108.24 (0.12) 100.38 (0.07) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5639 (0.0028) N2 1.5878 (0.0034) 118.92 (0.15) Cl3 1.9936 (0.0011) 109.34 (0.10) 109.04 (0.12) Cl4 1.9941 (0.0012) 109.92 (0.11) 107.42 (0.13) 100.65 (0.06) P3 - N3 N2 Cl3 Cl1 - Distance Angles P2 1.9975 (0.0013) Cl1 - Cl2 - Distance Angles P2 1.9927 (0.0013) Cl2 - Cl3 - Distance Angles P3 1.9936 (0.0011) Cl3 - Cl4 - Distance Angles P3 1.9941 (0.0012) Cl4 - O1 - Distance Angles C1 1.4645 (0.0040) P1 1.5640 (0.0020) 117.51 (0.21) O1 - C1 FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.0355 for 1530 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.3944 0.1311 0.2505 [ 0.70 A from O2 ] Deepest hole -0.35 at 0.7811 0.0003 -0.0029 [ 0.72 A from P3 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1711 / 17880 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3944 1.1311 0.2505 1.00000 0.05 0.28 0.70 O2 1.56 P1 1.95 C3 2.23 H3A Q2 1 0.6151 0.9988 0.0447 1.00000 0.05 0.27 1.11 H2A 1.59 N3 2.05 C2 2.42 H1B Q3 1 0.5124 1.2478 0.2568 1.00000 0.05 0.26 1.19 H3B 1.66 C3 1.88 O2 2.02 H3A Q4 1 0.3829 0.8689 0.2483 1.00000 0.05 0.24 0.65 O1 1.31 P1 1.97 C1 2.14 N3 Q5 1 0.1186 0.9948 0.5650 1.00000 0.05 0.24 1.51 CL3 1.65 P3 1.75 CL4 2.54 N2 Q6 1 0.1398 0.9884 -0.0192 1.00000 0.05 0.24 1.30 P2 1.48 CL2 1.65 CL1 2.30 N1 Q7 1 0.1231 1.2163 0.0041 1.00000 0.05 0.24 1.00 CL2 2.52 H1B 2.73 H3B 2.79 P2 Q8 1 0.0175 1.1188 0.0395 1.00000 0.05 0.24 1.34 CL2 2.52 CL4 2.68 P2 2.90 H1B Q9 1 0.1213 1.1080 0.2831 1.00000 0.05 0.24 1.44 N2 2.08 P3 2.13 P2 2.40 CL3 Q10 1 0.1424 0.9226 0.5412 1.00000 0.05 0.23 0.93 CL4 1.45 P3 2.21 CL3 2.38 N2 Q11 1 0.2570 0.8698 0.0098 1.00000 0.05 0.23 1.58 N1 1.80 CL1 1.87 P2 2.67 H2B Q12 1 0.3584 0.9975 0.0235 1.00000 0.05 0.23 1.13 N1 1.78 H2B 1.92 P1 2.21 H3A Q13 1 0.1775 1.0555 0.1144 1.00000 0.05 0.23 0.79 P2 1.49 CL2 1.69 N1 1.82 N2 Q14 1 0.1356 1.0722 0.2789 1.00000 0.05 0.22 1.06 N2 1.79 P3 1.81 P2 2.48 CL3 Q15 1 0.5079 0.7418 0.2540 1.00000 0.05 0.22 0.91 H1A 1.45 C1 1.73 O1 2.02 H1B Q16 1 0.0230 0.8889 0.0438 1.00000 0.05 0.22 1.57 CL1 2.35 CL3 2.37 P2 2.69 N2 Q17 1 0.6283 1.1206 0.2640 1.00000 0.05 0.21 0.89 H3B 1.35 C3 1.65 C2 1.68 H2B Q18 1 0.0132 0.8542 -0.0164 1.00000 0.05 0.21 1.55 CL1 2.29 CL3 2.75 H3A 2.83 P2 Q19 1 0.4802 1.1217 0.4650 1.00000 0.05 0.21 0.76 H3A 1.63 C3 2.20 H3B 2.25 O2 Q20 1 0.3450 0.9986 0.4734 1.00000 0.05 0.21 0.76 N3 1.86 H2A 2.03 P3 2.08 P1 Shortest distances between peaks (including symmetry equivalents) 9 14 0.43 16 18 0.66 2 20 0.83 5 10 0.86 6 13 1.47 13 14 1.57 9 13 1.76 7 8 1.79 11 12 1.93 2 19 1.95 6 16 1.98 1 3 2.02 6 11 2.04 3 17 2.07 7 13 2.10 3 9 2.14 4 15 2.16 8 10 2.20 5 8 2.21 6 8 2.22 6 18 2.23 1 19 2.23 19 20 2.25 5 16 2.28 3 19 2.32 3 18 2.33 15 16 2.33 2 17 2.34 8 13 2.35 3 8 2.39 11 13 2.43 4 12 2.44 6 7 2.44 8 16 2.45 4 20 2.48 18 19 2.48 5 18 2.50 1 12 2.51 1 20 2.51 3 14 2.54 9 18 2.57 8 9 2.57 12 19 2.57 15 18 2.60 12 17 2.62 12 13 2.64 11 17 2.67 5 14 2.67 17 19 2.67 8 14 2.70 4 11 2.71 3 7 2.71 7 9 2.72 5 9 2.77 6 14 2.79 4 7 2.79 1 4 2.79 13 16 2.81 14 18 2.81 10 14 2.82 7 15 2.84 8 18 2.86 8 15 2.87 7 14 2.88 7 17 2.88 17 20 2.89 9 17 2.90 10 20 2.91 16 19 2.93 15 19 2.94 1 2 2.95 6 12 2.97 6 9 2.97 2 4 2.98 3 16 2.99 10 16 3.00 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 0.94: 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 0.99: Structure factors and derivatives 0.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005sjc0007 finished at 19:44:11 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++