++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + lx2294isup2 started at 15:07:15 on 12-Jan-2015 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S965B IN P-1 CELL 0.71073 9.79350 11.21410 19.56960 103.60100 90.86700 108.24000 ZERR 2 0.00160 0.00180 0.00330 0.00400 0.00300 0.00400 LATT 1 SFAC C H N Cu Si P UNIT 78 106 10 2 2 2 V = 1974.81 F(000) = 760.0 Mu = 0.66 mm-1 Cell Wt = 1428.93 Rho = 1.202 OMIT 2 -3 4 OMIT 1 -2 2 OMIT -3 50.1 L.S. 22 ANIS ACTA BOND $H FMAP 2 PLAN 5 MPLA 3 N3 Cu1 N1 MPLA 4 N3 C13 C16 N1 MPLA 3 C13 N2 C16 MPLA 4 N3 C13 C16 N1 MPLA 3 N1 N5 P1 CU1 HTAB SIZE 0.32 0.31 0.28 SIMU 0.02 C10 C11 SIMU 0.02 C10 C12 WGHT 0.000000 0.000000 FVAR 0.254570 TEMP -78 MOLE 1 Cu1 4 0.215848 0.986465 0.270534 11.000000 0.047170 = 0.036210 0.041880 0.009340 -0.002950 0.014760 P1 6 0.093342 0.971964 0.174165 11.000000 0.051380 = 0.041160 0.040830 0.008810 -0.003860 0.019200 N1 3 0.316107 0.878649 0.303186 11.000000 0.045300 = 0.026360 0.049720 0.010350 -0.009460 0.011930 N2 3 0.499814 0.872313 0.381661 11.000000 0.057680 = 0.049450 0.077730 0.017530 -0.020820 0.019630 N3 3 0.505759 1.066708 0.364170 11.000000 0.039060 = 0.041480 0.054790 0.004000 -0.005390 0.011060 N4 3 0.555158 1.278649 0.374285 11.000000 0.053140 = 0.040250 0.081390 0.009130 -0.005600 0.002540 N5 3 0.312846 1.146257 0.343933 11.000000 0.038890 = 0.038330 0.044150 0.003360 -0.005810 0.009860 Si1 5 0.212538 1.225633 0.394370 11.000000 0.052860 = 0.039810 0.049750 0.003360 -0.005340 0.018770 C1 1 0.267508 0.744185 0.271639 11.000000 0.034630 = 0.032500 0.047550 0.015540 -0.004200 0.013210 C2 1 0.340424 0.687809 0.220304 11.000000 0.044900 = 0.041970 0.047970 0.013090 0.000990 0.018770 C3 1 0.281778 0.557635 0.186912 11.000000 0.071380 = 0.045020 0.066090 0.008070 0.004730 0.026060 AFIX 43 H3 2 0.332558 0.518533 0.152428 11.000000 -1.200000 AFIX 0 C4 1 0.151580 0.483765 0.202615 11.000000 0.081330 = 0.036410 0.075700 0.008690 -0.000520 0.022020 AFIX 43 H4 2 0.111820 0.394705 0.178347 11.000000 -1.200000 AFIX 0 C5 1 0.079465 0.537748 0.252786 11.000000 0.056570 = 0.041360 0.082730 0.025150 0.006390 0.008980 AFIX 43 H5 2 -0.009788 0.485547 0.264117 11.000000 -1.200000 AFIX 0 C6 1 0.134323 0.668158 0.287760 11.000000 0.046710 = 0.042620 0.064110 0.016530 0.000940 0.019030 C7 1 0.051998 0.725470 0.345346 11.000000 0.064140 = 0.049140 0.125850 0.030500 0.036110 0.018710 AFIX 13 H7 2 0.109587 0.818806 0.365725 11.000000 -1.200000 AFIX 0 C8 1 0.029299 0.657161 0.405527 11.000000 0.187080 = 0.197920 0.105540 0.069430 0.072620 0.101670 AFIX 137 H8A 2 -0.016408 0.701978 0.442680 11.000000 -1.500000 H8B 2 0.122846 0.658880 0.425038 11.000000 -1.500000 H8C 2 -0.033057 0.566946 0.387345 11.000000 -1.500000 AFIX 0 C9 1 -0.093784 0.719097 0.315290 11.000000 0.093420 = 0.144700 0.187180 0.072190 0.049710 0.072050 AFIX 137 H9A 2 -0.148941 0.629007 0.291311 11.000000 -1.500000 H9B 2 -0.080585 0.772810 0.281423 11.000000 -1.500000 H9C 2 -0.146434 0.751340 0.353631 11.000000 -1.500000 AFIX 0 C10 1 0.481626 0.766137 0.198995 11.000000 0.057920 = 0.057530 0.070860 0.017760 0.013770 0.021240 AFIX 13 H10 2 0.523281 0.847362 0.237539 11.000000 -1.200000 AFIX 0 C11 1 0.590429 0.696369 0.189065 11.000000 0.076450 = 0.116360 0.289430 0.065990 0.066710 0.050340 AFIX 137 H11A 2 0.604631 0.668986 0.231895 11.000000 -1.500000 H11B 2 0.682342 0.754519 0.179879 11.000000 -1.500000 H11C 2 0.555526 0.619937 0.148922 11.000000 -1.500000 AFIX 0 C12 1 0.453969 0.804599 0.132682 11.000000 0.117500 = 0.186810 0.098420 0.085350 0.015410 0.003210 AFIX 137 H12A 2 0.546315 0.846782 0.116093 11.000000 -1.500000 H12B 2 0.398652 0.864958 0.142683 11.000000 -1.500000 H12C 2 0.398946 0.727079 0.096129 11.000000 -1.500000 AFIX 0 C13 1 0.432884 0.938292 0.348872 11.000000 0.042420 = 0.045790 0.046350 0.011250 0.009330 0.019360 C14 1 0.639753 0.942151 0.422153 11.000000 0.081700 = 0.086590 0.148690 0.028560 -0.054500 0.029890 AFIX 137 H14A 2 0.699748 1.002077 0.396841 11.000000 -1.500000 H14B 2 0.687622 0.880102 0.428311 11.000000 -1.500000 H14C 2 0.626011 0.991247 0.468543 11.000000 -1.500000 AFIX 0 C15 1 0.431639 0.752410 0.396647 11.000000 0.119780 = 0.077530 0.121770 0.046050 -0.053690 0.006410 AFIX 137 H15A 2 0.327117 0.727176 0.385128 11.000000 -1.500000 H15B 2 0.452091 0.759890 0.446937 11.000000 -1.500000 H15C 2 0.468097 0.686429 0.368342 11.000000 -1.500000 AFIX 0 C16 1 0.450313 1.159230 0.359021 11.000000 0.052010 = 0.037800 0.037340 0.003100 0.007130 0.005060 C17 1 0.701081 1.302313 0.402436 11.000000 0.053310 = 0.061620 0.100940 0.000960 -0.012450 -0.008150 AFIX 137 H17A 2 0.702450 1.235166 0.426443 11.000000 -1.500000 H17B 2 0.736330 1.387677 0.436171 11.000000 -1.500000 H17C 2 0.763469 1.300151 0.363794 11.000000 -1.500000 AFIX 0 C18 1 0.536643 1.383254 0.346214 11.000000 0.093300 = 0.045220 0.084930 0.017120 0.003100 -0.004540 AFIX 137 H18A 2 0.614832 1.410779 0.316858 11.000000 -1.500000 H18B 2 0.539152 1.456920 0.385423 11.000000 -1.500000 H18C 2 0.443553 1.352075 0.317572 11.000000 -1.500000 AFIX 0 C19 1 0.312781 1.337857 0.477990 11.000000 0.078280 = 0.064310 0.058200 0.001960 0.000040 0.028350 AFIX 137 H19A 2 0.386634 1.305323 0.493595 11.000000 -1.500000 H19B 2 0.245534 1.343436 0.514256 11.000000 -1.500000 H19C 2 0.359181 1.424154 0.470336 11.000000 -1.500000 AFIX 0 C20 1 0.059198 1.101981 0.418838 11.000000 0.059660 = 0.075150 0.078200 0.006400 0.010780 0.016840 AFIX 137 H20A 2 0.004678 1.039016 0.375927 11.000000 -1.500000 H20B 2 -0.004296 1.144484 0.445250 11.000000 -1.500000 H20C 2 0.096163 1.057087 0.448269 11.000000 -1.500000 AFIX 0 C21 1 0.136826 1.319874 0.346566 11.000000 0.099350 = 0.063690 0.093040 0.011030 -0.018940 0.046780 AFIX 137 H21A 2 0.215736 1.391315 0.337070 11.000000 -1.500000 H21B 2 0.071030 1.355076 0.375689 11.000000 -1.500000 H21C 2 0.083916 1.262764 0.301813 11.000000 -1.500000 AFIX 0 C22 1 -0.003045 0.817883 0.113054 11.000000 0.058490 = 0.048240 0.040560 0.006360 -0.010140 0.024270 C23 1 0.015206 0.705189 0.122577 11.000000 0.096120 = 0.050900 0.072740 0.008920 -0.030510 0.030230 AFIX 43 H23 2 0.082089 0.709855 0.159579 11.000000 -1.200000 AFIX 0 C24 1 -0.062228 0.587024 0.079169 11.000000 0.151330 = 0.045930 0.099780 -0.004370 -0.059090 0.035450 AFIX 43 H24 2 -0.051957 0.510427 0.088089 11.000000 -1.200000 AFIX 0 C25 1 -0.153895 0.577120 0.023328 11.000000 0.122160 = 0.052410 0.097220 -0.013630 -0.054770 0.025240 AFIX 43 H25 2 -0.204613 0.494906 -0.007444 11.000000 -1.200000 AFIX 0 C26 1 -0.171325 0.687993 0.012527 11.000000 0.099750 = 0.069130 0.076500 -0.008040 -0.041940 0.039060 AFIX 43 H26 2 -0.235937 0.682618 -0.025638 11.000000 -1.200000 AFIX 0 C27 1 -0.097016 0.805494 0.055920 11.000000 0.082120 = 0.052470 0.057390 -0.001240 -0.023360 0.029800 AFIX 43 H27 2 -0.109556 0.881297 0.047011 11.000000 -1.200000 AFIX 0 C28 1 -0.041298 1.054353 0.178841 11.000000 0.042890 = 0.035690 0.046750 0.006290 -0.003870 0.014190 C29 1 -0.141181 1.035892 0.228445 11.000000 0.054190 = 0.057300 0.060680 0.014140 0.003860 0.022040 AFIX 43 H29 2 -0.135065 0.983492 0.259341 11.000000 -1.200000 AFIX 0 C30 1 -0.247564 1.091228 0.233736 11.000000 0.057810 = 0.074260 0.085620 0.009950 0.018220 0.027530 AFIX 43 H30 2 -0.314303 1.077683 0.268128 11.000000 -1.200000 AFIX 0 C31 1 -0.257708 1.166357 0.189267 11.000000 0.057080 = 0.063730 0.114480 0.003600 -0.007940 0.035290 AFIX 43 H31 2 -0.331696 1.205058 0.192745 11.000000 -1.200000 AFIX 0 C32 1 -0.160503 1.186028 0.139305 11.000000 0.070160 = 0.061620 0.094700 0.023730 -0.009700 0.033490 AFIX 43 H32 2 -0.167076 1.238829 0.108716 11.000000 -1.200000 AFIX 0 C33 1 -0.054518 1.129192 0.133954 11.000000 0.057370 = 0.046270 0.053410 0.012350 -0.000450 0.024830 AFIX 43 H33 2 0.010741 1.141520 0.098838 11.000000 -1.200000 AFIX 0 C34 1 0.229957 1.058411 0.124845 11.000000 0.046490 = 0.062170 0.046670 0.017540 0.002080 0.032840 C35 1 0.314730 1.183029 0.158400 11.000000 0.050120 = 0.061620 0.053390 0.010220 0.003130 0.014930 AFIX 43 H35 2 0.297275 1.221779 0.204620 11.000000 -1.200000 AFIX 0 C36 1 0.424070 1.251785 0.125811 11.000000 0.052360 = 0.069740 0.085450 0.032950 0.000450 0.013150 AFIX 43 H36 2 0.482496 1.337048 0.150037 11.000000 -1.200000 AFIX 0 C37 1 0.450026 1.198728 0.058538 11.000000 0.067330 = 0.100830 0.083950 0.052700 0.020170 0.034040 AFIX 43 H37 2 0.525658 1.246366 0.035958 11.000000 -1.200000 AFIX 0 C38 1 0.364862 1.076307 0.024976 11.000000 0.083210 = 0.113610 0.054930 0.032260 0.023890 0.051060 AFIX 43 H38 2 0.381856 1.038604 -0.021533 11.000000 -1.200000 AFIX 0 C39 1 0.254318 1.005636 0.056971 11.000000 0.072510 = 0.067540 0.054360 0.016950 0.007760 0.036460 AFIX 43 H39 2 0.195270 0.920910 0.032259 11.000000 -1.200000 AFIX HKLF 4 Covalent radii and connectivity table for S965B IN P-1 C 0.770 H 0.320 N 0.700 CU 1.280 SI 1.170 P 1.100 Cu1 - N5 N1 P1 P1 - C22 C28 C34 Cu1 N1 - C13 C1 Cu1 N2 - C13 C15 C14 N3 - C16 C13 N4 - C16 C17 C18 N5 - C16 Si1 Cu1 Si1 - N5 C19 C20 C21 C1 - C2 C6 N1 C2 - C3 C1 C10 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 C7 - C9 C6 C8 C8 - C7 C9 - C7 C10 - C11 C12 C2 C11 - C10 C12 - C10 C13 - N1 N3 N2 C14 - N2 C15 - N2 C16 - N5 N3 N4 C17 - N4 C18 - N4 C19 - Si1 C20 - Si1 C21 - Si1 C22 - C23 C27 P1 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C27 C25 C27 - C26 C22 C28 - C33 C29 P1 C29 - C30 C28 C30 - C29 C31 C31 - C30 C32 C32 - C33 C31 C33 - C32 C28 C34 - C35 C39 P1 C35 - C36 C34 C36 - C35 C37 C37 - C38 C36 C38 - C37 C39 C39 - C34 C38 14095 Reflections read, of which 3011 rejected -11 =< h =< 9, -11 =< k =< 13, -23 =< l =< 23, Max. 2-theta = 50.10 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 -2 1 1301.60 9.33 2 68.91 2 -1 1 304.45 4.75 2 31.32 2 1 1 283.70 5.68 2 29.12 -1 -1 2 687.42 6.71 2 82.40 0 -1 2 658.93 4.86 2 81.89 1 -1 2 342.23 2.60 3 21.44 -1 0 2 212.92 3.60 2 22.34 -1 -2 3 615.30 7.71 2 66.33 -2 -1 3 974.96 10.23 2 132.95 -1 -1 3 1189.65 9.62 2 158.50 0 -1 3 257.07 2.88 3 15.39 1 -1 3 593.41 4.55 3 23.65 -1 0 3 367.37 5.30 2 46.41 0 -2 4 572.03 5.18 3 28.89 1 -1 4 1784.67 9.04 3 82.52 -2 0 4 2143.54 15.91 2 213.47 -1 0 4 315.35 5.58 2 34.05 0 0 4 496.40 4.99 3 34.06 3 -3 5 1070.40 9.66 2 64.46 -2 -1 5 392.07 7.46 2 41.06 2 -3 6 769.46 6.97 2 45.78 21 Inconsistent equivalents 6988 Unique reflections, of which 0 suppressed R(int) = 0.0767 R(sigma) = 0.1738 Friedel opposites merged Maximum memory for data reduction = 4786 / 69945 Default effective X-H distances for T = -78.0 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 = 6097 / 565309 wR2 = 0.0891 before cycle 1 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.007 OSF Mean shift/esd = 0.001 Maximum = 0.012 for z Cu1 Max. shift = 0.000 A for H9C Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 2 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.004 for z Cu1 Max. shift = 0.000 A for H14B Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 3 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H14C Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 4 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H18C Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 5 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C14 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 6 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 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. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H18C Max. dU = 0.000 for C11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 7 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H8B Max. dU = 0.000 for C12 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 8 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H19C Max. dU = 0.000 for C11 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 9 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H19C Max. dU = 0.000 for C27 Least-squares cycle 10 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 10 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C7 Least-squares cycle 11 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 11 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H19B Max. dU = 0.000 for C11 Least-squares cycle 12 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 12 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H9B Max. dU = 0.000 for C11 Least-squares cycle 13 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 13 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for C11 Least-squares cycle 14 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 14 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C30 Max. dU = 0.000 for C12 Least-squares cycle 15 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 15 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C12 Least-squares cycle 16 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 16 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C12 Least-squares cycle 17 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 17 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C12 Least-squares cycle 18 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 18 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C9 Least-squares cycle 19 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 19 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C9 Least-squares cycle 20 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 20 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H12B Max. dU = 0.000 for C14 Least-squares cycle 21 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 21 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Si1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C17 Least-squares cycle 22 Maximum vector length = 511 Memory required = 6097 / 565309 wR2 = 0.0891 before cycle 22 for 6988 data and 435 / 435 parameters Disagreeable restraints before cycle 22 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25457 0.00025 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8A Max. dU = 0.000 for C31 Largest correlation matrix elements 0.615 U23 C12 / U22 C12 0.548 U12 C8 / U22 C8 0.522 U12 C21 / U11 C21 0.608 U23 C12 / U33 C12 0.544 U12 C34 / U22 C34 0.521 U12 C21 / U22 C21 0.592 U23 C37 / U33 C37 0.536 U23 C8 / U33 C8 0.519 U12 C39 / U11 C39 0.565 U13 C38 / U23 C38 0.533 z C37 / y C37 0.519 U12 C34 / U11 C34 0.556 y C38 / x C38 0.531 U23 C9 / U33 C9 0.519 U12 C38 / U11 C38 0.553 U12 C9 / U22 C9 0.529 U23 C15 / U33 C15 0.516 U23 C36 / U33 C36 0.552 U12 C9 / U11 C9 0.527 U23 C8 / U22 C8 0.515 U23 C9 / U22 C9 0.548 U23 C37 / U22 C37 0.523 U12 C8 / U11 C8 0.515 U12 C37 / U13 C37 Idealized hydrogen atom generation before cycle 23 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.3326 0.5185 0.1524 43 0.950 0.000 C3 C4 C2 H4 0.1118 0.3947 0.1783 43 0.950 0.000 C4 C5 C3 H5 -0.0098 0.4855 0.2641 43 0.950 0.000 C5 C4 C6 H7 0.1096 0.8188 0.3657 13 1.000 0.000 C7 C9 C6 C8 H8A -0.0164 0.7020 0.4427 137 0.980 0.000 C8 C7 H8A H8B 0.1228 0.6589 0.4250 137 0.980 0.000 C8 C7 H8A H8C -0.0331 0.5669 0.3873 137 0.980 0.000 C8 C7 H8A H9A -0.1489 0.6290 0.2913 137 0.980 0.000 C9 C7 H9A H9B -0.0806 0.7728 0.2814 137 0.980 0.000 C9 C7 H9A H9C -0.1464 0.7513 0.3536 137 0.980 0.000 C9 C7 H9A H10 0.5233 0.8474 0.2375 13 1.000 0.000 C10 C11 C12 C2 H11A 0.6046 0.6690 0.2319 137 0.980 0.000 C11 C10 H11A H11B 0.6823 0.7545 0.1799 137 0.980 0.000 C11 C10 H11A H11C 0.5555 0.6199 0.1489 137 0.980 0.000 C11 C10 H11A H12A 0.5463 0.8468 0.1161 137 0.980 0.000 C12 C10 H12A H12B 0.3987 0.8650 0.1427 137 0.980 0.000 C12 C10 H12A H12C 0.3989 0.7271 0.0961 137 0.980 0.000 C12 C10 H12A H14A 0.6997 1.0021 0.3968 137 0.980 0.000 C14 N2 H14A H14B 0.6876 0.8801 0.4283 137 0.980 0.000 C14 N2 H14A H14C 0.6260 0.9912 0.4685 137 0.980 0.000 C14 N2 H14A H15A 0.3271 0.7272 0.3851 137 0.980 0.000 C15 N2 H15A H15B 0.4521 0.7599 0.4469 137 0.980 0.000 C15 N2 H15A H15C 0.4681 0.6864 0.3683 137 0.980 0.000 C15 N2 H15A H17A 0.7025 1.2352 0.4264 137 0.980 0.000 C17 N4 H17A H17B 0.7363 1.3877 0.4362 137 0.980 0.000 C17 N4 H17A H17C 0.7635 1.3002 0.3638 137 0.980 0.000 C17 N4 H17A H18A 0.6148 1.4108 0.3169 137 0.980 0.000 C18 N4 H18A H18B 0.5392 1.4569 0.3854 137 0.980 0.000 C18 N4 H18A H18C 0.4436 1.3521 0.3176 137 0.980 0.000 C18 N4 H18A H19A 0.3866 1.3053 0.4936 137 0.980 0.000 C19 Si1 H19A H19B 0.2455 1.3434 0.5143 137 0.980 0.000 C19 Si1 H19A H19C 0.3592 1.4242 0.4703 137 0.980 0.000 C19 Si1 H19A H20A 0.0047 1.0390 0.3759 137 0.980 0.000 C20 Si1 H20A H20B -0.0043 1.1445 0.4453 137 0.980 0.000 C20 Si1 H20A H20C 0.0962 1.0571 0.4483 137 0.980 0.000 C20 Si1 H20A H21A 0.2157 1.3913 0.3371 137 0.980 0.000 C21 Si1 H21A H21B 0.0710 1.3551 0.3757 137 0.980 0.000 C21 Si1 H21A H21C 0.0839 1.2628 0.3018 137 0.980 0.000 C21 Si1 H21A H23 0.0821 0.7099 0.1596 43 0.950 0.000 C23 C24 C22 H24 -0.0520 0.5104 0.0881 43 0.950 0.000 C24 C25 C23 H25 -0.2046 0.4949 -0.0074 43 0.950 0.000 C25 C24 C26 H26 -0.2359 0.6826 -0.0256 43 0.950 0.000 C26 C27 C25 H27 -0.1096 0.8813 0.0470 43 0.950 0.000 C27 C26 C22 H29 -0.1351 0.9835 0.2593 43 0.950 0.000 C29 C30 C28 H30 -0.3143 1.0777 0.2681 43 0.950 0.000 C30 C29 C31 H31 -0.3317 1.2051 0.1927 43 0.950 0.000 C31 C30 C32 H32 -0.1671 1.2388 0.1087 43 0.950 0.000 C32 C33 C31 H33 0.0107 1.1415 0.0988 43 0.950 0.000 C33 C32 C28 H35 0.2973 1.2218 0.2046 43 0.950 0.000 C35 C36 C34 H36 0.4825 1.3370 0.1500 43 0.950 0.000 C36 C35 C37 H37 0.5257 1.2464 0.0360 43 0.950 0.000 C37 C38 C36 H38 0.3819 1.0386 -0.0215 43 0.950 0.000 C38 C37 C39 H39 0.1953 0.9209 0.0323 43 0.950 0.000 C39 C34 C38 S965B IN P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cu1 0.21585 0.98646 0.27053 1.00000 0.04717 0.03621 0.04188 0.00934 -0.00295 0.01476 0.04164 0.00113 0.00005 0.00005 0.00003 0.00000 0.00034 0.00033 0.00033 0.00028 0.00026 0.00027 0.00017 P1 0.09334 0.97196 0.17417 1.00000 0.05138 0.04116 0.04083 0.00881 -0.00386 0.01920 0.04383 0.00245 0.00012 0.00011 0.00006 0.00000 0.00078 0.00074 0.00074 0.00063 0.00060 0.00063 0.00032 N1 0.31611 0.87865 0.30319 1.00000 0.04530 0.02636 0.04972 0.01035 -0.00946 0.01193 0.04043 0.00749 0.00034 0.00031 0.00017 0.00000 0.00224 0.00206 0.00229 0.00188 0.00183 0.00180 0.00088 N2 0.49981 0.87231 0.38166 1.00000 0.05768 0.04945 0.07773 0.01753 -0.02082 0.01963 0.06114 0.00795 0.00038 0.00036 0.00020 0.00000 0.00267 0.00265 0.00293 0.00242 0.00223 0.00224 0.00111 N3 0.50576 1.06671 0.36417 1.00000 0.03906 0.04148 0.05479 0.00400 -0.00539 0.01106 0.04716 0.00724 0.00033 0.00035 0.00017 0.00000 0.00222 0.00235 0.00251 0.00207 0.00179 0.00197 0.00093 N4 0.55516 1.27865 0.37429 1.00000 0.05314 0.04025 0.08139 0.00913 -0.00560 0.00254 0.06253 0.00814 0.00040 0.00035 0.00020 0.00000 0.00267 0.00250 0.00307 0.00237 0.00223 0.00217 0.00111 N5 0.31285 1.14626 0.34393 1.00000 0.03889 0.03833 0.04415 0.00336 -0.00581 0.00986 0.04246 0.00693 0.00036 0.00030 0.00016 0.00000 0.00217 0.00217 0.00224 0.00186 0.00175 0.00181 0.00088 Si1 0.21254 1.22563 0.39437 1.00000 0.05286 0.03981 0.04975 0.00336 -0.00534 0.01877 0.04811 0.00266 0.00013 0.00012 0.00006 0.00000 0.00085 0.00079 0.00085 0.00070 0.00067 0.00068 0.00035 C1 0.26751 0.74419 0.27164 1.00000 0.03463 0.03250 0.04754 0.01554 -0.00420 0.01321 0.03681 0.00890 0.00042 0.00038 0.00022 0.00000 0.00257 0.00258 0.00285 0.00234 0.00216 0.00220 0.00102 C2 0.34042 0.68781 0.22030 1.00000 0.04490 0.04197 0.04797 0.01309 0.00099 0.01877 0.04357 0.00971 0.00045 0.00042 0.00023 0.00000 0.00286 0.00291 0.00298 0.00254 0.00234 0.00246 0.00111 C3 0.28178 0.55763 0.18691 1.00000 0.07138 0.04502 0.06609 0.00807 0.00473 0.02606 0.06020 0.01058 0.00053 0.00045 0.00024 0.00000 0.00370 0.00316 0.00358 0.00293 0.00291 0.00291 0.00134 H3 0.33256 0.51853 0.15243 1.00000 0.07224 0.00000 0.00000 C4 0.15158 0.48376 0.20261 1.00000 0.08133 0.03641 0.07570 0.00869 -0.00052 0.02202 0.06485 0.01112 0.00059 0.00046 0.00026 0.00000 0.00399 0.00295 0.00417 0.00303 0.00323 0.00302 0.00144 H4 0.11182 0.39470 0.17835 1.00000 0.07782 0.00000 0.00000 C5 0.07946 0.53775 0.25279 1.00000 0.05657 0.04136 0.08273 0.02514 0.00639 0.00898 0.06023 0.01060 0.00050 0.00044 0.00027 0.00000 0.00334 0.00318 0.00406 0.00313 0.00290 0.00269 0.00137 H5 -0.00979 0.48555 0.26412 1.00000 0.07227 0.00000 0.00000 C6 0.13432 0.66816 0.28776 1.00000 0.04671 0.04262 0.06411 0.01653 0.00094 0.01903 0.04958 0.01009 0.00047 0.00043 0.00024 0.00000 0.00299 0.00297 0.00340 0.00275 0.00256 0.00254 0.00119 C7 0.05200 0.72547 0.34535 1.00000 0.06414 0.04914 0.12585 0.03050 0.03611 0.01871 0.07787 0.01190 0.00053 0.00046 0.00031 0.00000 0.00377 0.00330 0.00527 0.00362 0.00364 0.00293 0.00168 H7 0.10959 0.81881 0.36573 1.00000 0.09344 0.00000 0.00000 C8 0.02930 0.65716 0.40553 1.00000 0.18708 0.19792 0.10554 0.06943 0.07262 0.10167 0.14802 0.01559 0.00072 0.00065 0.00031 0.00000 0.00736 0.00767 0.00550 0.00589 0.00506 0.00624 0.00282 H8A -0.01641 0.70198 0.44268 1.00000 0.22204 0.00000 0.00000 H8B 0.12285 0.65888 0.42504 1.00000 0.22204 0.00000 0.00000 H8C -0.03306 0.56695 0.38735 1.00000 0.22204 0.00000 0.00000 C9 -0.09378 0.71910 0.31529 1.00000 0.09342 0.14470 0.18718 0.07219 0.04971 0.07205 0.12804 0.01438 0.00060 0.00058 0.00034 0.00000 0.00502 0.00618 0.00711 0.00570 0.00474 0.00474 0.00250 H9A -0.14894 0.62901 0.29131 1.00000 0.19205 0.00000 0.00000 H9B -0.08059 0.77281 0.28142 1.00000 0.19205 0.00000 0.00000 H9C -0.14643 0.75134 0.35363 1.00000 0.19205 0.00000 0.00000 C10 0.48163 0.76614 0.19899 1.00000 0.05792 0.05753 0.07086 0.01776 0.01377 0.02124 0.06117 0.01053 0.00048 0.00044 0.00025 0.00000 0.00333 0.00329 0.00368 0.00297 0.00273 0.00279 0.00134 H10 0.52328 0.84736 0.23754 1.00000 0.07340 0.00000 0.00000 C11 0.59043 0.69637 0.18907 1.00000 0.07645 0.11636 0.28943 0.06599 0.06671 0.05034 0.15306 0.01490 0.00059 0.00055 0.00041 0.00000 0.00452 0.00558 0.00968 0.00620 0.00531 0.00427 0.00309 H11A 0.60463 0.66899 0.23189 1.00000 0.22959 0.00000 0.00000 H11B 0.68234 0.75452 0.17988 1.00000 0.22959 0.00000 0.00000 H11C 0.55553 0.61994 0.14892 1.00000 0.22959 0.00000 0.00000 C12 0.45397 0.80460 0.13268 1.00000 0.11750 0.18681 0.09842 0.08535 0.01541 0.00321 0.13662 0.01297 0.00061 0.00060 0.00029 0.00000 0.00534 0.00715 0.00506 0.00543 0.00403 0.00486 0.00271 H12A 0.54632 0.84678 0.11609 1.00000 0.20493 0.00000 0.00000 H12B 0.39865 0.86496 0.14268 1.00000 0.20493 0.00000 0.00000 H12C 0.39895 0.72708 0.09613 1.00000 0.20493 0.00000 0.00000 C13 0.43288 0.93829 0.34887 1.00000 0.04242 0.04580 0.04635 0.01125 0.00933 0.01936 0.04367 0.01006 0.00046 0.00043 0.00022 0.00000 0.00285 0.00307 0.00289 0.00261 0.00235 0.00257 0.00111 C14 0.63975 0.94215 0.42215 1.00000 0.08170 0.08659 0.14869 0.02856 -0.05450 0.02989 0.10599 0.01082 0.00053 0.00048 0.00030 0.00000 0.00417 0.00451 0.00559 0.00426 0.00390 0.00361 0.00214 H14A 0.69975 1.00208 0.39684 1.00000 0.15899 0.00000 0.00000 H14B 0.68762 0.88010 0.42831 1.00000 0.15899 0.00000 0.00000 H14C 0.62601 0.99125 0.46854 1.00000 0.15899 0.00000 0.00000 C15 0.43164 0.75241 0.39665 1.00000 0.11978 0.07753 0.12177 0.04606 -0.05369 0.00641 0.10958 0.01106 0.00057 0.00048 0.00028 0.00000 0.00511 0.00440 0.00523 0.00420 0.00400 0.00383 0.00225 H15A 0.32712 0.72718 0.38513 1.00000 0.16437 0.00000 0.00000 H15B 0.45209 0.75989 0.44694 1.00000 0.16437 0.00000 0.00000 H15C 0.46810 0.68643 0.36834 1.00000 0.16437 0.00000 0.00000 C16 0.45031 1.15923 0.35902 1.00000 0.05201 0.03780 0.03734 0.00310 0.00713 0.00506 0.04578 0.00946 0.00049 0.00042 0.00021 0.00000 0.00316 0.00281 0.00273 0.00235 0.00234 0.00264 0.00114 C17 0.70108 1.30231 0.40244 1.00000 0.05331 0.06162 0.10094 0.00096 -0.01245 -0.00815 0.08208 0.00953 0.00047 0.00043 0.00026 0.00000 0.00344 0.00367 0.00446 0.00334 0.00310 0.00286 0.00167 H17A 0.70245 1.23517 0.42644 1.00000 0.12312 0.00000 0.00000 H17B 0.73633 1.38768 0.43617 1.00000 0.12312 0.00000 0.00000 H17C 0.76347 1.30015 0.36379 1.00000 0.12312 0.00000 0.00000 C18 0.53664 1.38325 0.34621 1.00000 0.09330 0.04522 0.08493 0.01712 0.00310 -0.00454 0.08094 0.00994 0.00050 0.00041 0.00025 0.00000 0.00420 0.00323 0.00409 0.00321 0.00316 0.00300 0.00167 H18A 0.61483 1.41078 0.31686 1.00000 0.12140 0.00000 0.00000 H18B 0.53915 1.45692 0.38542 1.00000 0.12140 0.00000 0.00000 H18C 0.44355 1.35208 0.31757 1.00000 0.12140 0.00000 0.00000 C19 0.31278 1.33786 0.47799 1.00000 0.07828 0.06431 0.05820 0.00196 0.00004 0.02835 0.06815 0.00901 0.00046 0.00040 0.00022 0.00000 0.00360 0.00346 0.00335 0.00290 0.00272 0.00293 0.00142 H19A 0.38663 1.30532 0.49359 1.00000 0.10223 0.00000 0.00000 H19B 0.24553 1.34344 0.51426 1.00000 0.10223 0.00000 0.00000 H19C 0.35918 1.42415 0.47034 1.00000 0.10223 0.00000 0.00000 C20 0.05920 1.10198 0.41884 1.00000 0.05966 0.07515 0.07820 0.00640 0.01078 0.01684 0.07447 0.00974 0.00044 0.00042 0.00024 0.00000 0.00333 0.00374 0.00376 0.00324 0.00281 0.00288 0.00150 H20A 0.00468 1.03902 0.37593 1.00000 0.11171 0.00000 0.00000 H20B -0.00430 1.14448 0.44525 1.00000 0.11171 0.00000 0.00000 H20C 0.09616 1.05709 0.44827 1.00000 0.11171 0.00000 0.00000 C21 0.13683 1.31987 0.34657 1.00000 0.09935 0.06369 0.09304 0.01103 -0.01894 0.04678 0.08236 0.01026 0.00051 0.00043 0.00025 0.00000 0.00419 0.00361 0.00419 0.00329 0.00324 0.00326 0.00167 H21A 0.21574 1.39131 0.33707 1.00000 0.12354 0.00000 0.00000 H21B 0.07103 1.35508 0.37569 1.00000 0.12354 0.00000 0.00000 H21C 0.08392 1.26276 0.30181 1.00000 0.12354 0.00000 0.00000 C22 -0.00304 0.81788 0.11305 1.00000 0.05849 0.04824 0.04056 0.00636 -0.01014 0.02427 0.04846 0.00915 0.00044 0.00041 0.00021 0.00000 0.00303 0.00305 0.00278 0.00248 0.00231 0.00251 0.00118 C23 0.01521 0.70519 0.12258 1.00000 0.09612 0.05089 0.07274 0.00892 -0.03051 0.03023 0.07335 0.01097 0.00053 0.00046 0.00026 0.00000 0.00414 0.00338 0.00383 0.00311 0.00308 0.00317 0.00157 H23 0.08209 0.70985 0.15958 1.00000 0.08802 0.00000 0.00000 C24 -0.06223 0.58702 0.07917 1.00000 0.15133 0.04593 0.09978 -0.00437 -0.05909 0.03545 0.10301 0.01224 0.00065 0.00051 0.00030 0.00000 0.00583 0.00379 0.00482 0.00348 0.00427 0.00384 0.00216 H24 -0.05196 0.51043 0.08809 1.00000 0.12362 0.00000 0.00000 C25 -0.15390 0.57712 0.02333 1.00000 0.12216 0.05241 0.09722 -0.01363 -0.05477 0.02524 0.09782 0.01144 0.00061 0.00052 0.00030 0.00000 0.00508 0.00388 0.00480 0.00352 0.00389 0.00364 0.00201 H25 -0.20461 0.49491 -0.00744 1.00000 0.11738 0.00000 0.00000 C26 -0.17133 0.68799 0.01253 1.00000 0.09975 0.06913 0.07650 -0.00804 -0.04194 0.03906 0.08423 0.01142 0.00056 0.00052 0.00028 0.00000 0.00441 0.00402 0.00405 0.00347 0.00326 0.00363 0.00174 H26 -0.23594 0.68262 -0.02564 1.00000 0.10108 0.00000 0.00000 C27 -0.09702 0.80549 0.05592 1.00000 0.08212 0.05247 0.05739 -0.00124 -0.02336 0.02980 0.06510 0.01045 0.00049 0.00047 0.00024 0.00000 0.00372 0.00341 0.00339 0.00286 0.00284 0.00300 0.00144 H27 -0.10956 0.88130 0.04701 1.00000 0.07812 0.00000 0.00000 C28 -0.04130 1.05435 0.17884 1.00000 0.04289 0.03569 0.04675 0.00629 -0.00387 0.01419 0.04226 0.00835 0.00042 0.00037 0.00022 0.00000 0.00278 0.00264 0.00285 0.00237 0.00229 0.00224 0.00110 C29 -0.14118 1.03589 0.22845 1.00000 0.05419 0.05730 0.06068 0.01414 0.00386 0.02204 0.05661 0.00933 0.00049 0.00042 0.00024 0.00000 0.00314 0.00326 0.00340 0.00279 0.00269 0.00274 0.00128 H29 -0.13506 0.98349 0.25934 1.00000 0.06793 0.00000 0.00000 C30 -0.24756 1.09123 0.23374 1.00000 0.05781 0.07426 0.08562 0.00995 0.01822 0.02753 0.07280 0.01020 0.00052 0.00049 0.00028 0.00000 0.00358 0.00394 0.00426 0.00354 0.00307 0.00317 0.00155 H30 -0.31430 1.07768 0.26813 1.00000 0.08736 0.00000 0.00000 C31 -0.25771 1.16636 0.18927 1.00000 0.05708 0.06373 0.11448 0.00360 -0.00794 0.03529 0.07819 0.01052 0.00054 0.00049 0.00033 0.00000 0.00372 0.00385 0.00514 0.00372 0.00351 0.00317 0.00168 H31 -0.33170 1.20506 0.19274 1.00000 0.09383 0.00000 0.00000 C32 -0.16050 1.18603 0.13931 1.00000 0.07016 0.06162 0.09470 0.02373 -0.00970 0.03349 0.07209 0.01037 0.00056 0.00045 0.00029 0.00000 0.00388 0.00367 0.00450 0.00338 0.00337 0.00321 0.00155 H32 -0.16708 1.23883 0.10872 1.00000 0.08651 0.00000 0.00000 C33 -0.05452 1.12919 0.13395 1.00000 0.05737 0.04627 0.05341 0.01235 -0.00045 0.02483 0.05055 0.00866 0.00046 0.00039 0.00022 0.00000 0.00311 0.00292 0.00305 0.00257 0.00240 0.00253 0.00120 H33 0.01074 1.14152 0.09884 1.00000 0.06066 0.00000 0.00000 C34 0.22996 1.05841 0.12485 1.00000 0.04649 0.06217 0.04667 0.01754 0.00208 0.03284 0.04749 0.01074 0.00044 0.00046 0.00024 0.00000 0.00289 0.00340 0.00304 0.00277 0.00244 0.00269 0.00117 C35 0.31473 1.18303 0.15840 1.00000 0.05012 0.06162 0.05339 0.01022 0.00313 0.01493 0.05661 0.01046 0.00048 0.00046 0.00024 0.00000 0.00311 0.00351 0.00326 0.00303 0.00266 0.00278 0.00129 H35 0.29728 1.22178 0.20462 1.00000 0.06793 0.00000 0.00000 C36 0.42407 1.25178 0.12581 1.00000 0.05236 0.06974 0.08545 0.03295 0.00045 0.01315 0.06851 0.01152 0.00051 0.00049 0.00030 0.00000 0.00345 0.00389 0.00440 0.00374 0.00315 0.00297 0.00152 H36 0.48250 1.33705 0.15004 1.00000 0.08222 0.00000 0.00000 C37 0.45003 1.19873 0.05854 1.00000 0.06733 0.10083 0.08395 0.05270 0.02017 0.03404 0.07712 0.01448 0.00057 0.00060 0.00033 0.00000 0.00400 0.00512 0.00485 0.00444 0.00355 0.00381 0.00175 H37 0.52566 1.24637 0.03596 1.00000 0.09254 0.00000 0.00000 C38 0.36486 1.07631 0.02498 1.00000 0.08321 0.11361 0.05493 0.03226 0.02389 0.05106 0.07723 0.01389 0.00062 0.00061 0.00027 0.00000 0.00441 0.00520 0.00379 0.00413 0.00342 0.00401 0.00168 H38 0.38186 1.03860 -0.02153 1.00000 0.09267 0.00000 0.00000 C39 0.25432 1.00564 0.05697 1.00000 0.07251 0.06754 0.05436 0.01695 0.00776 0.03645 0.06124 0.01085 0.00052 0.00046 0.00026 0.00000 0.00372 0.00364 0.00348 0.00314 0.00288 0.00310 0.00136 H39 0.19527 0.92091 0.03226 1.00000 0.07348 0.00000 0.00000 Final Structure Factor Calculation for S965B IN P-1 Total number of l.s. parameters = 435 Maximum vector length = 511 Memory required = 5662 / 25039 wR2 = 0.0891 before cycle 23 for 6988 data and 0 / 435 parameters Disagreeable restraints before cycle 23 Observed Target Error Sigma Restraint -0.2186 0.0400 SIMU U33 C10 C11 -0.1293 0.0400 SIMU U22 C10 C12 Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 12. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.040 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.083 0.000 0.000 GooF = S = 0.749; Restrained GooF = 0.751 for 12 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0509 for 3246 Fo > 4sig(Fo) and 0.1189 for all 6988 data wR2 = 0.0891, GooF = S = 0.749, Restrained GooF = 0.751 for all data Occupancy sum of asymmetric unit = 47.00 for non-hydrogen and 53.00 for hydrogen atoms Principal mean square atomic displacements U 0.0530 0.0380 0.0339 Cu1 0.0576 0.0398 0.0341 P1 0.0633 0.0348 0.0232 N1 0.0998 0.0515 0.0322 N2 0.0633 0.0436 0.0345 N3 0.0873 0.0650 0.0353 N4 0.0540 0.0423 0.0311 N5 0.0653 0.0426 0.0364 Si1 0.0531 0.0353 0.0220 C1 0.0507 0.0462 0.0338 C2 0.0739 0.0673 0.0394 C3 0.0881 0.0726 0.0338 C4 0.0837 0.0618 0.0352 C5 0.0656 0.0484 0.0347 C6 0.1352 0.0550 0.0434 C7 0.2330 0.1430 0.0680 C8 0.2038 0.1203 0.0600 C9 0.0739 0.0568 0.0527 C10 0.2977 0.1083 0.0531 C11 may be split into 0.5992 0.7043 0.2001 and 0.5816 0.6885 0.1781 0.2389 0.1165 0.0544 C12 0.0496 0.0465 0.0349 C13 0.1958 0.0869 0.0353 C14 0.2072 0.0725 0.0491 C15 may be split into 0.4390 0.7414 0.3905 and 0.4243 0.7634 0.4028 0.0652 0.0397 0.0324 C16 0.1157 0.0969 0.0336 C17 0.1187 0.0854 0.0387 C18 0.0859 0.0689 0.0497 C19 0.0988 0.0663 0.0583 C20 0.1328 0.0741 0.0401 C21 0.0711 0.0430 0.0313 C22 0.1293 0.0521 0.0387 C23 0.2092 0.0585 0.0413 C24 may be split into -0.0485 0.5824 0.0729 and -0.0760 0.5917 0.0854 0.1847 0.0701 0.0386 C25 0.1525 0.0595 0.0407 C26 0.1088 0.0467 0.0399 C27 0.0550 0.0372 0.0347 C28 0.0622 0.0584 0.0493 C29 0.0982 0.0734 0.0468 C30 0.1315 0.0667 0.0364 C31 0.1059 0.0728 0.0376 C32 0.0640 0.0513 0.0363 C33 0.0678 0.0483 0.0264 C34 0.0666 0.0540 0.0492 C35 0.0956 0.0583 0.0516 C36 0.1171 0.0625 0.0518 C37 0.1187 0.0682 0.0448 C38 0.0807 0.0541 0.0490 C39 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.033 0.044 0.057 0.073 0.092 0.118 0.172 1.000 Number in group 700. 754. 696. 648. 724. 709. 681. 684. 689. 703. GooF 0.516 0.557 0.582 0.607 0.631 0.716 0.740 0.811 0.886 1.198 K 1.243 0.962 1.108 1.037 1.059 1.058 1.046 1.033 1.019 1.010 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.25 1.43 1.80 inf Number in group 722. 690. 689. 711. 681. 705. 691. 702. 694. 703. GooF 0.553 0.580 0.568 0.603 0.633 0.650 0.676 0.763 0.873 1.286 K 1.089 1.040 1.106 1.068 1.059 1.017 1.017 1.003 0.993 1.019 R1 0.313 0.264 0.215 0.187 0.160 0.129 0.100 0.070 0.050 0.037 Recommended weighting scheme: WGHT 0.0000 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 0 1 5343.39 4787.62 8.42 0.395 8.02 2 0 2 12446.94 11205.75 6.16 0.605 4.01 1 -3 3 7008.29 6427.83 5.98 0.458 3.51 3 -4 5 5473.94 4711.95 5.66 0.392 2.19 2 -2 9 515.73 376.98 4.91 0.111 1.98 -1 2 3 14320.80 15076.25 4.69 0.702 3.70 0 2 2 12187.70 11531.69 4.64 0.614 4.11 4 0 2 1062.85 789.21 4.47 0.161 2.20 2 -5 3 267.81 173.91 4.40 0.075 2.20 -3 5 0 3630.02 3310.01 4.34 0.329 2.05 -4 -1 2 1530.04 1370.08 4.33 0.212 2.13 4 -3 2 259.71 154.85 4.28 0.071 2.27 -3 -2 6 7489.76 6834.01 4.26 0.472 2.07 -2 -2 5 11053.57 11746.88 4.25 0.619 2.63 3 -6 6 3191.16 2688.56 4.23 0.296 1.70 2 -4 4 1622.20 1328.66 4.22 0.208 2.54 -2 2 4 1046.95 1272.49 4.17 0.204 2.97 0 0 3 1525.02 1305.28 4.10 0.206 6.31 2 -5 9 2710.57 2398.54 4.10 0.280 1.71 -1 -5 4 148.14 237.37 4.06 0.088 1.93 -2 4 2 169.49 295.84 4.01 0.098 2.42 -2 5 0 1871.97 1665.06 3.97 0.233 2.16 2 -4 6 3835.69 3413.58 3.92 0.334 2.27 0 1 1 630.49 728.26 3.92 0.154 8.22 -2 -1 1 1731.67 1395.19 3.91 0.213 3.84 -1 -1 1 1919.08 1759.81 3.91 0.240 6.08 -1 2 5 5257.14 5711.61 3.91 0.432 2.82 3 -2 7 748.26 856.79 3.85 0.167 2.11 2 -3 2 867.52 733.69 3.78 0.155 3.32 4 -6 5 1840.85 1467.69 3.77 0.219 1.63 3 -1 7 65.21 116.97 3.75 0.062 2.06 0 -4 5 832.37 718.37 3.73 0.153 2.44 1 -3 1 936.01 832.05 3.70 0.165 3.73 1 -2 6 1942.08 1626.75 3.65 0.230 2.99 -1 2 0 2290.67 2163.98 3.64 0.266 5.29 2 -4 7 5527.63 5060.28 3.61 0.406 2.12 3 -4 6 1081.21 840.30 3.53 0.166 2.08 0 -4 6 1004.89 902.18 3.52 0.172 2.30 -1 4 6 752.70 497.45 3.51 0.127 1.85 9 -9 1 290.09 26.51 3.50 0.029 0.93 1 -3 4 2349.12 2112.35 3.49 0.263 3.26 3 -4 8 6690.47 6133.50 3.48 0.448 1.84 2 -3 5 1052.66 857.99 3.48 0.167 2.75 6 -2 4 698.54 863.08 3.47 0.168 1.53 -1 -2 1 15026.90 15544.96 3.42 0.712 4.10 -2 1 5 5122.28 5499.87 3.37 0.424 2.96 -1 -9 3 260.10 397.14 3.36 0.114 1.13 1 1 2 7456.12 7805.07 3.30 0.505 4.64 0 4 3 1319.45 1092.85 3.29 0.189 2.20 3 1 7 2684.76 2944.79 3.29 0.310 1.79 Bond lengths and angles Cu1 - Distance Angles N5 1.9645 (0.0032) N1 1.9803 (0.0029) 95.88 (0.14) P1 2.1651 (0.0012) 126.26 (0.10) 135.59 (0.11) Cu1 - N5 N1 P1 - Distance Angles C22 1.8110 (0.0043) C28 1.8241 (0.0040) 100.94 (0.18) C34 1.8244 (0.0044) 105.50 (0.21) 103.48 (0.19) Cu1 2.1651 (0.0012) 122.58 (0.14) 119.03 (0.14) 103.22 (0.14) P1 - C22 C28 C34 N1 - Distance Angles C13 1.3280 (0.0047) C1 1.4090 (0.0045) 123.55 (0.34) Cu1 1.9803 (0.0029) 118.18 (0.28) 117.99 (0.24) N1 - C13 C1 N2 - Distance Angles C13 1.3795 (0.0045) C15 1.4033 (0.0049) 125.50 (0.39) C14 1.4570 (0.0051) 119.27 (0.38) 112.94 (0.38) N2 - C13 C15 N3 - Distance Angles C16 1.3348 (0.0047) C13 1.3491 (0.0047) 125.82 (0.37) N3 - C16 N4 - Distance Angles C16 1.3707 (0.0047) C17 1.4444 (0.0048) 123.61 (0.40) C18 1.4642 (0.0047) 120.53 (0.38) 114.13 (0.37) N4 - C16 C17 N5 - Distance Angles C16 1.3289 (0.0047) Si1 1.7015 (0.0034) 126.45 (0.29) Cu1 1.9645 (0.0031) 111.54 (0.27) 119.71 (0.19) N5 - C16 Si1 Si1 - Distance Angles N5 1.7015 (0.0034) C19 1.8533 (0.0042) 113.54 (0.19) C20 1.8541 (0.0041) 107.65 (0.19) 106.85 (0.21) C21 1.8645 (0.0040) 112.71 (0.20) 107.85 (0.20) 107.94 (0.22) Si1 - N5 C19 C20 C1 - Distance Angles C2 1.3873 (0.0051) C6 1.4038 (0.0051) 119.36 (0.41) N1 1.4090 (0.0045) 121.73 (0.38) 118.61 (0.39) C1 - C2 C6 C2 - Distance Angles C3 1.3795 (0.0052) C1 1.3873 (0.0051) 119.36 (0.42) C10 1.5123 (0.0053) 119.03 (0.43) 121.61 (0.41) C2 - C3 C1 C3 - Distance Angles C4 1.3700 (0.0056) C2 1.3795 (0.0052) 121.15 (0.46) H3 0.9500 119.43 119.43 C3 - C4 C2 C4 - Distance Angles C5 1.3559 (0.0056) C3 1.3700 (0.0056) 120.01 (0.48) H4 0.9500 120.00 120.00 C4 - C5 C3 C5 - Distance Angles C4 1.3559 (0.0056) C6 1.3864 (0.0055) 120.84 (0.46) H5 0.9500 119.58 119.58 C5 - C4 C6 C6 - Distance Angles C5 1.3864 (0.0054) C1 1.4038 (0.0051) 119.27 (0.43) C7 1.5311 (0.0058) 119.56 (0.43) 121.12 (0.42) C6 - C5 C1 C7 - Distance Angles C9 1.5101 (0.0063) C6 1.5311 (0.0058) 111.21 (0.47) C8 1.5326 (0.0064) 108.40 (0.45) 112.78 (0.42) H7 1.0000 108.10 108.10 108.10 C7 - C9 C6 C8 C8 - Distance Angles C7 1.5326 (0.0064) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C7 1.5101 (0.0063) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C11 1.4973 (0.0056) C12 1.5064 (0.0059) 110.31 (0.49) C2 1.5123 (0.0053) 113.07 (0.39) 109.73 (0.39) H10 1.0000 107.85 107.85 107.85 C10 - C11 C12 C2 C11 - Distance Angles C10 1.4973 (0.0056) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5064 (0.0059) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C13 - Distance Angles N1 1.3280 (0.0046) N3 1.3491 (0.0047) 124.60 (0.39) N2 1.3795 (0.0045) 122.74 (0.39) 112.45 (0.39) C13 - N1 N3 C14 - Distance Angles N2 1.4570 (0.0051) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - N2 H14A H14B C15 - Distance Angles N2 1.4033 (0.0049) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - N2 H15A H15B C16 - Distance Angles N5 1.3289 (0.0047) N3 1.3348 (0.0047) 127.77 (0.39) N4 1.3707 (0.0047) 121.09 (0.42) 111.11 (0.40) C16 - N5 N3 C17 - Distance Angles N4 1.4444 (0.0048) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - N4 H17A H17B C18 - Distance Angles N4 1.4642 (0.0047) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - N4 H18A H18B C19 - Distance Angles Si1 1.8533 (0.0041) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - Si1 H19A H19B C20 - Distance Angles Si1 1.8541 (0.0041) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - Si1 H20A H20B C21 - Distance Angles Si1 1.8645 (0.0040) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - Si1 H21A H21B C22 - Distance Angles C23 1.3838 (0.0051) C27 1.3900 (0.0051) 117.03 (0.43) P1 1.8110 (0.0043) 119.70 (0.33) 123.28 (0.36) C22 - C23 C27 C23 - Distance Angles C24 1.3692 (0.0059) C22 1.3838 (0.0051) 120.62 (0.43) H23 0.9500 119.69 119.69 C23 - C24 C22 C24 - Distance Angles C25 1.3650 (0.0061) C23 1.3692 (0.0059) 121.29 (0.50) H24 0.9500 119.35 119.35 C24 - C25 C23 C25 - Distance Angles C24 1.3650 (0.0061) C26 1.3693 (0.0059) 118.71 (0.52) H25 0.9500 120.65 120.65 C25 - C24 C26 C26 - Distance Angles C27 1.3571 (0.0056) C25 1.3693 (0.0059) 120.51 (0.46) H26 0.9500 119.74 119.74 C26 - C27 C25 C27 - Distance Angles C26 1.3571 (0.0056) C22 1.3900 (0.0051) 121.75 (0.44) H27 0.9500 119.12 119.12 C27 - C26 C22 C28 - Distance Angles C33 1.3799 (0.0048) C29 1.3923 (0.0053) 117.82 (0.39) P1 1.8241 (0.0039) 123.93 (0.36) 118.17 (0.32) C28 - C33 C29 C29 - Distance Angles C30 1.3635 (0.0054) C28 1.3923 (0.0053) 121.57 (0.44) H29 0.9500 119.21 119.21 C29 - C30 C28 C30 - Distance Angles C29 1.3635 (0.0054) C31 1.3681 (0.0060) 119.66 (0.50) H30 0.9500 120.17 120.17 C30 - C29 C31 C31 - Distance Angles C30 1.3681 (0.0060) C32 1.3817 (0.0062) 120.10 (0.48) H31 0.9500 119.95 119.95 C31 - C30 C32 C32 - Distance Angles C33 1.3714 (0.0052) C31 1.3817 (0.0062) 119.88 (0.46) H32 0.9500 120.06 120.06 C32 - C33 C31 C33 - Distance Angles C32 1.3714 (0.0052) C28 1.3799 (0.0048) 120.95 (0.45) H33 0.9500 119.52 119.52 C33 - C32 C28 C34 - Distance Angles C35 1.3781 (0.0054) C39 1.3783 (0.0053) 118.61 (0.44) P1 1.8244 (0.0044) 117.50 (0.37) 123.88 (0.41) C34 - C35 C39 C35 - Distance Angles C36 1.3722 (0.0054) C34 1.3781 (0.0053) 120.75 (0.47) H35 0.9500 119.62 119.62 C35 - C36 C34 C36 - Distance Angles C35 1.3722 (0.0054) C37 1.3741 (0.0062) 120.76 (0.53) H36 0.9500 119.62 119.62 C36 - C35 C37 C37 - Distance Angles C38 1.3617 (0.0064) C36 1.3741 (0.0062) 118.48 (0.54) H37 0.9500 120.76 120.76 C37 - C38 C36 C38 - Distance Angles C37 1.3617 (0.0064) C39 1.3816 (0.0058) 121.55 (0.54) H38 0.9500 119.22 119.22 C38 - C37 C39 C39 - Distance Angles C34 1.3783 (0.0053) C38 1.3816 (0.0058) 119.81 (0.50) H39 0.9500 120.09 120.09 C39 - C34 C38 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 5.3501 (0.0079) x + 0.0330 (0.0253) y + 16.5365 (0.0107) z = 3.3514 (0.0239) * 0.0000 (0.0000) N3 * 0.0000 (0.0000) Cu1 * 0.0000 (0.0000) N1 Rms deviation of fitted atoms = 0.0000 - 5.0979 (0.0289) x - 0.6054 (0.0279) y + 16.8595 (0.0343) z = 3.0116 (0.0169) Angle to previous plane (with approximate esd) = 3.30 ( 0.33 ) * -0.0959 (0.0025) N3 * 0.0954 (0.0025) C13 * 0.0439 (0.0012) C16 * -0.0434 (0.0011) N1 Rms deviation of fitted atoms = 0.0744 - 6.9346 (0.0431) x - 0.0945 (0.0214) y + 13.9648 (0.0923) z = 1.7814 (0.0658) Angle to previous plane (with approximate esd) = 14.16 ( 0.65 ) * 0.0000 (0.0001) C13 * 0.0000 (0.0000) N2 * 0.0000 (0.0000) C16 Rms deviation of fitted atoms = 0.0000 - 5.0979 (0.0289) x - 0.6054 (0.0279) y + 16.8595 (0.0343) z = 3.0116 (0.0169) Angle to previous plane (with approximate esd) = 14.16 ( 0.65 ) * -0.0959 (0.0025) N3 * 0.0954 (0.0025) C13 * 0.0439 (0.0012) C16 * -0.0434 (0.0011) N1 Rms deviation of fitted atoms = 0.0744 7.4689 (0.0061) x + 1.8507 (0.0166) y - 11.5571 (0.0119) z = 0.4832 (0.0162) Angle to previous plane (with approximate esd) = 26.47 ( 0.28 ) * 0.0000 (0.0000) N1 * 0.0000 (0.0000) N5 * 0.0000 (0.0000) P1 -0.1719 (0.0015) Cu1 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 44 GRID -1.220 -2 -2 1.220 2 2 R1 = 0.1155 for 6988 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.0978 0.9160 0.2534 [ 1.17 A from CU1 ] Deepest hole -0.24 at 0.0544 0.7048 0.4131 [ 0.50 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 5125 / 29407 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0978 0.9160 0.2534 1.00000 0.05 0.35 1.17 CU1 1.81 P1 2.15 H9B 2.53 N1 Q2 1 0.3383 1.0607 0.2822 1.00000 0.05 0.30 1.21 CU1 1.43 N5 1.76 C16 2.12 N1 Q3 1 0.2094 1.0562 0.3308 1.00000 0.05 0.26 1.16 N5 1.27 CU1 2.00 SI1 2.17 H20A Q4 1 0.1847 1.1064 0.2747 1.00000 0.05 0.26 1.45 CU1 1.71 N5 2.16 P1 2.18 H35 Q5 1 0.1871 0.9253 0.2093 1.00000 0.05 0.24 1.21 CU1 1.43 P1 2.27 H23 2.43 C22 Shortest distances between peaks (including symmetry equivalents) 1 5 1.24 3 4 1.39 2 3 1.59 2 4 1.75 1 3 1.93 1 4 1.97 2 5 2.01 4 5 2.14 1 2 2.37 3 5 2.45 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.06: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.68: Structure factors and derivatives 13.15: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.92: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + lx2294isup2 finished at 15:07:32 Total CPU time: 16.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++