+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0391 started at 16:39:28 on 24-Apr-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0391 in P-1 CELL 0.71073 8.0877 8.4452 9.3069 104.517 101.380 114.951 ZERR 1.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N O P CL UNIT 6 12 6 4 6 6 V = 523.64 F(000) = 314.0 Mu = 1.31 mm-1 Cell Wt = 630.74 Rho = 2.000 MERG 2 OMIT -3.00 55.00 OMIT 0 -2 1 OMIT -1 1 0 OMIT -1 0 1 OMIT -1 0 2 OMIT 0 -1 1 FMAP 2 PLAN 20 SIZE 0.20 0.40 0.60 ACTA BOND WGHT 0.03500 0.79330 L.S. 4 TEMP -153.00 FVAR 1.17230 C1 1 0.530940 0.720257 0.423244 11.00000 0.01766 0.01768 = 0.01371 0.00621 0.00900 0.00971 AFIX 23 H1A 2 0.552403 0.620715 0.446078 11.00000 -1.20000 H1B 2 0.655631 0.818105 0.425508 11.00000 -1.20000 AFIX 0 C4 1 0.243398 0.714833 0.254467 11.00000 0.01312 0.01377 = 0.00694 0.00428 0.00332 0.00155 AFIX 23 H4A 2 0.318553 0.853791 0.290120 11.00000 -1.20000 H4B 2 0.153094 0.664165 0.144895 11.00000 -1.20000 AFIX 0 C5 1 0.380433 0.635416 0.259072 11.00000 0.01457 0.01791 = 0.01166 0.00145 0.00644 0.00517 AFIX 23 H5A 2 0.447338 0.661898 0.182534 11.00000 -1.20000 H5B 2 0.304519 0.496965 0.226937 11.00000 -1.20000 AFIX 0 N1 3 0.193424 0.534010 0.589028 11.00000 0.01103 0.00776 = 0.00590 0.00209 0.00301 0.00412 N2 3 0.121335 0.691219 0.846495 11.00000 0.01422 0.00722 = 0.00703 0.00119 0.00396 0.00390 N3 3 0.254876 0.890761 0.667094 11.00000 0.01692 0.00656 = 0.00738 0.00170 0.00552 0.00397 O1 4 0.471349 0.804552 0.546579 11.00000 0.00861 0.01280 = 0.00845 0.00139 0.00362 0.00084 O2 4 0.130529 0.660815 0.360942 11.00000 0.01881 0.02108 = 0.01642 0.00740 0.00641 0.00621 P1 5 0.259176 0.720264 0.549209 11.00000 0.00781 0.00653 = 0.00510 0.00123 0.00176 0.00137 P2 5 0.100489 0.509368 0.721678 11.00000 0.00834 0.00644 = 0.00487 0.00178 0.00124 0.00246 P3 5 0.170181 0.871599 0.803655 11.00000 0.00945 0.00669 = 0.00612 0.00085 0.00185 0.00282 CL1 6 0.222014 0.402574 0.850265 11.00000 0.01625 0.01448 = 0.01195 0.00753 0.00201 0.00834 CL2 6 0.350504 1.101838 1.000005 11.00000 0.01477 0.00920 = 0.00882 -0.00163 0.00120 0.00403 CL3 6 -0.066049 0.902143 0.760920 11.00000 0.01337 0.01811 = 0.02066 0.00530 0.00356 0.00967 HKLF 4 Covalent radii and connectivity table for 2008src0391 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C5 C4 - O2 C5 C5 - C4 C1 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C4 P2_$1 P1 P1 - O1 N3 N1 O2 P2 - N1 N2 O2_$1 Cl1 P3 - N3 N2 Cl2 Cl3 Cl1 - P2 Cl2 - P3 Cl3 - P3 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 11632 Reflections read, of which 17 rejected -10 =< h =< 10, -10 =< k =< 10, -12 =< l =< 12, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 2389 Unique reflections, of which 0 suppressed R(int) = 0.0312 R(sigma) = 0.0241 Friedel opposites merged Maximum memory for data reduction = 1266 / 24581 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 = 1582 / 163215 wR2 = 0.0788 before cycle 1 for 2389 data and 127 / 127 parameters GooF = S = 1.134; Restrained GooF = 1.134 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16498 0.00211 -3.473 OSF Mean shift/esd = 0.394 Maximum = -3.473 for OSF Max. shift = 0.001 A for N2 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1582 / 163215 wR2 = 0.0786 before cycle 2 for 2389 data and 127 / 127 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16312 0.00210 -0.888 OSF Mean shift/esd = 0.131 Maximum = -0.888 for OSF Max. shift = 0.000 A for N2 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1582 / 163215 wR2 = 0.0786 before cycle 3 for 2389 data and 127 / 127 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16312 0.00209 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.008 for U11 O2 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1582 / 163215 wR2 = 0.0786 before cycle 4 for 2389 data and 127 / 127 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16312 0.00209 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U23 O2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for N3 Largest correlation matrix elements 0.641 U12 Cl3 / U22 Cl3 0.604 U12 C1 / U11 C1 0.582 U12 N3 / U22 N3 0.639 U12 Cl3 / U11 Cl3 0.603 U12 P2 / U11 P2 0.574 U12 N1 / U11 N1 0.634 U12 Cl1 / U22 Cl1 0.600 U12 P3 / U11 P3 0.570 U12 N2 / U11 N2 0.618 U12 Cl1 / U11 Cl1 0.599 U12 Cl2 / U11 Cl2 0.566 U12 N3 / U11 N3 0.614 U12 C1 / U22 C1 0.594 U12 P1 / U22 P1 0.565 U12 C5 / U22 C5 0.614 U12 P3 / U22 P3 0.593 U12 N1 / U22 N1 0.562 U12 O2 / U22 O2 0.607 U12 P2 / U22 P2 0.590 U12 P1 / U11 P1 0.561 U13 Cl3 / U23 Cl3 0.605 U12 Cl2 / U22 Cl2 0.585 U12 N2 / U22 N2 0.550 U12 O2 / U11 O2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5524 0.6207 0.4461 23 0.990 0.000 C1 O1 C5 H1B 0.6557 0.8181 0.4256 23 0.990 0.000 C1 O1 C5 H4A 0.3184 0.8538 0.2901 23 0.990 0.000 C4 O2 C5 H4B 0.1529 0.6642 0.1449 23 0.990 0.000 C4 O2 C5 H5A 0.4474 0.6619 0.1825 23 0.990 0.000 C5 C4 C1 H5B 0.3045 0.4969 0.2268 23 0.990 0.000 C5 C4 C1 2008src0391 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.53099 0.72021 0.42332 1.00000 0.01706 0.01728 0.01349 0.00639 0.00898 0.00959 0.01476 0.00631 0.00034 0.00033 0.00026 0.00000 0.00107 0.00111 0.00105 0.00088 0.00088 0.00095 0.00045 H1A 0.55244 0.62065 0.44613 1.00000 0.01771 0.00000 0.00000 H1B 0.65571 0.81810 0.42565 1.00000 0.01771 0.00000 0.00000 C4 0.24327 0.71488 0.25444 1.00000 0.01299 0.01355 0.00668 0.00446 0.00340 0.00158 0.01290 0.00590 0.00032 0.00032 0.00025 0.00000 0.00099 0.00103 0.00093 0.00079 0.00078 0.00086 0.00042 H4A 0.31842 0.85384 0.29012 1.00000 0.01548 0.00000 0.00000 H4B 0.15294 0.66424 0.14489 1.00000 0.01548 0.00000 0.00000 C5 0.38043 0.63537 0.25899 1.00000 0.01390 0.01740 0.01122 0.00136 0.00622 0.00470 0.01594 0.00610 0.00033 0.00033 0.00027 0.00000 0.00104 0.00111 0.00102 0.00086 0.00085 0.00093 0.00046 H5A 0.44738 0.66194 0.18249 1.00000 0.01913 0.00000 0.00000 H5B 0.30452 0.49691 0.22679 1.00000 0.01913 0.00000 0.00000 N1 0.19333 0.53405 0.58903 1.00000 0.01055 0.00745 0.00563 0.00217 0.00297 0.00391 0.00813 0.00463 0.00025 0.00024 0.00020 0.00000 0.00081 0.00081 0.00077 0.00064 0.00064 0.00069 0.00034 N2 0.12147 0.69131 0.84664 1.00000 0.01373 0.00700 0.00672 0.00107 0.00375 0.00368 0.01002 0.00476 0.00027 0.00025 0.00021 0.00000 0.00086 0.00082 0.00079 0.00066 0.00068 0.00072 0.00035 N3 0.25486 0.89069 0.66705 1.00000 0.01651 0.00619 0.00719 0.00172 0.00540 0.00373 0.01066 0.00480 0.00027 0.00024 0.00021 0.00000 0.00090 0.00081 0.00081 0.00066 0.00070 0.00074 0.00036 O1 0.47131 0.80441 0.54660 1.00000 0.00840 0.01239 0.00837 0.00130 0.00365 0.00078 0.01189 0.00398 0.00022 0.00022 0.00018 0.00000 0.00070 0.00074 0.00070 0.00058 0.00057 0.00061 0.00031 O2 0.13046 0.66082 0.36094 1.00000 0.01887 0.02078 0.01618 0.00733 0.00642 0.00633 0.01985 0.00461 0.00025 0.00025 0.00020 0.00000 0.00085 0.00088 0.00084 0.00070 0.00069 0.00073 0.00037 P1 0.25916 0.72027 0.54919 1.00000 0.00743 0.00611 0.00471 0.00105 0.00159 0.00117 0.00724 0.00136 0.00007 0.00007 0.00006 0.00000 0.00024 0.00025 0.00024 0.00019 0.00019 0.00020 0.00013 P2 0.10044 0.50933 0.72165 1.00000 0.00799 0.00609 0.00453 0.00169 0.00114 0.00238 0.00688 0.00137 0.00007 0.00007 0.00006 0.00000 0.00024 0.00024 0.00024 0.00019 0.00019 0.00020 0.00013 P3 0.17020 0.87161 0.80366 1.00000 0.00912 0.00632 0.00579 0.00075 0.00173 0.00268 0.00800 0.00138 0.00008 0.00007 0.00006 0.00000 0.00025 0.00025 0.00024 0.00019 0.00019 0.00021 0.00013 Cl1 0.22201 0.40257 0.85027 1.00000 0.01589 0.01409 0.01150 0.00738 0.00186 0.00818 0.01346 0.00141 0.00008 0.00007 0.00006 0.00000 0.00026 0.00026 0.00025 0.00020 0.00020 0.00022 0.00013 Cl2 0.35052 1.10185 1.00000 1.00000 0.01436 0.00876 0.00849 -0.00179 0.00108 0.00384 0.01287 0.00131 0.00008 0.00007 0.00006 0.00000 0.00025 0.00024 0.00024 0.00018 0.00019 0.00020 0.00013 Cl3 -0.06610 0.90212 0.76089 1.00000 0.01298 0.01769 0.02031 0.00519 0.00340 0.00948 0.01709 0.00148 0.00008 0.00008 0.00007 0.00000 0.00025 0.00028 0.00028 0.00022 0.00021 0.00022 0.00014 Final Structure Factor Calculation for 2008src0391 in P-1 Total number of l.s. parameters = 127 Maximum vector length = 511 Memory required = 1455 / 25039 wR2 = 0.0786 before cycle 5 for 2389 data and 0 / 127 parameters GooF = S = 1.133; Restrained GooF = 1.133 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0292 for 2248 Fo > 4sig(Fo) and 0.0312 for all 2389 data wR2 = 0.0786, GooF = S = 1.133, Restrained GooF = 1.133 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0184 0.0167 0.0091 C1 0.0232 0.0100 0.0055 C4 0.0260 0.0131 0.0087 C5 0.0113 0.0077 0.0054 N1 0.0158 0.0089 0.0054 N2 0.0193 0.0073 0.0054 N3 0.0211 0.0078 0.0068 O1 0.0269 0.0176 0.0150 O2 0.0113 0.0060 0.0044 P1 0.0099 0.0063 0.0045 P2 0.0107 0.0084 0.0049 P3 0.0193 0.0148 0.0063 Cl1 0.0171 0.0166 0.0049 Cl2 0.0238 0.0172 0.0103 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.029 0.063 0.097 0.128 0.161 0.199 0.248 0.308 0.415 1.000 Number in group 240. 241. 239. 235. 239. 243. 236. 239. 236. 241. GooF 1.240 1.092 1.121 1.054 1.112 1.150 1.120 0.971 0.826 1.506 K 1.561 1.028 0.993 1.001 1.001 1.007 1.022 1.011 1.005 0.965 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 246. 241. 229. 244. 239. 234. 238. 241. 238. 239. GooF 0.905 0.882 0.778 0.742 0.720 0.799 1.013 1.047 1.246 2.288 K 0.977 0.989 0.999 1.001 1.007 1.019 1.016 0.995 1.000 0.945 R1 0.043 0.036 0.030 0.026 0.022 0.025 0.026 0.023 0.026 0.048 Recommended weighting scheme: WGHT 0.0320 0.9126 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 1 1 5151.23 7868.29 7.66 0.981 3.17 -1 -2 1 350.02 225.11 6.17 0.166 2.91 4 -2 6 75.07 15.59 5.58 0.044 1.06 -2 2 3 92.37 49.22 5.09 0.078 2.17 0 -1 3 566.10 421.61 4.83 0.227 3.04 1 0 1 2981.62 3806.17 4.66 0.682 4.61 -1 -1 3 2681.45 3326.69 4.61 0.638 2.96 0 -3 2 10.52 0.91 4.55 0.011 2.50 -2 2 0 113.10 68.92 4.53 0.092 3.48 1 0 2 3623.10 4462.46 4.44 0.739 3.15 0 1 1 152.09 221.45 4.30 0.165 4.64 -1 3 3 158.34 106.13 4.26 0.114 1.71 0 -3 1 450.14 344.69 4.24 0.205 2.54 -1 2 1 5632.11 6748.43 4.14 0.909 3.39 1 -3 1 594.60 467.74 4.11 0.239 2.80 -3 3 1 106.61 158.22 3.85 0.139 2.23 -2 0 2 1414.02 1701.76 3.82 0.456 3.28 -3 -1 3 292.89 222.78 3.79 0.165 1.99 -1 2 3 4993.69 5885.41 3.75 0.849 2.11 -3 3 0 7.54 0.56 3.64 0.008 2.32 1 -1 1 3086.82 3880.86 3.55 0.689 5.43 -2 -1 3 3825.93 4452.17 3.39 0.738 2.48 1 -3 3 900.66 753.40 3.34 0.304 2.31 -2 -2 3 10.65 2.30 3.28 0.017 2.11 -3 3 3 58.41 36.21 3.24 0.067 1.77 2 -3 1 19.85 38.89 3.23 0.069 2.66 -2 -1 1 2722.14 3157.48 3.16 0.622 2.85 -5 2 4 202.88 155.77 3.14 0.138 1.43 -2 0 3 1229.28 1435.43 3.12 0.419 2.68 -4 3 1 8.54 21.63 3.07 0.051 1.90 1 -2 3 31.65 16.25 3.05 0.045 2.62 -2 1 0 29.30 49.62 2.98 0.078 3.96 2 -6 2 9.39 2.24 2.97 0.017 1.40 -5 -1 1 8.38 1.72 2.91 0.015 1.30 0 0 2 1570.95 1813.33 2.86 0.471 4.23 -1 1 1 1166.04 1361.73 2.86 0.408 5.32 -2 2 1 2474.70 2844.31 2.83 0.590 3.20 -1 -1 2 309.95 253.69 2.82 0.176 3.82 -2 2 4 26.19 13.79 2.82 0.041 1.79 4 -2 2 405.33 337.16 2.81 0.203 1.68 1 0 0 1089.51 1323.11 2.80 0.402 6.88 -1 -4 1 262.19 212.74 2.80 0.161 1.64 -2 -3 4 295.20 240.85 2.79 0.172 1.66 0 -2 4 155.55 119.57 2.79 0.121 2.22 1 1 2 2922.59 3329.18 2.73 0.638 2.45 2 -2 2 7257.00 8171.91 2.72 1.000 2.71 -1 3 1 764.60 660.64 2.71 0.284 2.37 5 2 5 25.91 12.29 2.71 0.039 0.79 -4 2 3 886.68 768.94 2.70 0.307 1.79 8 -1 3 292.56 369.79 2.69 0.213 0.80 Bond lengths and angles C1 - Distance Angles O1 1.4677 (0.0026) C5 1.5214 (0.0032) 112.33 (0.18) C1 - O1 C4 - Distance Angles O2 1.5019 (0.0026) C5 1.5191 (0.0033) 109.09 (0.18) C4 - O2 C5 - Distance Angles C4 1.5191 (0.0033) C1 1.5214 (0.0032) 111.55 (0.18) C5 - C4 N1 - Distance Angles P2 1.5793 (0.0017) P1 1.5994 (0.0018) 121.80 (0.11) N1 - P2 N2 - Distance Angles P3 1.5795 (0.0018) P2 1.5966 (0.0018) 118.68 (0.11) N2 - P3 N3 - Distance Angles P3 1.5698 (0.0018) P1 1.5943 (0.0018) 122.44 (0.12) N3 - P3 O1 - Distance Angles C1 1.4677 (0.0026) P1 1.5639 (0.0015) 124.84 (0.14) O1 - C1 O2 - Distance Angles C4 1.5019 (0.0026) P2_$1 1.6610 (0.0018) 118.26 (0.14) P1 1.6744 (0.0018) 116.93 (0.14) 121.53 (0.11) O2 - C4 P2_$1 P1 - Distance Angles O1 1.5639 (0.0015) N3 1.5943 (0.0018) 105.18 (0.09) N1 1.5994 (0.0018) 112.22 (0.09) 116.10 (0.09) O2 1.6744 (0.0018) 101.63 (0.09) 112.01 (0.10) 108.75 (0.09) P1 - O1 N3 N1 P2 - Distance Angles N1 1.5793 (0.0018) N2 1.5966 (0.0018) 118.56 (0.10) O2_$1 1.6610 (0.0018) 109.59 (0.09) 110.68 (0.10) Cl1 2.0093 (0.0007) 108.51 (0.07) 105.60 (0.07) 102.59 (0.07) P2 - N1 N2 O2_$1 P3 - Distance Angles N3 1.5698 (0.0018) N2 1.5795 (0.0018) 119.25 (0.10) Cl2 2.0054 (0.0007) 108.66 (0.07) 108.69 (0.07) Cl3 2.0110 (0.0008) 109.10 (0.08) 109.13 (0.07) 100.35 (0.03) P3 - N3 N2 Cl2 Cl1 - Distance Angles P2 2.0093 (0.0007) Cl1 - Cl2 - Distance Angles P3 2.0054 (0.0007) Cl2 - Cl3 - Distance Angles P3 2.0110 (0.0008) Cl3 - FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -2 2.381 2 2 R1 = 0.0311 for 2389 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.4752 0.8195 0.8643 [ 1.45 A from CL2 ] Deepest hole -0.66 at 0.1575 0.6276 0.3548 [ 0.42 A from O2 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 1548 / 18135 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5248 1.1805 1.1357 1.00000 0.05 0.35 1.45 CL2 2.55 N2 2.66 N3 2.66 P3 Q2 1 -0.2410 0.7592 0.6081 1.00000 0.05 0.34 1.54 CL3 1.70 H1A 2.01 H1B 2.10 C1 Q3 1 0.4236 0.8974 0.8274 1.00000 0.05 0.33 1.78 N3 1.93 P3 2.18 CL2 2.39 P1 Q4 1 0.0511 0.3549 0.7989 1.00000 0.05 0.32 1.21 CL1 1.59 P2 1.78 H4B 1.81 O2 Q5 1 0.1941 0.5595 0.3773 1.00000 0.05 0.31 1.19 O2 1.63 P1 1.89 H5B 1.92 C4 Q6 1 0.3492 0.7276 0.8537 1.00000 0.05 0.30 1.72 N2 1.93 P2 2.14 CL2 2.30 P3 Q7 1 0.0481 0.5396 0.5021 1.00000 0.05 0.30 1.31 N1 1.61 P1 1.73 N1 1.91 O2 Q8 1 0.0727 0.8485 0.3135 1.00000 0.05 0.30 1.95 O2 2.02 H4A 2.19 C4 2.28 CL1 Q9 1 -0.0321 0.7602 0.4387 1.00000 0.05 0.30 1.99 O2 2.15 P2 2.18 N1 2.42 N3 Q10 1 0.1740 0.8374 0.6960 1.00000 0.05 0.30 0.76 N3 0.98 P3 1.89 P1 2.08 N2 Q11 1 0.2274 0.4467 0.3575 1.00000 0.05 0.29 1.54 H5B 2.10 C5 2.21 N1 2.24 H1A Q12 1 0.2733 0.9172 0.7557 1.00000 0.05 0.28 0.76 N3 1.00 P3 2.15 P1 2.20 CL2 Q13 1 0.3915 0.5884 0.9102 1.00000 0.05 0.28 1.45 CL1 2.35 CL2 2.35 P2 2.35 H5A Q14 1 0.0555 0.4123 0.5140 1.00000 0.05 0.28 1.07 N1 1.79 P2 2.07 O2 2.18 P1 Q15 1 0.3083 0.6693 0.2518 1.00000 0.05 0.28 0.75 C5 0.77 C4 1.40 H5B 1.42 H5A Q16 1 0.1760 0.4357 0.5216 1.00000 0.05 0.28 0.84 N1 2.10 P2 2.13 P1 2.42 H1A Q17 1 0.2464 0.4018 0.2624 1.00000 0.05 0.27 0.92 H5B 1.82 C5 2.28 CL3 2.31 H1A Q18 1 0.5400 1.1818 1.0423 1.00000 0.05 0.27 1.31 CL2 2.36 N2 2.74 H5A 2.76 P3 Q19 1 0.1180 0.4340 0.2853 1.00000 0.05 0.27 1.63 H5B 1.75 N2 1.82 O2 2.01 P2 Q20 1 0.0777 0.4865 0.5748 1.00000 0.05 0.27 0.81 N1 1.30 P2 1.93 O2 2.01 P1 Shortest distances between peaks (including symmetry equivalents) 14 20 0.66 10 12 0.77 7 7 0.77 14 16 0.89 1 18 0.90 11 17 0.94 7 20 0.94 11 19 0.95 1 6 0.95 1 3 1.01 5 19 1.01 6 18 1.02 7 20 1.02 7 14 1.08 5 11 1.08 7 14 1.13 16 20 1.18 17 19 1.22 3 12 1.36 3 6 1.41 4 8 1.51 6 13 1.53 3 18 1.56 9 14 1.57 7 16 1.63 11 16 1.67 13 18 1.68 8 9 1.71 5 17 1.74 9 16 1.75 5 7 1.80 20 20 1.81 5 15 1.82 14 20 1.83 7 16 1.89 2 11 1.89 5 16 1.89 3 10 1.92 9 20 1.92 1 13 1.97 2 17 2.02 14 14 2.07 15 19 2.08 2 16 2.10 4 9 2.13 15 17 2.13 5 14 2.15 16 19 2.15 11 14 2.19 10 14 2.22 5 20 2.22 11 15 2.25 6 12 2.26 7 19 2.27 1 12 2.30 14 19 2.32 5 20 2.33 7 10 2.34 3 18 2.37 7 9 2.38 9 10 2.38 7 11 2.39 5 7 2.40 4 13 2.41 19 20 2.43 6 10 2.45 16 20 2.48 5 14 2.50 2 9 2.53 2 19 2.53 16 17 2.56 11 20 2.58 10 19 2.58 10 20 2.59 4 20 2.60 7 19 2.62 6 20 2.65 7 9 2.68 12 18 2.69 14 16 2.69 2 14 2.71 10 16 2.71 1 10 2.71 18 18 2.72 19 20 2.73 12 18 2.73 4 15 2.76 4 5 2.77 7 10 2.77 10 20 2.79 4 14 2.82 2 8 2.82 7 11 2.82 3 13 2.83 4 19 2.83 1 18 2.85 4 6 2.88 11 20 2.90 2 5 2.90 14 19 2.91 1 3 2.93 8 15 2.95 3 3 2.95 7 12 2.95 12 14 2.96 10 11 2.96 9 12 2.99 Time profile in seconds ----------------------- 0.06: 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 0.00: 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. 2.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.23: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0391 finished at 16:39:32 Total CPU time: 3.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++