+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src1026sq started at 11:35:19 on 02-Mar-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src1026t in P4(2)/mbc CELL 0.71073 22.0599 22.0599 19.5369 90.000 90.000 90.000 ZERR 4.00 0.0026 0.0026 0.0030 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, Z SYMM - Y, X, 1/2 + Z SYMM Y, - X, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM 1/2 + Y, 1/2 + X, 1/2 - Z SYMM 1/2 - Y, 1/2 - X, 1/2 - Z SFAC C H N O CL MN UNIT 232 200 104 64 16 12 V = 9507.42 F(000) = 3404.0 Mu = 0.57 mm-1 Cell Wt = 6695.44 Rho = 1.169 MERG 2 OMIT -3.00 55.00 OMIT 0 6 0 OMIT 1 5 0 delu simu SHEL 7 0.77 EQIV $1 X, Y, -Z DFIX 31 CL21 O21 CL21 O22 CL21 O23 DANG 31.6333 O21 O22 O21 O23 O21 O21_$1 O22 O23 O22 O21_$1 O23 O21_$1 DFIX 31 CL31 O31 CL31 O32 CL31 O33 DANG 31.6333 O31 O32 O31 O33 O31 O31_$1 O32 O33 O32 O31_$1 O33 O31_$1 DFIX 31 CL36 O36 CL36 O37 CL36 O38 DANG 31.6333 O36 O37 O36 O38 O36 O36_$1 O37 O38 O37 O36_$1 O38 O36_$1 FMAP 2 PLAN 10 ACTA size 0.22 0.2 0.11 BOND $H WGHT 0.15550 7.02540 L.S. 40 TEMP -153.00 FVAR 1.71668 0.71992 1.41716 MOLE 1 C1 1 0.199649 0.249909 0.156006 11.00000 0.17783 0.14273 = 0.04846 0.01331 0.01443 0.11671 AFIX 43 H1 2 0.215460 0.283264 0.130960 11.00000 -1.20000 AFIX 0 C2 1 0.218432 0.195013 0.137729 11.00000 0.27237 0.17977 = 0.06163 -0.00863 0.00339 0.17336 AFIX 43 H2 2 0.247537 0.189274 0.102480 11.00000 -1.20000 AFIX 0 C3 1 0.192810 0.145696 0.173510 11.00000 0.30662 0.14275 = 0.08522 -0.02383 -0.01455 0.16664 AFIX 43 H3 2 0.204296 0.105608 0.161367 11.00000 -1.20000 AFIX 0 C4 1 0.150304 0.154446 0.227194 11.00000 0.27053 0.09914 = 0.07826 -0.01043 -0.02474 0.11699 AFIX 43 H4 2 0.131875 0.121818 0.251158 11.00000 -1.20000 AFIX 0 C5 1 0.137687 0.216505 0.242006 11.00000 0.17978 0.09010 = 0.04125 -0.00470 -0.00847 0.08014 C6 1 0.093388 0.231959 0.298160 11.00000 0.13997 0.05964 = 0.04708 0.00512 -0.01291 0.04620 C7 1 0.062835 0.190308 0.337194 11.00000 0.16293 0.04863 = 0.07213 0.00722 -0.01987 0.02575 AFIX 43 H7 2 0.067768 0.148074 0.329490 11.00000 -1.20000 AFIX 0 C8 1 0.024570 0.211397 0.388178 11.00000 0.11918 0.06110 = 0.07088 0.01906 -0.01333 -0.00225 AFIX 43 H8 2 0.002688 0.183640 0.415957 11.00000 -1.20000 AFIX 0 C9 1 0.018615 0.271772 0.398088 11.00000 0.08310 0.05659 = 0.04850 0.01369 -0.00095 0.00092 AFIX 43 H9 2 -0.007178 0.286857 0.433104 11.00000 -1.20000 AFIX 0 C10 1 0.050339 0.311023 0.356877 11.00000 0.06954 0.05170 = 0.03286 0.00712 -0.00001 0.01556 C11 1 0.047467 0.378185 0.361345 11.00000 0.05408 0.05266 = 0.02565 0.00936 -0.00233 0.00617 C12 1 0.126954 0.501982 0.316365 11.00000 0.04322 0.06995 = 0.03135 0.00829 0.00255 0.00635 C13 1 0.123043 0.562020 0.284389 11.00000 0.04302 0.06255 = 0.03571 0.00930 -0.00405 -0.00824 C14 1 0.166994 0.605247 0.286467 11.00000 0.06240 0.08966 = 0.08233 0.01696 -0.02348 -0.01971 AFIX 43 H14 2 0.202953 0.599266 0.312357 11.00000 -1.20000 AFIX 0 C15 1 0.157934 0.657934 0.250000 10.50000 0.07627 0.07627 = 0.11759 0.02068 -0.02068 -0.03670 AFIX 43 H15 2 0.188386 0.688385 0.250000 10.50000 -1.20000 AFIX 0 N1 3 0.160026 0.262802 0.207055 11.00000 0.16026 0.10108 = 0.03631 0.00887 0.00741 0.08355 N2 3 0.087659 0.291026 0.308699 11.00000 0.10020 0.05610 = 0.03584 0.01054 -0.00033 0.03024 N3 3 0.003394 0.403706 0.397580 11.00000 0.06740 0.04779 = 0.03792 0.00519 0.01326 0.00627 AFIX 93 H3A 2 0.000282 0.443446 0.399314 11.00000 -1.20000 H3B 2 -0.022700 0.380878 0.419858 11.00000 -1.20000 AFIX 0 N4 3 0.088468 0.406816 0.326498 11.00000 0.05415 0.05292 = 0.03503 0.01135 0.00673 0.01040 N5 3 0.077533 0.468960 0.316447 11.00000 0.04305 0.05030 = 0.02990 0.00697 0.00096 0.00452 N6 3 0.180404 0.481283 0.338363 11.00000 0.04243 0.09363 = 0.04676 0.02412 -0.00550 -0.00228 AFIX 93 H6A 2 0.183549 0.443940 0.353802 11.00000 -1.20000 H6B 2 0.212478 0.504986 0.337420 11.00000 -1.20000 AFIX 0 N7 3 0.071108 0.571108 0.250000 10.50000 0.04799 0.04799 = 0.03069 0.00137 -0.00137 -0.00322 MN1 6 0.144121 0.355879 0.250000 10.50000 0.08033 0.08033 = 0.03683 0.01768 0.01768 0.04362 MN2 6 0.000000 0.500000 0.250000 10.25000 0.04031 0.04031 = 0.03059 0.00000 0.00000 0.00240 MOLE 2 O21 4 0.115144 0.309521 0.058984 11.00000 0.11193 0.12220 = 0.04595 0.01316 0.02303 0.03976 O22 4 0.204199 0.300371 0.000000 10.50000 0.09349 0.37045 = 0.06565 0.00000 0.00000 0.09911 O23 4 0.149641 0.393479 0.000000 10.50000 0.37338 0.10879 = 0.09280 0.00000 0.00000 -0.06040 CL21 5 0.146313 0.328451 0.000000 10.50000 0.09628 0.10213 = 0.03289 0.00000 0.00000 0.01201 MOLE 3 PART 1 O31 4 0.847282 0.387960 0.059513 21.00000 0.08471 0.09850 = 0.06066 -0.02158 -0.00853 -0.01328 O32 4 0.816182 0.305112 0.000000 20.50000 0.09540 0.04881 = 0.15712 0.00000 0.00000 -0.01827 O33 4 0.757195 0.396934 0.000000 20.50000 0.05101 0.07388 = 0.07115 0.00000 0.00000 -0.01635 CL31 5 0.817163 0.370457 0.000000 20.50000 0.05485 0.05497 = 0.05088 0.00000 0.00000 -0.02525 PART 2 SAME O31 > CL31 O36 4 0.891829 0.339825 0.055799 -21.00000 0.31261 0.19751 = 0.26802 0.08058 -0.19278 -0.03229 O37 4 0.803323 0.318767 0.000000 -20.50000 0.12438 0.09582 = 0.24356 0.00000 0.00000 -0.05285 O38 4 0.843698 0.419820 0.000000 -20.50000 0.14985 0.07079 = 0.10670 0.00000 0.00000 -0.02154 CL36 5 0.855492 0.356551 0.000000 -20.50000 0.05730 0.06795 = 0.06327 0.00000 0.00000 -0.01219 HKLF 4 Covalent radii and connectivity table for 04src1026t in P4(2)/mbc C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 MN 1.370 C1 - C2 N1 C2 - C1 C3 C3 - C2 C4 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C6 C8 C8 - C9 C7 C9 - C8 C10 C10 - N2 C9 C11 C11 - N4 N3 C10 C12 - N5 N6 C13 C13 - N7 C14 C12 C14 - C13 C15 C15 - C14_$2 C14 N1 - C5 C1 Mn1 N2 - C6 C10 Mn1 N3 - C11 N4 - C11 N5 Mn1 N5 - C12 N4 Mn2 N6 - C12 N7 - C13 C13_$2 Mn2 Mn1 - N2_$3 N2 N4_$3 N4 N1 N1_$3 Mn2 - N7 N7_$4 N5_$2 N5 N5_$4 N5_$3 O21 - Cl21 O22 - Cl21 O23 - Cl21 Cl21 - O21_$1 O21 O22 O23 O31_a - Cl31_a O32_a - Cl31_a O33_a - Cl31_a Cl31_a - O31_a O31_$1a O32_a O33_a O36_b - Cl36_b O37_b - Cl36_b O38_b - Cl36_b Cl36_b - O36_b O36_$1b O38_b O37_b Operators for generating equivalent atoms: $1 x, y, -z $2 y-1/2, x+1/2, -z+1/2 $3 -y+1/2, -x+1/2, -z+1/2 $4 -x, -y+1, z 61776 Reflections read, of which 313 rejected -28 =< h =< 28, -27 =< k =< 28, -16 =< l =< 25, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 4 0 21111.85 39.17 10 198.30 1 8 0 15248.20 45.98 15 940.72 5 10 0 2401.61 61.37 9 317.89 12 13 0 1291.98 94.62 8 519.42 1 5 1 18922.53 38.03 28 345.74 3 7 1 8977.27 23.43 27 233.18 7 8 1 4189.03 24.75 20 131.44 13 14 1 381.68 102.64 8 1099.88 4 7 2 4253.87 39.26 24 228.64 0 2 3 31946.52 157.57 10 1582.94 1 3 3 128547.72 113.94 29 853.80 4 12 4 3600.84 39.16 18 195.93 4 13 4 1177.58 77.09 18 487.50 9 20 4 231.56 152.64 8 802.37 4 13 5 7288.35 70.75 18 617.12 8 18 5 114.11 131.19 8 1708.74 8 20 5 304.54 154.12 7 1505.01 5 7 6 1312.43 49.98 12 503.47 9 16 8 393.57 186.07 6 7074.40 5 9 9 130.46 84.73 9 2604.91 4 8 10 631.46 72.34 10 1267.70 9 13 12 132.86 182.67 6 2543.13 2 25 12 604.30 381.19 4 3087.75 7 9 15 454.35 265.30 6 4165.35 1 4 18 350.94 146.39 9 3287.10 25 Inconsistent equivalents 5614 Unique reflections, of which 0 suppressed R(int) = 0.0743 R(sigma) = 0.0544 Friedel opposites merged Maximum memory for data reduction = 3583 / 60224 Special position constraints for C15 z = 0.2500 y = 1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N7 z = 0.2500 y = 1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Mn1 z = 0.2500 y = -1.0 * x + 0.5000 U22 = 1.0 * U11 U13 = 1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Mn2 x = 0.0000 y = 0.5000 z = 0.2500 U22 = 1.0 * U11 U23 = 0 U13 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for O22 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O23 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl21 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O32_a z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O33_a z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl31_a z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O37_b z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O38_b z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl36_b z = 0.0000 U23 = 0 U13 = 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 = 4369 / 353710 wR2 = 0.2819 before cycle 1 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 2.1803 2.3146 -0.1344 0.0400 DANG O36_b O36_$1b 0.2683 0.0800 SIMU U22 O22 Cl21 0.2771 0.0800 SIMU U11 O23 Cl21 0.2553 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.017 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.052; Restrained GooF = 1.038 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71647 0.00738 -0.029 OSF 2 0.71994 0.00771 0.002 FVAR 2 3 1.41710 0.00549 -0.012 FVAR 3 Mean shift/esd = 0.010 Maximum = 0.042 for y O21 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 2 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 2.1797 2.3145 -0.1348 0.0400 DANG O36_b O36_$1b 0.2687 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2557 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.017 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.052; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71644 0.00738 -0.004 OSF 2 0.71994 0.00771 0.000 FVAR 2 3 1.41707 0.00549 -0.005 FVAR 3 Mean shift/esd = 0.005 Maximum = 0.019 for y O21 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 3 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 2.1795 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2557 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71645 0.00738 0.002 OSF 2 0.71993 0.00771 -0.001 FVAR 2 3 1.41706 0.00549 -0.001 FVAR 3 Mean shift/esd = 0.001 Maximum = 0.005 for x O23 Max. shift = 0.000 A for O23 Max. dU = 0.000 for O37_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 4 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 2.1795 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.052; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.002 OSF 2 0.71992 0.00771 -0.001 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.002 for x O23 Max. shift = 0.000 A for O23 Max. dU = 0.000 for O36_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 5 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 2.1795 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for x O23 Max. shift = 0.000 A for O23 Max. dU = 0.000 for O36_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 6 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x O23 Max. shift = 0.000 A for O23 Max. dU = 0.000 for O36_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 7 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x O23 Max. shift = 0.000 A for O23 Max. dU = 0.000 for O36_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 8 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71647 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for Cl36_b Max. dU = 0.000 for O36_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 9 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71647 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 10 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for Cl36_b Max. dU = 0.000 for O36_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 11 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N2 Max. dU = 0.000 for O38_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 12 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O36_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 13 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O38_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 14 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 15 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O36_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 16 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O36_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 17 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 18 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O36_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 19 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 20 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for C1 Max. dU = 0.000 for O37_b Least-squares cycle 21 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 21 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O38_b Least-squares cycle 22 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 22 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 22 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O31_a Max. dU = 0.000 for O37_b Least-squares cycle 23 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 23 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 23 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O36_b Least-squares cycle 24 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 24 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 24 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 25 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 25 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 25 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O36_b Least-squares cycle 26 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 26 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 26 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 27 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 27 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 27 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 27 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for C8 Max. dU = 0.000 for O36_b Least-squares cycle 28 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 28 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 28 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 28 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O36_b Least-squares cycle 29 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 29 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 29 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 29 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for C3 Max. dU = 0.000 for O36_b Least-squares cycle 30 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 30 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 30 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 30 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O36_b Max. dU = 0.000 for O36_b Least-squares cycle 31 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 31 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 31 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 31 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O37_b Least-squares cycle 32 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 32 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 32 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 32 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for O36_b Least-squares cycle 33 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 33 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 33 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 33 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O36_b Least-squares cycle 34 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 34 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 34 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 34 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for O36_b Least-squares cycle 35 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 35 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 35 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 35 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O36_b Least-squares cycle 36 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 36 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 36 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 36 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for H4 Max. dU = 0.000 for O36_b Least-squares cycle 37 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 37 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 37 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 37 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O37_b Least-squares cycle 38 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 38 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 38 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 38 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for O37_b Least-squares cycle 39 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 39 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 39 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 39 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for x Mn1 Max. shift = 0.000 A for O22 Max. dU = 0.000 for O37_b Least-squares cycle 40 Maximum vector length = 511 Memory required = 4369 / 353710 wR2 = 0.2819 before cycle 40 for 5614 data and 282 / 282 parameters Disagreeable restraints before cycle 40 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 40 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.71646 0.00738 0.000 OSF 2 0.71992 0.00771 0.000 FVAR 2 3 1.41706 0.00549 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.000 for y C12 Max. shift = 0.000 A for O37_b Max. dU = 0.000 for O37_b Largest correlation matrix elements -0.747 U12 O37_b / U11 O37_b -0.673 U11 Cl36_b / FVAR 2 -0.611 U12 O37_b / U22 O37_b 0.747 x Cl36_b / x Cl31_a 0.647 y C2 / x C2 0.610 U12 C1 / U11 C1 -0.714 y O37_b / x O37_b 0.639 x Cl36_b / U11 Cl31_a 0.608 x Cl31_a / FVAR 2 -0.696 U13 O36_b / U11 O36_b 0.638 U12 C2 / U22 C2 0.602 y C3 / x C3 0.690 U12 C3 / U11 C3 -0.626 U11 Cl36_b / x Cl31_a 0.601 U22 O37_b / y O32_a 0.689 U12 C2 / U11 C2 -0.618 U12 O36_b / U23 O36_b 0.598 U12 C4 / U11 C4 -0.684 U13 O36_b / U33 O36_b 0.616 x Cl36_b / FVAR 2 0.596 U12 O37_b / x O32_a 0.674 U11 Cl31_a / FVAR 2 0.614 y C4 / x C4 0.593 U12 O22 / U22 O22 Idealized hydrogen atom generation before cycle 41 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2155 0.2833 0.1310 43 0.950 0.000 C1 C2 N1 H2 0.2475 0.1892 0.1025 43 0.950 0.000 C2 C1 C3 H3 0.2043 0.1056 0.1614 43 0.950 0.000 C3 C2 C4 H4 0.1318 0.1218 0.2511 43 0.950 0.000 C4 C3 C5 H7 0.0678 0.1481 0.3295 43 0.950 0.000 C7 C6 C8 H8 0.0027 0.1837 0.4160 43 0.950 0.000 C8 C9 C7 H9 -0.0072 0.2869 0.4331 43 0.950 0.000 C9 C8 C10 H14 0.2029 0.5993 0.3124 43 0.950 0.000 C14 C13 C15 H15 0.1884 0.6884 0.2500 43 0.950 0.000 C15 C14_$2 C14 H3A 0.0003 0.4434 0.3993 93 0.880 0.000 N3 C11 N4 H3B -0.0227 0.3809 0.4199 93 0.880 0.000 N3 C11 N4 H6A 0.1835 0.4439 0.3538 93 0.880 0.000 N6 C12 N5 H6B 0.2125 0.5050 0.3374 93 0.880 0.000 N6 C12 N5 04src1026t in P4(2)/mbc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.19965 0.24990 0.15601 1.00000 0.17783 0.14274 0.04849 0.01341 0.01454 0.11675 0.12302 0.01632 0.00039 0.00038 0.00029 0.00000 0.00658 0.00511 0.00303 0.00352 0.00373 0.00498 0.00275 H1 0.21546 0.28326 0.13096 1.00000 0.14762 0.00000 0.00000 C2 0.21843 0.19499 0.13773 1.00000 0.27254 0.17975 0.06161 -0.00859 0.00352 0.17338 0.17130 0.02115 0.00054 0.00050 0.00039 0.00000 0.01079 0.00704 0.00415 0.00457 0.00518 0.00751 0.00432 H2 0.24754 0.18924 0.10248 1.00000 0.20556 0.00000 0.00000 C3 0.19281 0.14569 0.17350 1.00000 0.30693 0.14276 0.08515 -0.02370 -0.01446 0.16678 0.17828 0.02005 0.00057 0.00045 0.00044 0.00000 0.01203 0.00565 0.00533 0.00464 0.00596 0.00691 0.00433 H3 0.20430 0.10561 0.16136 1.00000 0.21394 0.00000 0.00000 C4 0.15029 0.15444 0.22719 1.00000 0.27054 0.09910 0.07821 -0.01030 -0.02469 0.11698 0.14928 0.01818 0.00052 0.00037 0.00039 0.00000 0.01019 0.00436 0.00437 0.00393 0.00521 0.00563 0.00356 H4 0.13184 0.12182 0.25114 1.00000 0.17914 0.00000 0.00000 C5 0.13769 0.21650 0.24201 1.00000 0.17958 0.09019 0.04123 -0.00466 -0.00843 0.08012 0.10367 0.01361 0.00038 0.00031 0.00027 0.00000 0.00659 0.00368 0.00283 0.00263 0.00300 0.00409 0.00235 C6 0.09339 0.23197 0.29817 1.00000 0.13995 0.05958 0.04712 0.00508 -0.01290 0.04615 0.08222 0.01120 0.00031 0.00024 0.00027 0.00000 0.00500 0.00283 0.00260 0.00224 0.00271 0.00294 0.00167 C7 0.06284 0.19031 0.33720 1.00000 0.16282 0.04871 0.07223 0.00739 -0.01972 0.02580 0.09459 0.01190 0.00036 0.00026 0.00033 0.00000 0.00610 0.00291 0.00363 0.00267 0.00353 0.00321 0.00193 H7 0.06777 0.14808 0.32950 1.00000 0.11350 0.00000 0.00000 C8 0.02456 0.21141 0.38819 1.00000 0.11926 0.06106 0.07082 0.01902 -0.01330 -0.00229 0.08371 0.01056 0.00031 0.00025 0.00031 0.00000 0.00480 0.00305 0.00351 0.00285 0.00321 0.00307 0.00165 H8 0.00268 0.18365 0.41597 1.00000 0.10046 0.00000 0.00000 C9 0.01861 0.27177 0.39810 1.00000 0.08305 0.05653 0.04848 0.01366 -0.00096 0.00095 0.06268 0.00861 0.00024 0.00021 0.00025 0.00000 0.00334 0.00260 0.00253 0.00218 0.00237 0.00234 0.00124 H9 -0.00718 0.28686 0.43312 1.00000 0.07522 0.00000 0.00000 C10 0.05034 0.31103 0.35687 1.00000 0.06955 0.05164 0.03284 0.00708 0.00001 0.01558 0.05134 0.00794 0.00021 0.00020 0.00021 0.00000 0.00280 0.00229 0.00195 0.00180 0.00194 0.00204 0.00104 C11 0.04746 0.37818 0.36134 1.00000 0.05407 0.05267 0.02562 0.00935 -0.00231 0.00615 0.04412 0.00713 0.00019 0.00019 0.00019 0.00000 0.00234 0.00222 0.00172 0.00170 0.00171 0.00187 0.00092 C12 0.12696 0.50199 0.31636 1.00000 0.04323 0.06995 0.03133 0.00828 0.00252 0.00636 0.04817 0.00788 0.00019 0.00021 0.00020 0.00000 0.00211 0.00256 0.00192 0.00193 0.00174 0.00189 0.00097 C13 0.12305 0.56202 0.28439 1.00000 0.04301 0.06249 0.03567 0.00930 -0.00406 -0.00824 0.04706 0.00705 0.00018 0.00020 0.00020 0.00000 0.00217 0.00247 0.00207 0.00193 0.00180 0.00184 0.00097 C14 0.16699 0.60524 0.28647 1.00000 0.06234 0.08969 0.08232 0.01692 -0.02347 -0.01970 0.07812 0.00942 0.00024 0.00027 0.00031 0.00000 0.00305 0.00375 0.00397 0.00321 0.00293 0.00276 0.00163 H14 0.20295 0.59927 0.31237 1.00000 0.09374 0.00000 0.00000 C15 0.15792 0.65792 0.25000 0.50000 0.07623 0.07623 0.11756 0.02070 -0.02070 -0.03665 0.09001 0.01108 0.00025 0.00025 0.00000 0.00000 0.00341 0.00341 0.00800 0.00384 0.00384 0.00426 0.00289 H15 0.18838 0.68838 0.25000 0.50000 0.10801 0.00000 0.00000 N1 0.16003 0.26281 0.20706 1.00000 0.16027 0.10107 0.03633 0.00892 0.00743 0.08356 0.09922 0.01059 0.00027 0.00024 0.00022 0.00000 0.00493 0.00332 0.00210 0.00228 0.00251 0.00346 0.00190 N2 0.08766 0.29103 0.30870 1.00000 0.10024 0.05608 0.03581 0.01054 -0.00033 0.03028 0.06404 0.00771 0.00021 0.00017 0.00018 0.00000 0.00306 0.00213 0.00188 0.00168 0.00192 0.00203 0.00109 N3 0.00339 0.40371 0.39758 1.00000 0.06743 0.04777 0.03790 0.00517 0.01324 0.00627 0.05103 0.00628 0.00016 0.00015 0.00017 0.00000 0.00226 0.00192 0.00180 0.00159 0.00170 0.00166 0.00089 H3A 0.00028 0.44345 0.39932 1.00000 0.06124 0.00000 0.00000 H3B -0.02271 0.38088 0.41986 1.00000 0.06124 0.00000 0.00000 N4 0.08847 0.40681 0.32650 1.00000 0.05413 0.05289 0.03506 0.01135 0.00674 0.01039 0.04736 0.00635 0.00016 0.00015 0.00018 0.00000 0.00202 0.00194 0.00171 0.00152 0.00153 0.00155 0.00083 N5 0.07753 0.46896 0.31644 1.00000 0.04305 0.05029 0.02994 0.00697 0.00092 0.00450 0.04109 0.00567 0.00015 0.00015 0.00015 0.00000 0.00180 0.00190 0.00156 0.00146 0.00138 0.00147 0.00075 N6 0.18041 0.48128 0.33836 1.00000 0.04238 0.09363 0.04672 0.02407 -0.00547 -0.00233 0.06091 0.00699 0.00016 0.00020 0.00019 0.00000 0.00194 0.00294 0.00208 0.00204 0.00172 0.00191 0.00105 H6A 0.18355 0.44394 0.35380 1.00000 0.07309 0.00000 0.00000 H6B 0.21248 0.50498 0.33742 1.00000 0.07309 0.00000 0.00000 N7 0.07110 0.57110 0.25000 0.50000 0.04796 0.04796 0.03073 0.00136 -0.00136 -0.00325 0.04222 0.00644 0.00015 0.00015 0.00000 0.00000 0.00159 0.00159 0.00227 0.00141 0.00141 0.00203 0.00107 Mn1 0.14412 0.35588 0.25000 0.50000 0.08032 0.08032 0.03681 0.01767 0.01767 0.04360 0.06582 0.00000 0.00003 0.00003 0.00000 0.00000 0.00057 0.00057 0.00054 0.00039 0.00039 0.00058 0.00042 Mn2 0.00000 0.50000 0.25000 0.25000 0.04031 0.04031 0.03058 0.00000 0.00000 0.00242 0.03706 0.00000 0.00000 0.00000 0.00000 0.00000 0.00043 0.00043 0.00059 0.00000 0.00000 0.00047 0.00033 O21 0.11515 0.30953 0.05898 1.00000 0.11201 0.12210 0.04589 0.01314 0.02310 0.03976 0.09334 0.00837 0.00020 0.00020 0.00018 0.00000 0.00307 0.00322 0.00199 0.00212 0.00204 0.00263 0.00133 O22 0.20420 0.30038 0.00000 0.50000 0.09330 0.37094 0.06560 0.00000 0.00000 0.09908 0.17661 0.01662 0.00032 0.00057 0.00000 0.00000 0.00480 0.01287 0.00421 0.00000 0.00000 0.00726 0.00459 O23 0.14967 0.39348 0.00000 0.50000 0.37370 0.10900 0.09284 0.00000 0.00000 -0.06072 0.19184 0.01444 0.00063 0.00038 0.00000 0.00000 0.01548 0.00512 0.00586 0.00000 0.00000 0.00624 0.00468 Cl21 0.14632 0.32845 0.00000 0.50000 0.09628 0.10210 0.03289 0.00000 0.00000 0.01200 0.07709 0.00343 0.00010 0.00011 0.00000 0.00000 0.00147 0.00155 0.00082 0.00000 0.00000 0.00112 0.00062 O31_a 0.84728 0.38795 0.05951 0.71992 0.08471 0.09847 0.06064 -0.02161 -0.00848 -0.01335 0.08127 0.00819 0.00024 0.00029 0.00027 0.00771 0.00364 0.00437 0.00334 0.00316 0.00270 0.00297 0.00189 O32_a 0.81620 0.30512 0.00000 0.35996 0.09535 0.04875 0.15696 0.00000 0.00000 -0.01822 0.10035 0.01212 0.00056 0.00040 0.00000 0.00385 0.00638 0.00405 0.01002 0.00000 0.00000 0.00400 0.00366 O33_a 0.75719 0.39694 0.00000 0.35996 0.05096 0.07384 0.07120 0.00000 0.00000 -0.01630 0.06533 0.00821 0.00026 0.00029 0.00000 0.00385 0.00338 0.00426 0.00442 0.00000 0.00000 0.00294 0.00194 Cl31_a 0.81716 0.37046 0.00000 0.35996 0.05484 0.05498 0.05088 0.00000 0.00000 -0.02524 0.05357 0.00338 0.00017 0.00012 0.00000 0.00385 0.00199 0.00157 0.00129 0.00000 0.00000 0.00128 0.00093 O36_b 0.89181 0.33980 0.05578 0.28008 0.31312 0.19788 0.26855 0.08092 -0.19300 -0.03219 0.25985 0.03609 0.00113 0.00111 0.00090 0.00771 0.02931 0.02175 0.02801 0.02171 0.02356 0.02154 0.01558 O37_b 0.80330 0.31879 0.00000 0.14004 0.12456 0.09561 0.24433 0.00000 0.00000 -0.05278 0.15483 0.02112 0.00121 0.00131 0.00000 0.00385 0.02088 0.01908 0.03395 0.00000 0.00000 0.01862 0.01467 O38_b 0.84371 0.41983 0.00000 0.14004 0.15055 0.07076 0.10585 0.00000 0.00000 -0.02184 0.10905 0.02918 0.00110 0.00059 0.00000 0.00385 0.02025 0.00855 0.01867 0.00000 0.00000 0.01069 0.00789 Cl36_b 0.85548 0.35655 0.00000 0.14004 0.05734 0.06792 0.06332 0.00000 0.00000 -0.01217 0.06286 0.01061 0.00048 0.00033 0.00000 0.00385 0.00542 0.00403 0.00406 0.00000 0.00000 0.00345 0.00232 Final Structure Factor Calculation for 04src1026t in P4(2)/mbc Total number of l.s. parameters = 282 Maximum vector length = 511 Memory required = 4087 / 25039 wR2 = 0.2819 before cycle 41 for 5614 data and 0 / 282 parameters Disagreeable restraints before cycle 41 Observed Target Error Sigma Restraint 2.1794 2.3145 -0.1350 0.0400 DANG O36_b O36_$1b 0.2688 0.0800 SIMU U22 O22 Cl21 0.2774 0.0800 SIMU U11 O23 Cl21 0.2558 0.0800 SIMU U11 O36_b Cl36_b Summary of restraints applied in cycle 41 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 9. 18. 6. 0. 0. 0. 89. 240. 0. 0. rms sigma 0.000 0.020 0.040 0.032 0.000 0.000 0.000 0.010 0.061 0.000 0.000 rms deviation 0.000 0.018 0.051 0.017 0.000 0.000 0.000 0.007 0.054 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.037 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1555 * P )^2 + 7.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0871 for 3455 Fo > 4sig(Fo) and 0.1472 for all 5614 data wR2 = 0.2819, GooF = S = 1.051, Restrained GooF = 1.037 for all data Occupancy sum of asymmetric unit = 26.75 for non-hydrogen and 12.50 for hydrogen atoms Principal mean square atomic displacements U 0.2800 0.0469 0.0421 C1 may be split into 0.2079 0.2570 0.1571 and 0.1914 0.2428 0.1550 0.4056 0.0658 0.0425 C2 may be split into 0.2289 0.2030 0.1376 and 0.2080 0.1869 0.1378 0.4126 0.0865 0.0357 C3 may be split into 0.2038 0.1525 0.1724 and 0.1819 0.1388 0.1746 0.3326 0.0755 0.0397 C4 may be split into 0.1605 0.1596 0.2258 and 0.1401 0.1493 0.2285 0.2271 0.0432 0.0407 C5 may be split into 0.1461 0.2214 0.2414 and 0.1293 0.2116 0.2426 0.1618 0.0531 0.0318 C6 0.1716 0.0732 0.0389 C7 0.1235 0.0819 0.0457 C8 0.0831 0.0667 0.0382 C9 0.0788 0.0455 0.0297 C10 0.0603 0.0499 0.0222 C11 0.0732 0.0418 0.0295 C12 0.0686 0.0400 0.0325 C13 0.1194 0.0697 0.0453 C14 0.1446 0.0859 0.0396 C15 0.2200 0.0432 0.0345 N1 may be split into 0.1678 0.2683 0.2077 and 0.1523 0.2573 0.2064 0.1159 0.0480 0.0283 N2 0.0747 0.0460 0.0324 N3 0.0688 0.0439 0.0294 N4 0.0543 0.0412 0.0278 N5 0.1041 0.0443 0.0344 N6 0.0514 0.0447 0.0306 N7 0.1306 0.0367 0.0302 Mn1 0.0427 0.0379 0.0306 Mn2 0.1626 0.0788 0.0386 O21 0.4027 0.0656 0.0616 O22 may be split into 0.2082 0.3129 0.0000 and 0.2002 0.2879 0.0000 0.3870 0.0957 0.0928 O23 may be split into 0.1616 0.3909 0.0000 and 0.1377 0.3961 0.0000 0.1115 0.0868 0.0329 Cl21 0.1114 0.0863 0.0461 O31_a 0.1570 0.1016 0.0425 O32_a 0.0823 0.0712 0.0425 O33_a 0.0801 0.0509 0.0297 Cl31_a 0.5051 0.1929 0.0815 O36_b may be split into 0.9008 0.3367 0.0463 and 0.8829 0.3429 0.0652 0.2443 0.1648 0.0554 O37_b 0.1561 0.1058 0.0652 O38_b 0.0759 0.0633 0.0494 Cl36_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.008 0.012 0.016 0.022 0.029 0.039 0.056 0.090 1.000 Number in group 601. 673. 552. 452. 576. 529. 550. 556. 567. 558. GooF 1.011 1.149 1.127 1.024 1.057 0.954 1.089 1.038 1.000 1.025 K 39.039 6.567 2.922 1.880 1.397 1.127 1.044 1.020 1.010 1.013 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.67 inf Number in group 565. 571. 554. 560. 559. 569. 556. 557. 562. 561. GooF 0.974 0.939 0.930 0.957 0.899 0.882 0.895 0.927 1.004 1.787 K 1.919 1.443 1.303 1.175 1.060 1.007 1.015 1.004 0.999 1.027 R1 0.458 0.359 0.306 0.263 0.174 0.127 0.105 0.082 0.063 0.085 Recommended weighting scheme: WGHT 0.1564 6.7747 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) 2 3 5 492.66 19.46 8.70 0.008 3.29 2 6 6 341.88 20.17 7.82 0.008 2.38 3 5 3 995.73 147.76 7.56 0.021 3.27 0 4 1 3015.59 299.27 7.05 0.030 5.31 4 4 2 948.58 179.71 6.60 0.023 3.62 2 6 0 726.07 3096.59 6.06 0.097 3.49 3 8 0 1215.04 418.06 5.87 0.036 2.58 1 3 1 1362.70 66.66 5.52 0.014 6.57 4 7 2 1443.82 533.03 5.24 0.040 2.63 2 5 3 263.42 21.37 5.13 0.008 3.47 2 2 6 2169.23 941.94 5.04 0.053 3.00 2 5 0 3911.93 1797.02 4.81 0.074 4.10 1 8 1 3871.86 1866.69 4.60 0.075 2.71 0 6 1 370.77 93.70 4.60 0.017 3.61 0 4 3 28046.03 14288.71 4.50 0.208 4.21 5 10 5 813.38 348.74 4.45 0.033 1.76 1 5 2 6780.08 3471.36 4.30 0.103 3.96 1 11 6 197.02 45.51 4.25 0.012 1.70 2 9 0 10273.71 5470.21 4.12 0.129 2.39 1 5 3 2004.74 1020.54 4.08 0.056 3.60 3 5 5 3788.64 2017.84 4.02 0.078 2.72 2 9 7 148.57 463.61 4.01 0.038 1.82 7 8 3 151.25 29.58 3.99 0.009 1.98 3 4 3 4624.75 2482.55 3.99 0.087 3.65 2 6 1 10310.55 5757.66 3.83 0.132 3.43 2 4 3 12749.01 7163.08 3.82 0.148 3.93 1 11 1 850.95 1865.81 3.79 0.075 1.99 4 5 3 6897.93 3852.93 3.74 0.108 3.05 7 8 2 152.28 422.75 3.66 0.036 2.03 4 8 1 215.84 546.85 3.64 0.041 2.45 1 5 9 1076.69 552.03 3.64 0.041 1.94 1 7 0 15236.08 28917.99 3.50 0.296 3.12 1 3 7 1383.00 2690.74 3.42 0.090 2.59 4 7 12 148.30 29.33 3.40 0.009 1.40 6 6 6 480.20 1016.37 3.39 0.056 2.03 1 9 6 1024.82 1998.31 3.32 0.078 1.95 8 11 2 357.37 145.09 3.27 0.021 1.60 1 1 4 41143.38 25288.96 3.22 0.277 4.66 3 7 1 3047.01 5531.84 3.20 0.130 2.87 3 3 2 37591.07 66549.85 3.18 0.450 4.59 1 5 10 1229.48 699.34 3.15 0.046 1.78 1 3 3 43630.84 27324.83 3.10 0.288 4.76 1 6 11 133.91 33.71 3.07 0.010 1.60 1 9 0 8050.00 5033.02 3.04 0.124 2.44 2 4 1 2643.30 1617.40 3.04 0.070 4.78 5 8 1 10.82 103.26 3.03 0.018 2.32 0 6 2 1677.17 1011.42 3.03 0.055 3.44 1 8 9 1029.84 609.92 2.93 0.043 1.70 3 23 10 155.96 469.87 2.91 0.038 0.86 5 14 12 411.87 195.76 2.91 0.024 1.10 Bond lengths and angles C1 - Distance Angles C2 1.3292 (0.0102) N1 1.3563 (0.0075) 126.13 (0.91) H1 0.9500 116.93 116.93 C1 - C2 N1 C2 - Distance Angles C1 1.3292 (0.0102) C3 1.4108 (0.0156) 116.40 (0.83) H2 0.9500 121.80 121.80 C2 - C1 C3 C3 - Distance Angles C2 1.4108 (0.0156) C4 1.4205 (0.0128) 121.71 (0.69) H3 0.9500 119.15 119.15 C3 - C2 C4 C4 - Distance Angles C3 1.4205 (0.0129) C5 1.4266 (0.0089) 114.13 (0.93) H4 0.9500 122.93 122.93 C4 - C3 C5 C5 - Distance Angles N1 1.3238 (0.0092) C4 1.4266 (0.0089) 124.29 (0.68) C6 1.5084 (0.0086) 116.22 (0.49) 119.39 (0.77) C5 - N1 C4 C6 - Distance Angles N2 1.3252 (0.0063) C7 1.3712 (0.0092) 121.71 (0.55) C5 1.5084 (0.0086) 113.40 (0.58) 124.85 (0.53) C6 - N2 C7 C7 - Distance Angles C6 1.3712 (0.0092) C8 1.3863 (0.0088) 118.30 (0.50) H7 0.9500 120.85 120.85 C7 - C6 C8 C8 - Distance Angles C9 1.3520 (0.0071) C7 1.3863 (0.0088) 119.52 (0.56) H8 0.9500 120.24 120.24 C8 - C9 C7 C9 - Distance Angles C8 1.3520 (0.0071) C10 1.3743 (0.0063) 119.16 (0.53) H9 0.9500 120.42 120.42 C9 - C8 C10 C10 - Distance Angles N2 1.3258 (0.0057) C9 1.3743 (0.0063) 121.51 (0.42) C11 1.4854 (0.0059) 113.58 (0.38) 124.90 (0.41) C10 - N2 C9 C11 - Distance Angles N4 1.2965 (0.0051) N3 1.3279 (0.0051) 125.76 (0.39) C10 1.4854 (0.0059) 115.16 (0.37) 119.04 (0.37) C11 - N4 N3 C12 - Distance Angles N5 1.3113 (0.0055) N6 1.3355 (0.0055) 122.93 (0.41) C13 1.4667 (0.0061) 116.95 (0.36) 119.86 (0.39) C12 - N5 N6 C13 - Distance Angles N7 1.3434 (0.0045) C14 1.3604 (0.0066) 121.21 (0.43) C12 1.4667 (0.0061) 113.45 (0.37) 125.32 (0.41) C13 - N7 C14 C14 - Distance Angles C13 1.3604 (0.0065) C15 1.3778 (0.0068) 118.19 (0.51) H14 0.9500 120.91 120.91 C14 - C13 C15 C15 - Distance Angles C14_$2 1.3778 (0.0068) C14 1.3778 (0.0068) 120.82 (0.71) H15 0.9500 119.59 119.59 C15 - C14_$2 C14 N1 - Distance Angles C5 1.3238 (0.0092) C1 1.3563 (0.0075) 117.21 (0.56) Mn1 2.2456 (0.0049) 117.04 (0.35) 124.56 (0.56) N1 - C5 C1 N2 - Distance Angles C6 1.3252 (0.0063) C10 1.3258 (0.0057) 119.78 (0.48) Mn1 2.2166 (0.0043) 120.04 (0.39) 120.10 (0.30) N2 - C6 C10 N3 - Distance Angles C11 1.3279 (0.0051) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.2965 (0.0051) N5 1.4058 (0.0046) 115.38 (0.33) Mn1 2.2367 (0.0035) 119.28 (0.28) 119.39 (0.23) N4 - C11 N5 N5 - Distance Angles C12 1.3113 (0.0055) N4 1.4058 (0.0046) 113.53 (0.33) Mn2 2.2537 (0.0031) 117.48 (0.26) 120.47 (0.24) N5 - C12 N4 N6 - Distance Angles C12 1.3355 (0.0055) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C13 1.3434 (0.0045) C13_$2 1.3434 (0.0045) 120.31 (0.49) Mn2 2.2182 (0.0046) 119.84 (0.24) 119.84 (0.24) N7 - C13 C13_$2 Mn1 - Distance Angles N2_$3 2.2166 (0.0043) N2 2.2166 (0.0043) 173.23 (0.20) N4_$3 2.2367 (0.0035) 70.74 (0.13) 114.69 (0.14) N4 2.2367 (0.0035) 114.69 (0.14) 70.74 (0.13) 83.98 (0.17) N1 2.2456 (0.0049) 102.69 (0.19) 72.00 (0.18) 109.31 (0.14) 142.63 (0.18) N1_$3 2.2456 (0.0049) 72.00 (0.18) 102.69 (0.19) 142.63 (0.18) 109.31 (0.14) 81.59 (0.29) Mn1 - N2_$3 N2 N4_$3 N4 N1 Mn2 - Distance Angles N7 2.2182 (0.0046) N7_$4 2.2182 (0.0046) 180.00 N5_$2 2.2537 (0.0031) 71.23 (0.08) 108.77 (0.08) N5 2.2537 (0.0031) 71.23 (0.08) 108.77 (0.08) 142.45 (0.17) N5_$4 2.2537 (0.0031) 108.77 (0.08) 71.23 (0.08) 82.56 (0.16) 109.67 (0.15) N5_$3 2.2537 (0.0031) 108.77 (0.08) 71.23 (0.08) 109.67 (0.15) 82.56 (0.16) 142.45 (0.17) Mn2 - N7 N7_$4 N5_$2 N5 N5_$4 O21 - Distance Angles Cl21 1.4052 (0.0038) O21 - O22 - Distance Angles Cl21 1.4191 (0.0070) O22 - O23 - Distance Angles Cl21 1.4365 (0.0085) O23 - Cl21 - Distance Angles O21_$1 1.4052 (0.0038) O21 1.4052 (0.0038) 110.18 (0.42) O22 1.4191 (0.0070) 108.10 (0.33) 108.10 (0.33) O23 1.4365 (0.0085) 108.77 (0.35) 108.77 (0.35) 112.91 (0.73) Cl21 - O21_$1 O21 O22 O31_a - Distance Angles Cl31_a 1.3936 (0.0050) O31_a - O32_a - Distance Angles Cl31_a 1.4415 (0.0090) O32_a - O33_a - Distance Angles Cl31_a 1.4462 (0.0071) O33_a - Cl31_a - Distance Angles O31_a 1.3936 (0.0050) O31_$1a 1.3936 (0.0050) 113.08 (0.50) O32_a 1.4415 (0.0090) 106.49 (0.41) 106.49 (0.41) O33_a 1.4462 (0.0071) 108.93 (0.31) 108.93 (0.31) 112.98 (0.59) Cl31_a - O31_a O31_$1a O32_a O36_b - Distance Angles Cl36_b 1.4023 (0.0115) O36_b - O37_b - Distance Angles Cl36_b 1.4208 (0.0134) O37_b - O38_b - Distance Angles Cl36_b 1.4199 (0.0125) O38_b - Cl36_b - Distance Angles O36_b 1.4023 (0.0115) O36_$1b 1.4023 (0.0115) 101.99 (2.21) O38_b 1.4199 (0.0125) 111.32 (1.06) 111.32 (1.06) O37_b 1.4208 (0.0134) 107.97 (1.15) 107.97 (1.15) 115.36 (1.67) Cl36_b - O36_b O36_$1b O38_b FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -1 1.190 2 1 R1 = 0.1446 for 5614 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.66 at 0.6000 0.1522 0.0000 [ 1.11 A from CL21 ] Deepest hole -0.55 at 0.6716 0.1800 0.0000 [ 0.59 A from CL21 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 4780 / 58638 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1000 0.3478 0.0000 0.50000 0.05 0.66 1.11 CL21 1.47 O21 1.49 O23 2.53 O22 Q2 1 0.8229 0.3381 0.0606 1.00000 0.05 0.47 1.23 O31 1.33 O37 1.39 CL31 1.40 O32 Q3 1 0.9612 0.3073 0.0189 1.00000 0.05 0.39 1.84 O36 2.23 O36 2.60 CL36 2.94 H6B Q4 1 0.0360 0.1944 0.3475 1.00000 0.05 0.37 0.63 C7 0.91 C8 1.29 H7 1.54 H8 Q5 1 0.0000 0.5000 0.5000 0.25000 0.05 0.34 2.33 H3A 2.92 N3 3.10 H3B 3.87 O38 Q6 1 0.8140 0.4035 0.0327 1.00000 0.05 0.32 0.97 O31 0.97 CL31 0.98 O38 1.41 O33 Q7 1 0.2077 0.2807 0.0000 0.50000 0.05 0.32 0.44 O22 1.72 CL21 2.43 O21 2.56 H1 Q8 1 0.1391 0.3250 0.2633 1.00000 0.05 0.31 0.74 MN1 1.62 N2 1.82 N1 2.26 N1 Q9 1 0.9059 0.3477 0.0000 0.50000 0.05 0.29 1.13 CL36 1.15 O36 1.95 O31 2.02 CL31 Q10 1 0.0079 0.0518 0.5000 0.50000 0.05 0.28 3.34 H8 4.16 C8 4.16 H7 4.57 C7 Shortest distances between peaks (including symmetry equivalents) 3 3 0.74 8 8 1.23 6 6 1.28 3 9 1.55 2 6 1.56 2 9 2.19 10 10 2.31 2 6 2.33 2 2 2.37 6 9 2.46 1 7 2.80 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 0.01: 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. 2.41: Read intensity data, sort/merge etc. 0.01: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 41.05: Structure factors and derivatives 28.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.23: Apply other restraints 2.10: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.05: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src1026sq finished at 11:36:37 Total CPU time: 73.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++