+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0008 started at 18:23:12 on 03-Feb-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0008 in C2/c CELL 0.71073 32.1378 8.5084 11.6735 90.000 110.275 90.000 ZERR 4.00 0.0021 0.0006 0.0005 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O P CL UNIT 56 116 36 28 24 8 V = 2994.24 F(000) = 1424.0 Mu = 0.59 mm-1 Cell Wt = 2768.73 Rho = 1.535 MERG 2 OMIT -3.00 55.00 ISOR 0.001 N5 C7 C8 C9 FMAP 2 PLAN 10 SIZE 0.04 0.04 0.14 ACTA WGHT 0.02560 47.16760 L.S. 5 TEMP -153.00 FVAR 2.93896 C1 1 0.020356 0.872683 0.361389 11.00000 0.05702 0.05508 = 0.04074 -0.00132 0.01589 -0.00895 AFIX 23 H1A 2 -0.003396 0.811558 0.376742 11.00000 -1.20000 H1B 2 0.041143 0.797626 0.344916 11.00000 -1.20000 AFIX 0 C2 1 0.000000 0.979169 0.250000 10.50000 0.08584 0.05096 = 0.02094 0.00000 0.01543 0.00000 C3 1 0.035944 1.078969 0.230270 11.00000 0.09873 0.05284 = 0.02990 -0.00216 0.02722 -0.00953 AFIX 23 H3A 2 0.057854 1.010183 0.212738 11.00000 -1.20000 H3B 2 0.022673 1.148697 0.159002 11.00000 -1.20000 AFIX 0 C4 1 0.125566 1.564214 0.665711 11.00000 0.25302 0.07163 = 0.10788 0.00827 0.09272 -0.02443 AFIX 23 H4A 2 0.093100 1.562309 0.622059 11.00000 -1.20000 H4B 2 0.137116 1.663639 0.644311 11.00000 -1.20000 AFIX 0 C5 1 0.134378 1.561987 0.799097 11.00000 0.16890 0.05461 = 0.08700 -0.02654 0.05470 -0.00429 AFIX 23 H5A 2 0.117631 1.647842 0.820615 11.00000 -1.20000 H5B 2 0.166373 1.579938 0.843551 11.00000 -1.20000 AFIX 0 C6 1 0.120778 1.405872 0.837490 11.00000 0.26801 0.08468 = 0.08546 0.01103 0.10979 0.01141 AFIX 23 H6A 2 0.131689 1.401678 0.927830 11.00000 -1.20000 H6B 2 0.087977 1.401703 0.808984 11.00000 -1.20000 AFIX 0 N1 3 0.087419 1.211649 0.566096 11.00000 0.06665 0.06247 = 0.04026 -0.01036 0.01174 0.01981 N2 3 0.174555 1.161342 0.651469 11.00000 0.05374 0.08914 = 0.12693 -0.04955 0.00451 0.01859 N3 3 0.122724 0.992043 0.462118 11.00000 0.10107 0.05917 = 0.09779 -0.04018 0.06671 -0.03127 O3 4 0.144502 1.439813 0.626138 11.00000 0.15964 0.05975 = 0.07933 0.00101 0.07902 0.00665 O1 4 0.043897 0.966029 0.468637 11.00000 0.07343 0.06943 = 0.02787 0.00140 0.01909 -0.00478 O2 4 0.057960 1.172701 0.337109 11.00000 0.13304 0.06686 = 0.03075 -0.01793 0.02654 -0.03826 N4 3 0.135365 1.278054 0.796260 11.00000 0.12317 0.04010 = 0.03436 -0.00152 0.01127 -0.01013 AFIX 43 H4 2 0.145422 1.198203 0.846115 11.00000 -1.20000 AFIX 0 P1 5 0.080886 1.085278 0.463604 11.00000 0.08238 0.05908 = 0.03608 -0.01431 0.02652 -0.00870 P2 5 0.135110 1.265508 0.657200 11.00000 0.08538 0.04290 = 0.04658 -0.01045 0.01788 0.00478 P3 5 0.170736 1.031934 0.554071 11.00000 0.08305 0.05382 = 0.12150 -0.01395 0.05598 0.00132 PART 1 CL1 6 0.209130 0.838578 0.663749 10.50000 0.08994 0.10285 = 0.05056 0.01114 0.00589 0.03010 CL2 6 0.216567 1.078582 0.475010 10.50000 0.08048 0.07189 = 0.13335 0.01376 0.05479 0.00266 PART 2 N5 3 0.182240 0.869520 0.599268 10.50000 0.03894 0.03907 = 0.03956 0.00023 0.01324 0.00040 AFIX 43 H5 2 0.163172 0.793748 0.595504 10.50000 -1.20000 AFIX 0 O4 4 0.196104 1.086004 0.462476 10.50000 0.07260 0.18881 = 0.23270 0.05824 0.10640 0.06128 C7 1 0.227936 0.856504 0.648425 10.50000 0.12156 0.12159 = 0.12152 0.00006 0.04220 0.00002 AFIX 23 H7A 2 0.239440 0.940314 0.710176 10.50000 -1.20000 H7B 2 0.235498 0.754259 0.691100 10.50000 -1.20000 AFIX 0 C8 1 0.250006 0.867416 0.561178 10.50000 0.09895 0.09912 = 0.09897 -0.00011 0.03422 0.00008 AFIX 23 H8A 2 0.238171 0.787589 0.496287 10.50000 -1.20000 H8B 2 0.282229 0.849224 0.601492 10.50000 -1.20000 AFIX 0 C9 1 0.242338 1.018592 0.511170 10.50000 0.07365 0.07378 = 0.07390 0.00002 0.02550 -0.00012 AFIX 23 H9A 2 0.254267 1.021349 0.443562 10.50000 -1.20000 H9B 2 0.260595 1.091840 0.574622 10.50000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src0008 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3_$1 C3 C1_$1 C1 C3 - O2 C2 C4 - O3 C5 C5 - C4 C6 C6 - N4 C5 N1 - P1 P2 N2 - P3 P2 N3 - P1 P3 O3 - C4 P2 O1 - C1 P1 O2 - C3 P1 N4 - C6 P2 P1 - N3 N1 O1 O2 P2 - N2 O3 N1 N4 P3 - N5_b N2 N3 O4_b Cl2_a Cl1_a C7_b Cl1_a - P3 Cl2_a - P3 N5_b - C7_b P3 O4_b - C9_b P3 C7_b - N5_b C8_b P3 C8_b - C9_b C7_b C9_b - C8_b O4_b Operators for generating equivalent atoms: $1 -x, y, -z+1/2 15445 Reflections read, of which 10 rejected -38 =< h =< 41, -11 =< k =< 10, -15 =< l =< 14, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 16 0 4 4708.55 414.26 4 2247.78 -2 2 13 4000.62 949.68 2 5041.00 2 Inconsistent equivalents 3392 Unique reflections, of which 0 suppressed R(int) = 0.1264 R(sigma) = 0.1554 Friedel opposites merged Maximum memory for data reduction = 2146 / 41828 Special position constraints for C2 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 2734 / 254845 wR2 = 0.2590 before cycle 1 for 3392 data and 204 / 204 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.93872 0.01238 -0.020 OSF Mean shift/esd = 0.018 Maximum = 0.173 for U11 Cl2_a Max. shift = 0.004 A for C7_b Max. dU = 0.001 for O4_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 2734 / 254845 wR2 = 0.2590 before cycle 2 for 3392 data and 204 / 204 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.93886 0.01239 0.011 OSF Mean shift/esd = 0.014 Maximum = 0.173 for U11 Cl2_a Max. shift = 0.003 A for O4_b Max. dU = 0.001 for O4_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 2734 / 254845 wR2 = 0.2590 before cycle 3 for 3392 data and 204 / 204 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.93886 0.01239 0.000 OSF Mean shift/esd = 0.008 Maximum = 0.115 for U11 Cl2_a Max. shift = 0.002 A for O4_b Max. dU = 0.001 for O4_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2734 / 254845 wR2 = 0.2590 before cycle 4 for 3392 data and 204 / 204 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.93886 0.01239 0.000 OSF Mean shift/esd = 0.005 Maximum = 0.077 for U11 Cl2_a Max. shift = 0.002 A for O4_b Max. dU = 0.001 for O4_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2734 / 254845 wR2 = 0.2590 before cycle 5 for 3392 data and 204 / 204 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.93885 0.01239 -0.001 OSF Mean shift/esd = 0.003 Maximum = 0.051 for U11 Cl2_a Max. shift = 0.001 A for O4_b Max. dU = 0.000 for O4_b Largest correlation matrix elements 0.996 U33 C7_b / U22 C7_b 0.982 U33 C8_b / U11 C8_b 0.938 U13 C9_b / U11 C9_b 0.996 U22 C7_b / U11 C7_b 0.979 U33 C9_b / U22 C9_b 0.936 U13 C9_b / U22 C9_b 0.996 U33 C7_b / U11 C7_b 0.979 U22 C9_b / U11 C9_b 0.903 U22 N5_b / U11 N5_b 0.986 U13 C7_b / U11 C7_b 0.979 U33 C9_b / U11 C9_b 0.902 U33 N5_b / U22 N5_b 0.986 U13 C7_b / U33 C7_b 0.945 U13 C8_b / U33 C8_b 0.901 U33 N5_b / U11 N5_b 0.986 U13 C7_b / U22 C7_b 0.945 U13 C8_b / U11 C8_b 0.779 U13 N5_b / U11 N5_b 0.982 U22 C8_b / U11 C8_b 0.944 U13 C8_b / U22 C8_b 0.779 U13 N5_b / U33 N5_b 0.982 U33 C8_b / U22 C8_b 0.939 U13 C9_b / U33 C9_b 0.769 U13 N5_b / U22 N5_b Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0034 0.8116 0.3767 23 0.990 0.000 C1 O1 C2 H1B 0.0411 0.7977 0.3449 23 0.990 0.000 C1 O1 C2 H3A 0.0578 1.0102 0.2127 23 0.990 0.000 C3 O2 C2 H3B 0.0226 1.1487 0.1590 23 0.990 0.000 C3 O2 C2 H4A 0.0931 1.5624 0.6221 23 0.990 0.000 C4 O3 C5 H4B 0.1371 1.6637 0.6443 23 0.990 0.000 C4 O3 C5 H5A 0.1176 1.6479 0.8206 23 0.990 0.000 C5 C4 C6 H5B 0.1664 1.5799 0.8435 23 0.990 0.000 C5 C4 C6 H6A 0.1317 1.4017 0.9278 23 0.990 0.000 C6 N4 C5 H6B 0.0880 1.4017 0.8089 23 0.990 0.000 C6 N4 C5 H4 0.1454 1.1982 0.8461 43 0.880 0.000 N4 C6 P2 H5 0.1632 0.7935 0.5951 43 0.880 0.000 N5_b C7_b P3 ** Bond(s) to P3 ignored in idealizing H-atoms attached to C7_b ** H7A 0.2355 0.7558 0.6921 23 0.990 0.000 C7_b N5_b C8_b H7B 0.2392 0.9421 0.7095 23 0.990 0.000 C7_b N5_b C8_b H8A 0.2822 0.8489 0.6017 23 0.990 0.000 C8_b C9_b C7_b H8B 0.2381 0.7872 0.4965 23 0.990 0.000 C8_b C9_b C7_b H9A 0.2542 1.0212 0.4438 23 0.990 0.000 C9_b C8_b O4_b H9B 0.2606 1.0914 0.5749 23 0.990 0.000 C9_b C8_b O4_b 2008src0008 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.02036 0.87271 0.36138 1.00000 0.05717 0.05496 0.04068 -0.00137 0.01597 -0.00914 0.05120 0.01615 0.00029 0.00104 0.00067 0.00000 0.00565 0.00593 0.00438 0.00413 0.00408 0.00465 0.00227 H1A -0.00339 0.81157 0.37673 1.00000 0.06144 0.00000 0.00000 H1B 0.04115 0.79767 0.34491 1.00000 0.06144 0.00000 0.00000 C2 0.00000 0.97914 0.25000 0.50000 0.08565 0.05121 0.02090 0.00000 0.01535 0.00000 0.05340 0.01254 0.00000 0.00147 0.00000 0.00000 0.00962 0.00791 0.00496 0.00000 0.00574 0.00000 0.00338 C3 0.03592 1.07898 0.23026 1.00000 0.09860 0.05296 0.02997 -0.00211 0.02730 -0.00951 0.05919 0.01698 0.00033 0.00110 0.00067 0.00000 0.00749 0.00583 0.00396 0.00409 0.00453 0.00550 0.00257 H3A 0.05783 1.01022 0.21268 1.00000 0.07103 0.00000 0.00000 H3B 0.02264 1.14872 0.15901 1.00000 0.07103 0.00000 0.00000 C4 0.12554 1.56430 0.66570 1.00000 0.25257 0.07145 0.10799 0.00818 0.09280 -0.02426 0.13604 0.03222 0.00061 0.00159 0.00123 0.00000 0.01980 0.00962 0.01082 0.00834 0.01223 0.01139 0.00612 H4A 0.09307 1.56238 0.62205 1.00000 0.16325 0.00000 0.00000 H4B 0.13709 1.66373 0.64431 1.00000 0.16325 0.00000 0.00000 C5 0.13436 1.56200 0.79907 1.00000 0.16889 0.05478 0.08702 -0.02652 0.05472 -0.00409 0.10084 0.02494 0.00049 0.00131 0.00104 0.00000 0.01322 0.00777 0.00824 0.00653 0.00851 0.00777 0.00426 H5A 0.11762 1.64786 0.82062 1.00000 0.12101 0.00000 0.00000 H5B 0.16636 1.57992 0.84351 1.00000 0.12101 0.00000 0.00000 C6 0.12075 1.40586 0.83747 1.00000 0.26757 0.08462 0.08559 0.01094 0.10977 0.01118 0.13318 0.03312 0.00060 0.00161 0.00113 0.00000 0.01994 0.01009 0.00880 0.00785 0.01139 0.01165 0.00610 H6A 0.13165 1.40167 0.92781 1.00000 0.15981 0.00000 0.00000 H6B 0.08795 1.40168 0.80893 1.00000 0.15981 0.00000 0.00000 N1 0.08741 1.21167 0.56609 1.00000 0.06647 0.06243 0.04026 -0.01035 0.01164 0.01987 0.05819 0.01424 0.00024 0.00090 0.00057 0.00000 0.00511 0.00518 0.00361 0.00362 0.00348 0.00417 0.00208 N2 0.17456 1.16134 0.65146 1.00000 0.05362 0.08914 0.12699 -0.04963 0.00460 0.01846 0.09692 0.01677 0.00027 0.00112 0.00090 0.00000 0.00544 0.00715 0.00803 0.00621 0.00533 0.00500 0.00338 N3 0.12273 0.99202 0.46211 1.00000 0.10092 0.05912 0.09791 -0.04020 0.06669 -0.03126 0.07752 0.01644 0.00030 0.00093 0.00078 0.00000 0.00684 0.00562 0.00644 0.00483 0.00580 0.00503 0.00270 O3 0.14449 1.43983 0.62613 1.00000 0.15944 0.05981 0.07929 0.00104 0.07893 0.00659 0.08965 0.01650 0.00029 0.00086 0.00063 0.00000 0.00750 0.00493 0.00477 0.00395 0.00510 0.00491 0.00247 O1 0.04389 0.96602 0.46864 1.00000 0.07327 0.06951 0.02796 0.00130 0.01908 -0.00466 0.05651 0.01138 0.00020 0.00072 0.00044 0.00000 0.00415 0.00421 0.00267 0.00281 0.00275 0.00350 0.00164 O2 0.05796 1.17271 0.33710 1.00000 0.13309 0.06681 0.03086 -0.01797 0.02664 -0.03824 0.07739 0.01165 0.00025 0.00077 0.00047 0.00000 0.00624 0.00455 0.00295 0.00309 0.00347 0.00433 0.00222 N4 0.13535 1.27806 0.79626 1.00000 0.12341 0.04006 0.03428 -0.00150 0.01129 -0.01019 0.07013 0.01422 0.00029 0.00091 0.00058 0.00000 0.00744 0.00468 0.00366 0.00353 0.00417 0.00476 0.00251 H4 0.14542 1.19822 0.84612 1.00000 0.08415 0.00000 0.00000 P1 0.08089 1.08529 0.46360 1.00000 0.08233 0.05913 0.03607 -0.01429 0.02649 -0.00872 0.05761 0.00495 0.00009 0.00031 0.00020 0.00000 0.00186 0.00166 0.00113 0.00115 0.00116 0.00145 0.00074 P2 0.13511 1.26551 0.65720 1.00000 0.08546 0.04291 0.04661 -0.01042 0.01792 0.00483 0.05963 0.00508 0.00009 0.00029 0.00021 0.00000 0.00194 0.00153 0.00127 0.00114 0.00125 0.00137 0.00076 P3 0.17073 1.03194 0.55407 1.00000 0.08306 0.05382 0.12148 -0.01390 0.05595 0.00139 0.08074 0.00693 0.00011 0.00035 0.00033 0.00000 0.00218 0.00176 0.00260 0.00177 0.00204 0.00162 0.00098 Cl1_a 0.20909 0.83848 0.66376 0.50000 0.09041 0.10284 0.05075 0.01125 0.00636 0.02912 0.08608 0.01562 0.00029 0.00092 0.00053 0.00000 0.00539 0.00524 0.00304 0.00303 0.00361 0.00441 0.00212 Cl2_a 0.21648 1.07848 0.47477 0.50000 0.08471 0.07116 0.13250 0.01364 0.05587 0.00230 0.09134 0.02146 0.00035 0.00109 0.00105 0.00000 0.00738 0.00499 0.00629 0.00437 0.00623 0.00505 0.00246 N5_b 0.18222 0.86949 0.59912 0.50000 0.03925 0.03937 0.03985 0.00023 0.01334 0.00041 0.03959 0.02751 0.00047 0.00158 0.00121 0.00000 0.00326 0.00328 0.00324 0.00101 0.00144 0.00101 0.00314 H5_b 0.16320 0.79348 0.59515 0.50000 0.04750 0.00000 0.00000 O4_b 0.19641 1.08640 0.46311 0.50000 0.08210 0.18991 0.23701 0.05891 0.11243 0.06377 0.15467 0.07890 0.00082 0.00431 0.00374 0.00000 0.01902 0.02671 0.02924 0.02027 0.02182 0.01821 0.01485 C7_b 0.22785 0.85736 0.64847 0.50000 0.11884 0.11885 0.11879 0.00007 0.04118 0.00002 0.11883 0.07758 0.00109 0.00522 0.00333 0.00000 0.01559 0.01559 0.01559 0.00103 0.00547 0.00103 0.01557 H7A_b 0.23552 0.75576 0.69205 0.50000 0.14259 0.00000 0.00000 H7B_b 0.23920 0.94207 0.70951 0.50000 0.14259 0.00000 0.00000 C8_b 0.25001 0.86713 0.56130 0.50000 0.09885 0.09902 0.09888 -0.00011 0.03418 0.00009 0.09894 0.05166 0.00085 0.00300 0.00221 0.00000 0.00764 0.00765 0.00764 0.00102 0.00279 0.00102 0.00759 H8A_b 0.28223 0.84893 0.60169 0.50000 0.11872 0.00000 0.00000 H8B_b 0.23814 0.78720 0.49651 0.50000 0.11872 0.00000 0.00000 C9_b 0.24226 1.01840 0.51143 0.50000 0.07532 0.07545 0.07556 0.00003 0.02607 -0.00013 0.07546 0.04997 0.00086 0.00300 0.00222 0.00000 0.00715 0.00716 0.00715 0.00102 0.00263 0.00102 0.00710 H9A_b 0.25417 1.02121 0.44379 0.50000 0.09055 0.00000 0.00000 H9B_b 0.26060 1.09142 0.57494 0.50000 0.09055 0.00000 0.00000 Final Structure Factor Calculation for 2008src0008 in C2/c Total number of l.s. parameters = 204 Maximum vector length = 511 Memory required = 2530 / 25039 wR2 = 0.2590 before cycle 6 for 3392 data and 0 / 204 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 24. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.050 for 24 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0256 * P )^2 + 47.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1412 for 1551 Fo > 4sig(Fo) and 0.2595 for all 3392 data wR2 = 0.2590, GooF = S = 1.053, Restrained GooF = 1.050 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 14.50 for hydrogen atoms Principal mean square atomic displacements U 0.0660 0.0471 0.0404 C1 0.0892 0.0512 0.0198 C2 0.1012 0.0511 0.0253 C3 0.2558 0.0960 0.0563 C4 may be split into 0.1318 1.5613 0.6661 and 0.1193 1.5673 0.6654 0.1692 0.0961 0.0372 C5 0.2698 0.0850 0.0447 C6 may be split into 0.1276 1.4075 0.8391 and 0.1139 1.4043 0.8358 0.0940 0.0468 0.0338 N1 0.1889 0.0587 0.0432 N2 0.1454 0.0536 0.0335 N3 0.1653 0.0599 0.0437 O3 0.0775 0.0664 0.0257 O1 0.1529 0.0559 0.0233 O2 0.1371 0.0394 0.0338 N4 0.0853 0.0611 0.0264 P1 0.0911 0.0548 0.0330 P2 0.1272 0.0687 0.0463 P3 0.1307 0.0848 0.0428 Cl1_a 0.1369 0.0733 0.0639 Cl2_a 0.0402 0.0397 0.0388 N5_b 0.2881 0.1530 0.0230 O4_b 0.1189 0.1188 0.1187 C7_b 0.0992 0.0988 0.0988 C8_b 0.0757 0.0755 0.0752 C9_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.012 0.018 0.024 0.032 0.043 0.057 0.082 0.137 1.000 Number in group 369. 353. 351. 323. 315. 352. 313. 347. 331. 338. GooF 1.056 1.119 1.137 1.085 1.012 0.940 1.061 1.015 1.093 0.999 K 133.038 20.917 8.052 4.094 2.532 1.617 1.378 1.080 0.969 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.33 1.66 inf Number in group 339. 344. 342. 344. 329. 340. 337. 337. 338. 342. GooF 0.982 1.160 1.109 1.066 1.032 1.021 0.975 0.937 0.947 1.255 K 4.385 3.674 2.833 2.129 1.590 1.329 0.999 1.028 0.992 1.020 R1 0.668 0.602 0.537 0.508 0.411 0.351 0.207 0.126 0.104 0.061 Recommended weighting scheme: WGHT 0.0253 47.3134 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) 6 2 0 2856.78 951.92 5.85 0.091 3.25 9 3 0 509.00 33.63 4.39 0.017 2.16 1 3 0 647.79 51.79 4.05 0.021 2.82 -35 3 8 924.04 102.17 4.01 0.030 0.84 8 2 0 787.32 1856.62 3.69 0.127 2.82 5 3 0 3213.17 1853.77 3.68 0.127 2.57 -12 2 3 417.18 11.30 3.53 0.010 2.17 -24 8 2 917.32 57.69 3.38 0.022 0.83 5 1 0 46782.98 54079.76 3.35 0.686 4.92 2 8 7 925.62 161.50 3.28 0.037 0.87 -11 9 7 1941.11 13.02 3.11 0.011 0.82 -20 4 5 509.40 7.81 3.03 0.008 1.23 -27 7 2 614.05 43.34 3.02 0.019 0.85 14 8 5 516.50 18.59 2.98 0.013 0.83 -24 2 9 1094.02 376.42 2.97 0.057 1.05 20 4 8 1721.55 214.90 2.96 0.043 0.81 -10 2 2 17891.28 14735.81 2.95 0.358 2.53 29 5 3 1123.33 29.30 2.93 0.016 0.81 2 4 0 285.40 1.58 2.88 0.004 2.11 -31 5 7 629.34 24.84 2.88 0.015 0.86 14 6 1 1113.42 431.84 2.88 0.061 1.15 -36 0 4 1305.08 356.28 2.87 0.056 0.89 18 0 2 819.92 5.39 2.86 0.007 1.47 4 4 12 645.68 15.04 2.85 0.011 0.81 -26 6 10 735.33 40.91 2.84 0.019 0.81 -20 6 1 1054.77 294.81 2.81 0.051 1.05 21 3 2 82.63 478.30 2.80 0.065 1.17 0 2 0 32020.25 25673.76 2.79 0.473 4.25 -18 2 13 644.43 4.39 2.77 0.006 0.87 -7 1 2 236.93 0.15 2.77 0.001 3.73 4 4 0 11029.59 13525.08 2.76 0.343 2.05 14 2 3 407.31 25.28 2.76 0.015 1.52 23 1 6 907.80 45.73 2.73 0.020 0.92 3 5 4 469.57 1116.88 2.73 0.099 1.39 -29 7 3 702.47 157.10 2.68 0.037 0.82 -20 6 8 581.84 33.98 2.67 0.017 0.94 -31 3 8 442.54 23.11 2.67 0.014 0.91 -17 9 7 2159.82 125.80 2.67 0.033 0.79 -12 10 5 970.22 3.65 2.64 0.006 0.79 9 5 8 263.36 989.63 2.63 0.093 0.95 -32 0 12 929.48 57.39 2.63 0.022 0.81 -17 5 10 645.01 109.94 2.63 0.031 0.94 3 3 0 1426.89 765.15 2.61 0.082 2.73 -3 9 5 1750.29 0.22 2.60 0.001 0.88 11 1 0 6405.41 8098.82 2.58 0.265 2.61 11 7 4 904.02 181.08 2.58 0.040 0.98 0 6 9 610.81 36.27 2.56 0.018 0.92 -21 5 9 451.74 5.20 2.56 0.007 0.95 35 1 2 1136.60 29.99 2.56 0.016 0.81 13 1 2 1893.04 1148.95 2.55 0.100 1.86 Bond lengths and angles C1 - Distance Angles O1 1.4539 (0.0092) C2 1.5327 (0.0107) 110.47 (0.71) C1 - O1 C2 - Distance Angles C3_$1 1.5139 (0.0108) C3 1.5139 (0.0108) 111.74 (1.12) C1_$1 1.5327 (0.0107) 109.68 (0.48) 109.04 (0.44) C1 1.5327 (0.0107) 109.04 (0.44) 109.68 (0.47) 107.57 (1.00) C2 - C3_$1 C3 C1_$1 C3 - Distance Angles O2 1.4426 (0.0092) C2 1.5139 (0.0108) 110.51 (0.59) C3 - O2 C4 - Distance Angles O3 1.3787 (0.0149) C5 1.4828 (0.0151) 113.31 (1.18) C4 - O3 C5 - Distance Angles C4 1.4828 (0.0151) C6 1.5142 (0.0163) 110.65 (1.00) C5 - C4 C6 - Distance Angles N4 1.3381 (0.0138) C5 1.5142 (0.0163) 115.68 (1.04) C6 - N4 N1 - Distance Angles P1 1.5678 (0.0069) P2 1.6004 (0.0075) 123.19 (0.46) N1 - P1 N2 - Distance Angles P3 1.5565 (0.0088) P2 1.5673 (0.0084) 124.80 (0.56) N2 - P3 N3 - Distance Angles P1 1.5666 (0.0088) P3 1.5812 (0.0091) 121.53 (0.47) N3 - P1 O3 - Distance Angles C4 1.3787 (0.0149) P2 1.5806 (0.0075) 120.16 (0.72) O3 - C4 O1 - Distance Angles C1 1.4539 (0.0092) P1 1.5796 (0.0063) 119.50 (0.47) O1 - C1 O2 - Distance Angles C3 1.4426 (0.0092) P1 1.5883 (0.0064) 118.39 (0.57) O2 - C3 N4 - Distance Angles C6 1.3381 (0.0138) P2 1.6241 (0.0071) 122.14 (0.72) N4 - C6 P1 - Distance Angles N3 1.5666 (0.0088) N1 1.5678 (0.0069) 117.88 (0.43) O1 1.5796 (0.0063) 109.57 (0.39) 108.39 (0.37) O2 1.5883 (0.0064) 110.51 (0.43) 106.53 (0.38) 102.87 (0.34) P1 - N3 N1 O1 P2 - Distance Angles N2 1.5673 (0.0084) O3 1.5806 (0.0075) 107.42 (0.52) N1 1.6004 (0.0075) 114.37 (0.42) 109.34 (0.44) N4 1.6241 (0.0071) 110.86 (0.52) 103.44 (0.38) 110.78 (0.42) P2 - N2 O3 N1 P3 - Distance Angles N5_b 1.4795 (0.0141) N2 1.5565 (0.0088) 117.02 (0.67) N3 1.5812 (0.0092) 96.04 (0.66) 117.35 (0.45) O4_b 1.6218 (0.0300) 112.26 (1.24) 110.29 (1.50) 102.42 (1.36) Cl2_a 2.0294 (0.0097) 102.32 (0.59) 107.98 (0.51) 115.02 (0.46) 14.59 (1.27) Cl1_a 2.1852 (0.0074) 21.14 (0.55) 102.65 (0.44) 117.10 (0.43) 106.69 (1.09) 93.64 (0.40) C7_b 2.3213 (0.0387) 34.36 (1.06) 104.86 (1.07) 127.58 (1.08) 89.75 (1.33) 76.27 (0.89) 17.64 (0.87) P3 - N5_b N2 N3 O4_b Cl2_a Cl1_a Cl1_a - Distance Angles P3 2.1852 (0.0074) Cl1_a - Cl2_a - Distance Angles P3 2.0294 (0.0096) Cl2_a - N5_b - Distance Angles C7_b 1.3811 (0.0341) P3 1.4795 (0.0140) 108.43 (2.01) N5_b - C7_b O4_b - Distance Angles C9_b 1.4995 (0.0311) P3 1.6218 (0.0298) 107.47 (2.49) O4_b - C9_b C7_b - Distance Angles N5_b 1.3811 (0.0339) C8_b 1.4325 (0.0343) 114.63 (2.83) P3 2.3213 (0.0386) 37.20 (1.23) 97.57 (2.24) C7_b - N5_b C8_b C8_b - Distance Angles C9_b 1.3989 (0.0305) C7_b 1.4325 (0.0343) 106.75 (2.67) C8_b - C9_b C9_b - Distance Angles C8_b 1.3989 (0.0305) O4_b 1.4995 (0.0311) 121.44 (2.57) C9_b - C8_b FMAP and GRID set by program FMAP 2 2 14 GRID -2.273 -2 -1 2.273 2 1 R1 = 0.2586 for 3392 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.4912 0.0021 0.6901 [ 2.69 A from H6B ] Deepest hole -0.35 at 0.1460 0.2261 0.0677 [ 0.56 A from H5 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3467 / 34226 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0088 1.5021 0.8099 1.00000 0.05 0.38 2.69 H6B 2.73 H1B 2.85 H1A 3.06 H6B Q2 1 0.1214 1.3214 0.7227 1.00000 0.05 0.37 0.90 N4 1.11 P2 1.53 C6 1.73 H4 Q3 1 0.0116 1.4387 0.4664 1.00000 0.05 0.37 2.82 H4A 2.88 H1A 2.89 H3B 3.01 N1 Q4 1 0.1678 1.5390 0.7037 1.00000 0.05 0.35 1.27 O3 1.29 C4 1.45 H4B 1.69 H5B Q5 1 0.1827 0.8974 0.6581 1.00000 0.05 0.34 0.72 N5 0.97 CL1 1.18 H5 1.53 C7 Q6 1 0.1386 1.0322 0.6742 1.00000 0.05 0.34 1.68 N2 1.99 P2 2.01 P3 2.28 N1 Q7 1 0.1603 1.4226 0.8797 1.00000 0.05 0.34 1.20 C6 1.25 H6A 1.44 H5B 1.56 C5 Q8 1 0.0817 1.1084 0.5525 1.00000 0.05 0.33 0.90 N1 1.05 P1 1.75 O1 2.18 P2 Q9 1 0.1567 1.1126 0.5808 1.00000 0.05 0.32 0.92 N2 0.93 P3 1.76 N3 1.84 P2 Q10 1 0.0033 0.4738 0.4046 1.00000 0.05 0.32 2.89 H1A 2.91 H3B 3.02 H4A 3.18 H1B Shortest distances between peaks (including symmetry equivalents) 3 10 0.74 1 10 1.20 1 1 1.31 6 9 1.56 3 3 1.63 1 3 1.87 5 6 1.88 3 10 1.88 6 8 2.00 2 7 2.02 5 9 2.08 8 9 2.32 10 10 2.35 4 7 2.37 1 10 2.40 2 4 2.43 2 6 2.63 2 8 2.67 2 9 2.91 1 3 2.95 Time profile in seconds ----------------------- 0.03: 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 0.00: Analyse other restraints etc. 0.95: Read intensity data, sort/merge etc. 0.01: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.41: Structure factors and derivatives 1.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0008 finished at 18:23:16 Total CPU time: 4.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++