+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0400 started at 17:59:59 on 22-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0400 in P2(1)/c CELL 0.71073 8.6518 11.3633 16.0178 90.000 102.006 90.000 ZERR 2.00 0.0001 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N P CL UNIT 24 52 16 12 16 V = 1540.31 F(000) = 760.0 Mu = 1.06 mm-1 Cell Wt = 1503.66 Rho = 1.621 MERG 2 OMIT -3.00 55.00 OMIT -1 2 2 OMIT -1 1 1 OMIT 1 2 2 OMIT -1 0 2 OMIT 1 1 0 OMIT 4 0 0 OMIT 1 1 1 FMAP 2 PLAN 20 SIZE 0.30 0.30 0.55 ACTA BOND WGHT 0.03350 1.18900 L.S. 4 TEMP -153.00 FVAR 0.63836 C1 1 0.277170 0.580054 0.063238 11.00000 0.01908 0.02080 = 0.01518 0.00171 0.00565 0.00151 AFIX 23 H1A 2 0.301847 0.576214 0.126365 11.00000 -1.20000 H1B 2 0.200256 0.516884 0.041928 11.00000 -1.20000 AFIX 0 C2 1 0.203007 0.698252 0.035373 11.00000 0.01969 0.02033 = 0.01624 0.00087 0.00384 0.00275 AFIX 23 H2A 2 0.187014 0.705582 -0.027428 11.00000 -1.20000 H2B 2 0.274852 0.762115 0.061520 11.00000 -1.20000 AFIX 0 C3 1 0.044523 0.710596 0.062262 11.00000 0.01836 0.02586 = 0.01919 -0.00165 0.00333 0.00238 AFIX 23 H3A 2 -0.023471 0.643034 0.039380 11.00000 -1.20000 H3B 2 0.062613 0.707343 0.125314 11.00000 -1.20000 AFIX 0 C4 1 -0.041333 0.823256 0.031854 11.00000 0.03060 0.03423 = 0.02309 0.00507 0.00962 0.01351 AFIX 23 H4A 2 -0.055991 0.828273 -0.031009 11.00000 -1.20000 H4B 2 0.024257 0.891028 0.056763 11.00000 -1.20000 AFIX 0 C5 1 -0.202514 0.831236 0.056386 11.00000 0.02682 0.04382 = 0.03541 0.00206 0.00876 0.00939 AFIX 23 H5A 2 -0.266365 0.761792 0.033242 11.00000 -1.20000 H5B 2 -0.187198 0.828752 0.119356 11.00000 -1.20000 AFIX 0 C6 1 -0.292577 0.941352 0.023984 11.00000 0.04440 0.05882 = 0.05029 0.00562 0.01521 0.02772 AFIX 137 H6A 2 -0.230614 1.010581 0.047055 11.00000 -1.50000 H6B 2 -0.393789 0.942038 0.042340 11.00000 -1.50000 H6C 2 -0.311859 0.942998 -0.038499 11.00000 -1.50000 AFIX 0 N1 3 0.728414 0.519429 0.121427 11.00000 0.01894 0.01905 = 0.01308 0.00348 -0.00032 -0.00192 N2 3 0.751069 0.362146 0.251400 11.00000 0.02145 0.03688 = 0.01635 0.01324 -0.00223 -0.00409 N3 3 0.497759 0.358447 0.117863 11.00000 0.01868 0.02153 = 0.01379 0.00580 -0.00057 -0.00302 N4 3 0.423082 0.559498 0.031376 11.00000 0.01736 0.01895 = 0.00938 0.00251 0.00163 0.00352 P1 4 0.566721 0.463854 0.070571 11.00000 0.01595 0.01541 = 0.00924 0.00310 0.00058 0.00091 P2 4 0.825450 0.465777 0.206884 11.00000 0.01633 0.02094 = 0.01222 0.00235 -0.00092 -0.00054 P3 4 0.588576 0.305731 0.205077 11.00000 0.01906 0.01829 = 0.01169 0.00552 0.00267 0.00111 CL1 5 1.037192 0.412396 0.188544 11.00000 0.01823 0.03224 = 0.03569 0.00786 0.00505 0.00349 CL2 5 0.889303 0.594599 0.291260 11.00000 0.04510 0.03507 = 0.02325 -0.01050 -0.00702 -0.00038 CL3 5 0.622641 0.133630 0.190333 11.00000 0.06271 0.02089 = 0.02974 0.00311 0.00224 0.01205 CL4 5 0.444389 0.303663 0.287595 11.00000 0.02615 0.04480 = 0.02014 0.00745 0.01039 -0.00066 HKLF 4 Covalent radii and connectivity table for 2007src0400 in P2(1)/c C 0.770 H 0.320 N 0.700 P 1.100 CL 0.990 C1 - N4 C2 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 N1 - P2 P1 N2 - P2 P3 N3 - P3 P1 N4 - C1 P1 P1_$1 P1 - N1 N3 N4 N4_$1 P1_$1 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl4 Cl3 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z h k l Fo^2 Sigma Why rejected -5 0 1 2.04 0.23 observed but should be systematically absent -4 0 1 4.30 0.89 observed but should be systematically absent -4 0 1 9.59 1.99 observed but should be systematically absent -4 0 1 3.89 0.56 observed but should be systematically absent -2 0 1 2.63 0.36 observed but should be systematically absent -2 0 1 3.57 0.65 observed but should be systematically absent -2 0 1 2.47 0.50 observed but should be systematically absent 5 0 5 5.80 1.30 observed but should be systematically absent 21040 Reflections read, of which 538 rejected -11 =< h =< 10, -14 =< k =< 13, -20 =< l =< 20, Max. 2-theta = 54.99 8 Systematic absence violations 0 Inconsistent equivalents 3526 Unique reflections, of which 0 suppressed R(int) = 0.0284 R(sigma) = 0.0201 Friedel opposites merged Maximum memory for data reduction = 1634 / 34906 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 = 2050 / 194827 wR2 = 0.0726 before cycle 1 for 3526 data and 155 / 155 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0335 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63799 0.00084 -0.439 OSF Mean shift/esd = 0.050 Maximum = -0.439 for OSF Max. shift = 0.002 A for H6B Max. dU = 0.000 for N3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2050 / 194827 wR2 = 0.0726 before cycle 2 for 3526 data and 155 / 155 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0335 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63787 0.00084 -0.146 OSF Mean shift/esd = 0.017 Maximum = -0.146 for OSF Max. shift = 0.001 A for H6B Max. dU = 0.000 for N3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2050 / 194827 wR2 = 0.0726 before cycle 3 for 3526 data and 155 / 155 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0335 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63787 0.00084 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.013 for tors H6A Max. shift = 0.000 A for H6B Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2050 / 194827 wR2 = 0.0726 before cycle 4 for 3526 data and 155 / 155 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0335 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63787 0.00084 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for tors H6A Max. shift = 0.000 A for H6C Max. dU = 0.000 for C6 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 0.3018 0.5762 0.1264 23 0.990 0.000 C1 N4 C2 H1B 0.2003 0.5169 0.0419 23 0.990 0.000 C1 N4 C2 H2A 0.1870 0.7056 -0.0274 23 0.990 0.000 C2 C1 C3 H2B 0.2748 0.7621 0.0615 23 0.990 0.000 C2 C1 C3 H3A -0.0235 0.6430 0.0394 23 0.990 0.000 C3 C4 C2 H3B 0.0626 0.7073 0.1253 23 0.990 0.000 C3 C4 C2 H4A -0.0560 0.8283 -0.0310 23 0.990 0.000 C4 C3 C5 H4B 0.0242 0.8910 0.0568 23 0.990 0.000 C4 C3 C5 H5A -0.2664 0.7618 0.0332 23 0.990 0.000 C5 C6 C4 H5B -0.1872 0.8288 0.1194 23 0.990 0.000 C5 C6 C4 H6A -0.2308 1.0106 0.0472 137 0.980 0.000 C6 C5 H6A H6B -0.3940 0.9419 0.0422 137 0.980 0.000 C6 C5 H6A H6C -0.3115 0.9431 -0.0385 137 0.980 0.000 C6 C5 H6A 2007src0400 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.27717 0.58005 0.06324 1.00000 0.01901 0.02078 0.01513 0.00172 0.00562 0.00148 0.01801 0.00321 0.00019 0.00015 0.00010 0.00000 0.00077 0.00083 0.00075 0.00062 0.00061 0.00064 0.00032 H1A 0.30185 0.57621 0.12637 1.00000 0.02161 0.00000 0.00000 H1B 0.20026 0.51688 0.04193 1.00000 0.02161 0.00000 0.00000 C2 0.20301 0.69825 0.03538 1.00000 0.01960 0.02028 0.01619 0.00084 0.00381 0.00275 0.01868 0.00321 0.00019 0.00015 0.00011 0.00000 0.00077 0.00082 0.00076 0.00061 0.00061 0.00063 0.00033 H2A 0.18701 0.70558 -0.02743 1.00000 0.02241 0.00000 0.00000 H2B 0.27485 0.76211 0.06152 1.00000 0.02241 0.00000 0.00000 C3 0.04453 0.71059 0.06227 1.00000 0.01830 0.02581 0.01914 -0.00165 0.00332 0.00235 0.02117 0.00330 0.00020 0.00016 0.00011 0.00000 0.00078 0.00090 0.00081 0.00067 0.00063 0.00067 0.00035 H3A -0.02346 0.64303 0.03938 1.00000 0.02540 0.00000 0.00000 H3B 0.06263 0.70733 0.12532 1.00000 0.02540 0.00000 0.00000 C4 -0.04134 0.82327 0.03186 1.00000 0.03055 0.03418 0.02304 0.00506 0.00962 0.01351 0.02867 0.00405 0.00023 0.00018 0.00012 0.00000 0.00096 0.00104 0.00090 0.00077 0.00075 0.00082 0.00041 H4A -0.05598 0.82830 -0.03100 1.00000 0.03441 0.00000 0.00000 H4B 0.02425 0.89104 0.05678 1.00000 0.03441 0.00000 0.00000 C5 -0.20252 0.83124 0.05638 1.00000 0.02683 0.04370 0.03536 0.00208 0.00881 0.00939 0.03496 0.00437 0.00024 0.00021 0.00014 0.00000 0.00097 0.00123 0.00110 0.00093 0.00083 0.00088 0.00046 H5A -0.26636 0.76179 0.03324 1.00000 0.04195 0.00000 0.00000 H5B -0.18722 0.82876 0.11935 1.00000 0.04195 0.00000 0.00000 C6 -0.29259 0.94134 0.02398 1.00000 0.04432 0.05890 0.05021 0.00564 0.01519 0.02774 0.05037 0.00577 0.00031 0.00025 0.00017 0.00000 0.00136 0.00159 0.00145 0.00121 0.00113 0.00120 0.00064 H6A -0.23079 1.01057 0.04720 1.00000 0.07555 0.00000 0.00000 H6B -0.39396 0.94189 0.04216 1.00000 0.07555 0.00000 0.00000 H6C -0.31155 0.94312 -0.03850 1.00000 0.07555 0.00000 0.00000 N1 0.72840 0.51943 0.12143 1.00000 0.01888 0.01902 0.01301 0.00353 -0.00032 -0.00192 0.01750 0.00256 0.00016 0.00012 0.00009 0.00000 0.00066 0.00068 0.00064 0.00052 0.00052 0.00054 0.00028 N2 0.75106 0.36214 0.25140 1.00000 0.02139 0.03681 0.01627 0.01325 -0.00226 -0.00409 0.02572 0.00290 0.00017 0.00014 0.00009 0.00000 0.00074 0.00091 0.00070 0.00064 0.00057 0.00066 0.00034 N3 0.49776 0.35845 0.11786 1.00000 0.01861 0.02144 0.01372 0.00579 -0.00059 -0.00304 0.01850 0.00259 0.00016 0.00013 0.00009 0.00000 0.00067 0.00072 0.00065 0.00053 0.00052 0.00055 0.00029 N4 0.42308 0.55950 0.03138 1.00000 0.01730 0.01889 0.00935 0.00251 0.00162 0.00351 0.01535 0.00256 0.00016 0.00012 0.00008 0.00000 0.00064 0.00066 0.00059 0.00050 0.00049 0.00052 0.00027 P1 0.56672 0.46385 0.07057 1.00000 0.01590 0.01536 0.00920 0.00310 0.00057 0.00091 0.01379 0.00075 0.00005 0.00004 0.00002 0.00000 0.00020 0.00020 0.00019 0.00014 0.00015 0.00015 0.00010 P2 0.82545 0.46578 0.20688 1.00000 0.01627 0.02089 0.01218 0.00235 -0.00093 -0.00054 0.01701 0.00078 0.00005 0.00004 0.00003 0.00000 0.00020 0.00022 0.00020 0.00015 0.00015 0.00016 0.00010 P3 0.58858 0.30573 0.20508 1.00000 0.01901 0.01824 0.01164 0.00552 0.00265 0.00111 0.01637 0.00080 0.00005 0.00004 0.00003 0.00000 0.00021 0.00021 0.00019 0.00015 0.00015 0.00016 0.00010 Cl1 1.03719 0.41240 0.18854 1.00000 0.01818 0.03220 0.03563 0.00786 0.00503 0.00349 0.02875 0.00092 0.00005 0.00004 0.00003 0.00000 0.00021 0.00025 0.00025 0.00019 0.00017 0.00017 0.00012 Cl2 0.88930 0.59460 0.29126 1.00000 0.04505 0.03501 0.02321 -0.01051 -0.00703 -0.00039 0.03647 0.00088 0.00007 0.00005 0.00003 0.00000 0.00030 0.00027 0.00024 0.00019 0.00020 0.00022 0.00013 Cl3 0.62265 0.13363 0.19033 1.00000 0.06264 0.02084 0.02970 0.00311 0.00222 0.01206 0.03880 0.00105 0.00007 0.00004 0.00003 0.00000 0.00036 0.00023 0.00025 0.00018 0.00023 0.00022 0.00014 Cl4 0.44439 0.30366 0.28759 1.00000 0.02611 0.04476 0.02009 0.00745 0.01038 -0.00066 0.02951 0.00092 0.00005 0.00005 0.00003 0.00000 0.00022 0.00028 0.00021 0.00018 0.00017 0.00019 0.00012 Final Structure Factor Calculation for 2007src0400 in P2(1)/c Total number of l.s. parameters = 155 Maximum vector length = 511 Memory required = 1895 / 24017 wR2 = 0.0726 before cycle 5 for 3526 data and 0 / 155 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0335 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0284 for 3218 Fo > 4sig(Fo) and 0.0321 for all 3526 data wR2 = 0.0726, GooF = S = 1.070, Restrained GooF = 1.070 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0222 0.0183 0.0136 C1 0.0227 0.0173 0.0160 C2 0.0271 0.0188 0.0176 C3 0.0466 0.0211 0.0183 C4 0.0480 0.0349 0.0219 C5 0.0807 0.0484 0.0220 C6 0.0244 0.0170 0.0110 N1 0.0468 0.0210 0.0094 N2 0.0283 0.0167 0.0105 N3 0.0217 0.0158 0.0086 N4 0.0172 0.0165 0.0077 P1 0.0225 0.0183 0.0102 P2 0.0214 0.0192 0.0085 P3 0.0420 0.0269 0.0173 Cl1 0.0572 0.0378 0.0144 Cl2 0.0690 0.0307 0.0167 Cl3 0.0468 0.0281 0.0136 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.038 0.058 0.078 0.101 0.128 0.157 0.200 0.277 1.000 Number in group 353. 364. 341. 353. 355. 350. 358. 345. 355. 352. GooF 1.104 1.024 1.133 1.034 1.085 1.001 1.064 0.959 0.958 1.302 K 1.424 1.023 0.966 0.973 0.983 0.991 1.003 1.015 1.016 0.971 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 358. 361. 353. 349. 351. 343. 355. 349. 354. 353. GooF 0.984 0.928 0.881 0.822 0.831 0.858 0.968 0.911 1.067 1.959 K 0.965 0.995 1.005 1.005 1.016 1.022 1.014 1.000 1.001 0.949 R1 0.061 0.048 0.042 0.030 0.027 0.027 0.026 0.020 0.020 0.038 Recommended weighting scheme: WGHT 0.0332 1.2033 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) 0 1 4 21748.05 28451.47 6.88 0.996 3.70 2 0 2 19929.68 28668.10 6.51 1.000 3.44 0 0 4 15982.45 19892.97 5.61 0.833 3.92 1 3 5 26.09 4.59 4.84 0.013 2.23 -5 0 4 56.04 22.84 4.48 0.028 1.69 -1 2 5 30.52 70.19 4.37 0.049 2.76 1 2 1 9094.29 10801.38 4.35 0.614 4.38 2 3 1 186.57 122.71 4.27 0.065 2.71 3 2 2 362.09 264.95 4.26 0.096 2.28 0 0 8 23761.68 28065.09 4.23 0.989 1.96 -3 3 3 177.37 117.25 4.16 0.064 2.22 9 2 6 156.88 240.93 4.00 0.092 0.82 -3 1 1 7.82 0.01 3.96 0.001 2.79 3 2 3 377.02 284.55 3.91 0.100 2.12 1 1 3 14883.03 17447.33 3.90 0.780 3.84 0 2 7 603.35 477.89 3.74 0.129 2.08 1 0 8 1918.08 1611.96 3.66 0.237 1.83 3 3 1 576.12 461.33 3.64 0.127 2.19 -2 3 7 667.42 540.88 3.61 0.137 1.89 2 4 3 19105.37 21908.69 3.59 0.874 2.06 -3 3 6 416.63 527.17 3.55 0.136 1.87 2 4 2 1424.49 1685.46 3.52 0.242 2.19 3 3 4 11.11 1.56 3.48 0.007 1.83 2 3 5 1141.19 958.83 3.42 0.183 1.97 1 2 6 267.76 349.77 3.41 0.110 2.18 -2 2 5 52.78 90.25 3.38 0.056 2.52 2 1 1 10801.75 12320.31 3.33 0.656 3.68 -4 2 3 24.50 49.43 3.30 0.042 1.99 0 3 2 10887.92 12355.72 3.30 0.656 3.41 1 4 3 3662.44 4190.35 3.27 0.382 2.33 -6 3 2 11.78 0.09 3.23 0.002 1.35 4 8 2 672.94 554.17 3.20 0.139 1.15 7 10 5 18.02 65.43 3.19 0.048 0.77 2 1 0 7411.81 8412.37 3.18 0.542 3.97 1 6 8 165.02 118.54 3.13 0.064 1.31 5 1 0 686.89 820.46 3.08 0.169 1.67 -4 6 4 89.11 130.14 3.06 0.067 1.39 -1 5 2 5998.70 5328.32 3.06 0.431 2.14 2 2 4 4868.04 5506.69 3.05 0.438 2.38 -1 3 3 1088.67 935.85 3.00 0.181 3.00 0 2 4 1195.51 1031.70 3.00 0.190 3.22 -3 0 2 49.24 27.79 2.98 0.031 2.85 0 1 6 58.31 90.13 2.96 0.056 2.54 0 6 0 237.08 179.42 2.94 0.079 1.89 -3 6 3 291.58 363.87 2.94 0.113 1.56 -1 4 6 6.40 0.01 2.93 0.000 1.94 -3 6 5 87.80 58.38 2.86 0.045 1.48 -3 2 7 565.38 671.57 2.86 0.153 1.86 -1 4 5 24.89 11.00 2.84 0.020 2.11 -2 4 13 23.99 9.49 2.84 0.018 1.13 Bond lengths and angles C1 - Distance Angles N4 1.4753 (0.0020) C2 1.5152 (0.0023) 112.27 (0.13) C1 - N4 C2 - Distance Angles C1 1.5152 (0.0023) C3 1.5267 (0.0023) 110.40 (0.14) C2 - C1 C3 - Distance Angles C4 1.5093 (0.0025) C2 1.5267 (0.0023) 113.43 (0.15) C3 - C4 C4 - Distance Angles C3 1.5093 (0.0025) C5 1.5281 (0.0026) 112.44 (0.17) C4 - C3 C5 - Distance Angles C6 1.5079 (0.0031) C4 1.5281 (0.0026) 113.24 (0.19) C5 - C6 C6 - Distance Angles C5 1.5079 (0.0031) C6 - N1 - Distance Angles P2 1.5723 (0.0014) P1 1.5954 (0.0014) 122.94 (0.09) N1 - P2 N2 - Distance Angles P2 1.5813 (0.0015) P3 1.5823 (0.0015) 119.70 (0.09) N2 - P2 N3 - Distance Angles P3 1.5720 (0.0014) P1 1.5975 (0.0014) 122.69 (0.09) N3 - P3 N4 - Distance Angles C1 1.4753 (0.0020) P1 1.6718 (0.0014) 126.57 (0.11) P1_$1 1.6748 (0.0013) 125.79 (0.11) 94.43 (0.07) N4 - C1 P1 P1 - Distance Angles N1 1.5954 (0.0014) N3 1.5975 (0.0014) 115.40 (0.07) N4 1.6718 (0.0014) 116.02 (0.07) 110.10 (0.07) N4_$1 1.6748 (0.0013) 110.01 (0.07) 116.37 (0.07) 85.57 (0.07) P1_$1 2.4562 (0.0008) 122.14 (0.06) 122.46 (0.06) 42.83 (0.05) 42.74 (0.05) P1 - N1 N3 N4 N4_$1 P2 - Distance Angles N1 1.5723 (0.0014) N2 1.5813 (0.0015) 119.18 (0.08) Cl2 1.9910 (0.0006) 109.17 (0.06) 108.84 (0.06) Cl1 2.0085 (0.0006) 109.14 (0.06) 108.07 (0.06) 100.87 (0.03) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5720 (0.0014) N2 1.5823 (0.0015) 119.57 (0.08) Cl4 1.9974 (0.0006) 109.09 (0.06) 108.10 (0.06) Cl3 1.9990 (0.0006) 109.06 (0.06) 108.26 (0.07) 101.21 (0.03) P3 - N3 N2 Cl4 Cl1 - Distance Angles P2 2.0085 (0.0006) Cl1 - Cl2 - Distance Angles P2 1.9910 (0.0006) Cl2 - Cl3 - Distance Angles P3 1.9990 (0.0006) Cl3 - Cl4 - Distance Angles P3 1.9974 (0.0006) Cl4 - FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0319 for 3526 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.6952 0.8389 0.0104 [ 0.98 A from H5A ] Deepest hole -0.48 at 0.5706 0.8588 0.1967 [ 0.70 A from CL4 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1981 / 19437 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3048 0.8389 0.0104 1.00000 0.05 0.55 0.98 H5A 1.03 C5 1.19 C6 1.41 H6C Q2 1 -0.1568 0.9068 0.0662 1.00000 0.05 0.41 0.94 C5 1.29 C6 1.29 H5B 1.35 H6A Q3 1 0.4454 0.2438 0.2679 1.00000 0.05 0.35 0.75 CL4 1.89 P3 2.50 CL3 2.85 N3 Q4 1 0.0067 0.8851 0.0351 1.00000 0.05 0.34 0.35 H4B 0.81 C4 1.26 H4A 2.01 C5 Q5 1 0.0177 0.7762 0.0537 1.00000 0.05 0.28 0.77 C4 0.78 C3 1.31 H4B 1.38 H3B Q6 1 0.0109 0.8769 -0.0078 1.00000 0.05 0.27 0.83 H4A 1.03 H4B 1.05 C4 2.19 C3 Q7 1 0.7749 0.5119 0.1541 1.00000 0.05 0.26 0.60 N1 1.01 P2 2.08 P1 2.35 N2 Q8 1 0.6993 0.5445 0.1299 1.00000 0.05 0.25 0.42 N1 1.61 P1 1.72 P2 2.58 N4 Q9 1 0.5245 0.3744 0.0911 1.00000 0.05 0.24 0.56 N3 1.15 P1 1.96 P3 2.23 N4 Q10 1 0.7141 0.4686 0.0986 1.00000 0.05 0.24 0.68 N1 1.26 P1 1.80 P2 2.19 N4 Q11 1 0.7774 0.3559 0.2713 1.00000 0.05 0.24 0.36 N2 1.73 P2 1.84 P3 2.56 H3B Q12 1 0.4332 0.3276 0.1054 1.00000 0.05 0.24 0.65 N3 1.88 P3 2.08 P1 2.59 H5A Q13 1 0.6799 0.3580 0.2671 1.00000 0.05 0.24 0.71 N2 1.28 P3 2.13 P2 2.22 CL4 Q14 1 -0.1475 0.8949 0.1417 1.00000 0.05 0.24 0.87 H5B 1.53 C5 2.02 H6A 2.10 C6 Q15 1 -0.3597 0.8479 -0.1132 1.00000 0.05 0.22 1.60 H6C 2.36 CL3 2.40 C6 2.51 H5A Q16 1 0.7877 0.4806 0.1258 1.00000 0.05 0.22 0.67 N1 1.28 P2 1.94 P1 2.32 CL1 Q17 1 0.8138 0.5750 0.3076 1.00000 0.05 0.22 0.78 CL2 2.05 P2 2.60 N2 2.82 H4A Q18 1 0.4965 0.5378 0.0560 1.00000 0.05 0.22 0.72 N4 1.03 P1 1.98 C1 1.99 P1 Q19 1 0.2362 0.6409 0.0498 1.00000 0.05 0.21 0.73 C2 0.79 C1 1.42 H2B 1.42 H2A Q20 1 0.6462 0.5042 0.1017 1.00000 0.05 0.21 0.74 N1 0.89 P1 2.09 P2 2.12 N4 Shortest distances between peaks (including symmetry equivalents) 7 16 0.60 4 6 0.70 10 16 0.71 10 20 0.72 8 20 0.73 7 8 0.78 11 13 0.83 9 12 1.02 8 10 1.02 7 10 1.06 8 16 1.07 2 14 1.20 16 20 1.23 7 20 1.25 4 5 1.27 18 20 1.40 5 6 1.50 1 2 1.60 2 4 1.61 9 20 1.80 8 18 1.90 1 15 1.94 9 18 1.94 9 10 1.94 18 18 2.00 10 18 2.02 2 6 2.08 12 15 2.10 2 5 2.16 15 17 2.33 1 14 2.34 4 14 2.38 3 13 2.41 5 19 2.45 8 9 2.45 7 17 2.51 18 19 2.52 9 18 2.53 9 16 2.53 11 17 2.56 7 11 2.58 5 14 2.59 7 18 2.60 12 18 2.61 18 20 2.61 16 18 2.62 3 15 2.65 7 9 2.69 1 4 2.69 1 12 2.72 12 20 2.73 4 6 2.74 13 17 2.74 11 16 2.74 10 18 2.75 3 12 2.75 7 13 2.76 10 19 2.79 6 6 2.82 1 5 2.82 8 17 2.83 4 4 2.84 1 6 2.84 9 13 2.87 10 12 2.93 9 15 2.96 13 16 2.97 10 11 2.99 2 6 3.00 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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. 4.95: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.99: Structure factors and derivatives 1.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0400 finished at 18:00:08 Total CPU time: 7.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++