+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1636sq started at 09:19:05 on 28-Feb-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in C2/c CELL 0.71073 31.7262 14.3868 23.1234 90.000 123.332 90.000 ZERR 4.00 0.0017 0.0007 0.0013 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O SI UNIT 140 392 28 108 32 V = 8818.21 F(000) = 2740.0 Mu = 0.18 mm-1 Cell Wt = 5095.70 Rho = 0.960 MERG 2 OMIT -3.00 55.00 OMIT 0 4 0 SHEL 7 0.77 EQIV $1 -X+2, Y, -Z+1/2 FREE C41 C45_$1 FREE C42 C45_$1 FREE C44 C44_$1 FREE C45 C42_$1 FREE C45 C41_$1 DELU SIMU htab FMAP 2 PLAN 10 SIZE 0.16 0.50 0.62 ACTA BOND $H BUMP -0.01000 WGHT 0.20000 L.S. 10 TEMP -153.00 FVAR 0.58702 MOLE 1 O1 4 0.848912 0.744574 0.069462 11.00000 0.02956 0.04440 = 0.02953 0.00912 0.01778 0.00791 O2 4 0.795288 0.588997 0.028166 11.00000 0.03343 0.04255 = 0.02550 -0.00012 0.01353 0.00770 O3 4 0.755045 0.662491 -0.095270 11.00000 0.04972 0.03296 = 0.02888 0.00192 0.02751 0.00245 O4 4 0.796281 0.827168 -0.051648 11.00000 0.03408 0.04721 = 0.02045 -0.00247 0.01605 -0.00123 O5 4 0.882743 0.899928 0.048131 11.00000 0.02814 0.04799 = 0.02795 -0.00208 0.01777 -0.00253 O6 4 0.881068 0.596604 0.150336 11.00000 0.02618 0.04520 = 0.02294 0.00785 0.01156 0.01280 O7 4 0.749421 0.481704 -0.082913 11.00000 0.04798 0.03315 = 0.03555 -0.00337 0.02904 0.00589 O8 4 0.750614 0.784345 -0.183699 11.00000 0.03502 0.04624 = 0.02095 0.00242 0.01988 0.00411 O9 4 0.803327 0.902899 0.057145 11.00000 0.03102 0.04020 = 0.03207 -0.00536 0.02108 0.00184 O10 4 0.802210 0.688387 0.128708 11.00000 0.03024 0.05210 = 0.02447 0.00499 0.01900 0.01001 SI1 5 0.833981 0.845234 0.031220 11.00000 0.02337 0.03752 = 0.01930 0.00009 0.01359 0.00196 SI2 5 0.832021 0.654463 0.094002 11.00000 0.02220 0.03964 = 0.01774 0.00348 0.01187 0.00783 SI3 5 0.749107 0.579880 -0.052561 11.00000 0.02920 0.03079 = 0.02028 -0.00055 0.01686 0.00460 SI4 5 0.750148 0.771673 -0.115953 11.00000 0.02543 0.03585 = 0.01598 0.00188 0.01405 0.00474 MOLE 2 C11 1 0.998987 0.876049 0.109223 11.00000 0.03653 0.34285 = 0.06110 0.05064 0.01451 -0.01086 AFIX 23 H11A 2 0.976519 0.922635 0.074132 11.00000 -1.20000 H11B 2 1.005333 0.827601 0.084486 11.00000 -1.20000 AFIX 0 C12 1 1.045952 0.921164 0.155060 11.00000 0.06257 0.16244 = 0.08271 0.06507 0.02205 0.00508 AFIX 23 H12A 2 1.038184 0.980013 0.169529 11.00000 -1.20000 H12B 2 1.059832 0.938494 0.127267 11.00000 -1.20000 AFIX 0 C13 1 1.133058 0.925094 0.252864 11.00000 0.09003 0.27821 = 0.09823 0.00218 0.02378 -0.09687 AFIX 33 H13A 2 1.157994 0.890027 0.294092 11.00000 -1.50000 H13B 2 1.128272 0.986522 0.266731 11.00000 -1.50000 H13C 2 1.145059 0.932361 0.222081 11.00000 -1.50000 AFIX 0 C14 1 1.072862 0.852111 0.268441 11.00000 0.06116 0.25180 = 0.04781 0.04975 0.01515 -0.01151 AFIX 33 H14A 2 1.040934 0.817767 0.244474 11.00000 -1.50000 H14B 2 1.069123 0.909126 0.288412 11.00000 -1.50000 H14C 2 1.099443 0.813394 0.305435 11.00000 -1.50000 AFIX 0 C15 1 1.103370 0.787024 0.204243 11.00000 0.34065 0.15334 = 0.15041 0.03023 0.11985 0.12448 AFIX 33 H15A 2 1.074484 0.744745 0.179681 11.00000 -1.50000 H15B 2 1.129498 0.758868 0.248276 11.00000 -1.50000 H15C 2 1.117029 0.798516 0.175812 11.00000 -1.50000 AFIX 0 N11 3 1.086786 0.876698 0.217873 11.00000 0.03934 0.07648 = 0.03371 0.00990 0.00932 -0.00460 O11 4 0.971371 0.833944 0.132668 11.00000 0.02434 0.10822 = 0.04668 0.00056 0.01026 0.00328 AFIX 147 H11 2 0.943083 0.817431 0.098592 11.00000 -1.50000 AFIX 0 MOLE 3 same C11 > O11 C21 1 0.710424 0.329892 0.174122 11.00000 0.13073 0.18103 = 0.08122 0.04432 0.07144 0.01179 AFIX 23 H21A 2 0.689296 0.385502 0.151171 11.00000 -1.20000 H21B 2 0.688076 0.280114 0.172024 11.00000 -1.20000 AFIX 0 C22 1 0.732797 0.298806 0.134390 11.00000 0.15774 0.08448 = 0.06414 0.00816 0.06895 -0.01600 AFIX 23 H22A 2 0.761596 0.257044 0.164350 11.00000 -1.20000 H22B 2 0.707142 0.262059 0.093944 11.00000 -1.20000 AFIX 0 C23 1 0.719586 0.452238 0.076185 11.00000 0.30036 0.11818 = 0.13835 0.06912 0.15434 0.09295 AFIX 33 H23A 2 0.736771 0.495387 0.062923 11.00000 -1.50000 H23B 2 0.712619 0.483547 0.107714 11.00000 -1.50000 H23C 2 0.687771 0.431930 0.034694 11.00000 -1.50000 AFIX 0 C24 1 0.767869 0.338411 0.064934 11.00000 0.30709 0.13450 = 0.15334 0.01999 0.19263 0.03165 AFIX 33 H24A 2 0.789996 0.284663 0.087489 11.00000 -1.50000 H24B 2 0.786397 0.387297 0.058410 11.00000 -1.50000 H24C 2 0.738509 0.319674 0.019832 11.00000 -1.50000 AFIX 0 C25 1 0.795610 0.420083 0.170891 11.00000 0.15641 0.15220 = 0.14550 -0.03693 0.11550 -0.05827 AFIX 33 H25A 2 0.821060 0.372791 0.198980 11.00000 -1.50000 H25B 2 0.785261 0.451271 0.198850 11.00000 -1.50000 H25C 2 0.809896 0.465870 0.154895 11.00000 -1.50000 AFIX 0 N21 3 0.750559 0.374579 0.109490 11.00000 0.12252 0.05105 = 0.05031 0.00532 0.05651 0.00006 O21 4 0.747275 0.351928 0.245909 11.00000 0.18120 0.06507 = 0.07616 0.00803 0.10101 -0.00693 AFIX 147 H21 2 0.751332 0.305704 0.270668 11.00000 -1.50000 AFIX 0 MOLE 4 SAME C11 > O11 C31 1 1.002369 0.624210 0.047805 11.00000 0.08588 0.41704 = 0.39556 -0.08437 -0.03524 0.04450 AFIX 23 H31A 2 1.032816 0.630598 0.046284 11.00000 -1.20000 H31B 2 0.996679 0.686029 0.061154 11.00000 -1.20000 AFIX 0 C32 1 0.959826 0.610486 -0.025248 11.00000 0.09145 0.35262 = 0.30257 -0.07904 0.11158 0.03990 AFIX 23 H32A 2 0.965764 0.655256 -0.052564 11.00000 -1.20000 H32B 2 0.965022 0.547970 -0.038202 11.00000 -1.20000 AFIX 0 C33 1 0.897896 0.696994 -0.024749 11.00000 0.09242 0.27882 = 0.21847 -0.19276 0.07414 -0.02819 AFIX 33 H33A 2 0.861923 0.703096 -0.042855 11.00000 -1.50000 H33B 2 0.909261 0.752083 -0.037434 11.00000 -1.50000 H33C 2 0.917145 0.691326 0.025775 11.00000 -1.50000 AFIX 0 C34 1 0.866583 0.621478 -0.131063 11.00000 0.25934 0.24467 = 0.08596 -0.06642 0.02534 -0.01963 AFIX 33 H34A 2 0.870602 0.567994 -0.153871 11.00000 -1.50000 H34B 2 0.871329 0.679050 -0.149474 11.00000 -1.50000 H34C 2 0.832659 0.620724 -0.139797 11.00000 -1.50000 AFIX 0 C35 1 0.887288 0.545087 -0.025722 11.00000 0.32972 0.36737 = 0.39681 0.17973 0.16347 -0.10760 AFIX 33 H35A 2 0.890140 0.483258 -0.041055 11.00000 -1.50000 H35B 2 0.851915 0.557576 -0.042824 11.00000 -1.50000 H35C 2 0.907688 0.547501 0.024971 11.00000 -1.50000 AFIX 0 N31 3 0.905683 0.616298 -0.053430 11.00000 0.04868 0.06909 = 0.07633 0.00122 0.04042 0.01844 O31 4 1.017177 0.564045 0.106318 11.00000 0.09674 0.39677 = 0.30639 -0.14327 -0.05885 0.07505 AFIX 147 H31 2 0.993732 0.526507 0.095848 11.00000 -1.50000 AFIX 0 MOLE 5 SAME C11 > O11 C41 1 0.915454 0.377141 0.180556 10.50000 0.09179 0.09582 = 0.09513 0.04665 0.04874 0.03444 AFIX 23 H41A 2 0.888448 0.338100 0.177065 10.50000 -1.20000 H41B 2 0.926195 0.421321 0.219081 10.50000 -1.20000 AFIX 0 C42 1 0.958744 0.315795 0.200580 10.50000 0.09491 0.20371 = 0.12972 0.08697 0.04598 0.07406 AFIX 23 H42A 2 0.973523 0.296183 0.249100 10.50000 -1.20000 H42B 2 0.945561 0.259195 0.171548 10.50000 -1.20000 AFIX 0 C43 1 0.980740 0.362282 0.122473 10.50000 0.13151 0.49941 = 0.27558 0.19641 0.15946 0.17094 AFIX 33 H43A 2 1.008023 0.384151 0.117886 10.50000 -1.50000 H43B 2 0.953005 0.407314 0.100991 10.50000 -1.50000 H43C 2 0.968540 0.301974 0.099395 10.50000 -1.50000 AFIX 0 C44 1 1.009143 0.454041 0.216890 10.50000 0.28149 0.30634 = 0.45417 0.06911 0.11506 -0.06273 AFIX 33 H44A 2 1.023545 0.459005 0.266659 10.50000 -1.50000 H44B 2 0.977267 0.488453 0.191275 10.50000 -1.50000 H44C 2 1.032819 0.480192 0.206547 10.50000 -1.50000 AFIX 0 C45 1 1.045363 0.302343 0.217513 10.50000 0.13079 0.47322 = 0.42166 0.30194 0.15080 0.13585 AFIX 33 H45A 2 1.063651 0.290407 0.267377 10.50000 -1.50000 H45B 2 1.066549 0.339433 0.207527 10.50000 -1.50000 H45C 2 1.037030 0.243117 0.192600 10.50000 -1.50000 AFIX 0 N41 3 0.999534 0.352486 0.195488 10.50000 0.10197 0.29771 = 0.22920 0.10875 0.08094 0.05709 O41 4 0.894307 0.428266 0.120504 10.50000 0.07086 0.04986 = 0.04057 0.00150 0.02139 0.02193 AFIX 147 H41 2 0.889169 0.393633 0.087983 10.50000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s93 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 O1 - Si2 Si1 O2 - Si2 Si3 O3 - Si3 Si4 O4 - Si4 Si1 O5 - Si1 O6 - Si2 O7 - Si3 O8 - Si4 O9 - Si1 Si3_$2 O10 - Si2 Si4_$2 Si1 - O5 O9 O1 O4 Si2 - O6 O10 O2 O1 Si3 - O7 O3 O2 O9_$2 Si4 - O8 O4 O10_$2 O3 C11 - O11 C12 C12 - C11 N11 C13 - N11 C14 - N11 C15 - N11 N11 - C13 C12 C15 C14 O11 - C11 C21 - O21 C22 C22 - N21 C21 C23 - N21 C24 - N21 C25 - N21 N21 - C23 C22 C24 C25 O21 - C21 C31 - O31 C32 C32 - N31 C31 C33 - N31 C34 - N31 C35 - N31 N31 - C33 C32 C35 C34 O31 - C31 C41 - O41 C42 C42 - N41 C41 C43 - N41 C44 - N41 C45 - N41 N41 - C45 C43 C42 C44 O41 - C41 Operators for generating equivalent atoms: $1 -x+2, y, -z+1/2 $2 -x+3/2, -y+3/2, -z 75813 Reflections read, of which 68 rejected -41 =< h =< 41, -18 =< k =< 18, -30 =< l =< 30, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 2 0 11062.81 40.58 10 649.73 14 2 0 729.64 4.01 13 34.55 4 4 0 3305.89 25.09 15 198.01 1 5 0 411.65 4.40 14 28.84 -5 1 1 2969.20 1.69 14 20.67 3 1 1 6067.01 3.15 16 21.27 5 1 1 2623.23 2.69 15 15.76 -2 2 1 822.43 5.00 10 82.28 0 2 1 100421.02 64.44 7 1386.88 -9 3 1 922.17 3.44 9 32.99 -2 4 1 4402.29 7.88 15 51.74 0 4 1 1127.12 3.30 11 20.50 9 5 1 771.78 5.21 10 27.12 -4 6 1 1645.99 4.49 9 48.67 -6 0 2 9892.57 9.18 6 54.34 14 0 2 2757.44 5.94 7 43.06 1 1 2 14353.23 3.54 2 102.50 5 1 2 13052.19 9.67 16 51.12 -4 2 2 7689.66 15.72 13 93.63 0 2 2 5080.73 5.98 9 30.26 7 3 2 1977.49 2.99 14 21.44 6 4 2 3595.31 2.25 14 44.42 -7 5 2 1488.52 2.77 13 31.65 -11 1 3 2638.80 5.40 9 36.17 -3 1 3 2096.42 34.07 4 172.05 -1 1 3 16818.60 62.29 9 658.67 -10 2 3 3198.24 4.11 9 25.58 -4 2 3 2591.35 2.27 13 23.72 -2 2 3 2172.23 5.08 14 27.76 6 2 3 403.36 2.66 15 16.32 8 2 3 4637.55 3.83 13 20.26 -15 3 3 636.37 6.30 7 54.73 -3 3 3 9453.46 3.06 7 173.41 -9 5 3 3693.56 5.06 12 40.32 9 5 3 1867.82 4.96 10 31.45 -4 6 3 518.88 4.18 10 25.93 6 12 3 20.50 22.51 4 170.75 -11 1 4 1852.15 6.40 7 48.96 3 1 4 6701.22 2.94 13 33.65 5 1 4 469.29 3.59 13 26.80 7 1 4 3603.59 3.99 12 21.73 8 2 4 624.84 3.47 13 21.18 9 3 4 4754.50 4.90 12 106.68 -8 4 4 341.19 4.12 9 29.90 2 6 4 804.31 5.59 12 29.52 -9 7 4 389.77 2.74 10 19.78 -9 3 5 8354.71 5.42 11 51.05 -2 4 5 1445.60 3.87 10 22.87 2 4 5 3183.49 2.65 11 19.16 -12 10 5 638.28 8.96 7 48.33 ** etc. ** 87 Inconsistent equivalents 10096 Unique reflections, of which 0 suppressed R(int) = 0.0461 R(sigma) = 0.0320 Friedel opposites merged Maximum memory for data reduction = 5328 / 124108 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 = 6548 / 489745 wR2 = 0.3165 before cycle 1 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0803 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1281 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.010 for x Si3 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C44 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 2 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0803 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.004 for U23 Si2 Max. shift = 0.000 A for H31 Max. dU = 0.000 for C44 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 3 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0803 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x Si2 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C44 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 4 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0803 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H11 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C35 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 5 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H21 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C44 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 6 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for x C23 Max. shift = 0.000 A for C23 Max. dU = 0.000 for C44 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 7 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0803 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1667 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for x C23 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C44 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 8 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for y C35 Max. shift = 0.000 A for H31 Max. dU = 0.000 for C44 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 9 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.004 for x C23 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C44 Least-squares cycle 10 Maximum vector length = 511 Memory required = 6548 / 489745 wR2 = 0.3165 before cycle 10 for 10096 data and 383 / 383 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1667 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58702 0.00234 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for x C23 Max. shift = 0.000 A for H31 Max. dU = 0.000 for C44 Largest correlation matrix elements 0.887 U13 C24 / U11 C24 0.796 U13 N41 / U11 N41 0.738 U12 C23 / U23 C23 -0.882 y C43 / tors H31 -0.795 U23 C33 / U33 C33 0.737 U13 C25 / U33 C25 0.878 U13 C24 / U33 C24 0.794 U13 C45 / U11 C45 0.734 z C23 / x C23 0.849 z C24 / x C24 0.774 U33 N41 / U33 C43 0.724 y C35 / y C33 0.846 U13 C43 / U11 C43 0.763 z O21 / x O21 0.723 U13 C21 / U11 C21 0.836 U12 C24 / U23 C24 0.763 U13 C43 / U33 C43 0.723 U13 C22 / U33 C22 0.807 U13 O21 / U11 O21 0.746 U12 O21 / U23 O21 0.723 y N41 / y C44 0.804 U13 O21 / U33 O21 0.738 U13 C23 / U33 C23 0.720 U23 C45 / U33 C45 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H11A 0.9765 0.9226 0.0741 23 0.990 0.000 C11 O11 C12 H11B 1.0053 0.8276 0.0845 23 0.990 0.000 C11 O11 C12 H12A 1.0382 0.9800 0.1695 23 0.990 0.000 C12 C11 N11 H12B 1.0598 0.9385 0.1273 23 0.990 0.000 C12 C11 N11 H13A 1.1580 0.8900 0.2941 33 0.980 0.000 C13 N11 H13A H13B 1.1283 0.9865 0.2667 33 0.980 0.000 C13 N11 H13A H13C 1.1451 0.9324 0.2221 33 0.980 0.000 C13 N11 H13A H14A 1.0409 0.8178 0.2445 33 0.980 0.000 C14 N11 H14A H14B 1.0691 0.9091 0.2884 33 0.980 0.000 C14 N11 H14A H14C 1.0994 0.8134 0.3054 33 0.980 0.000 C14 N11 H14A H15A 1.0745 0.7447 0.1797 33 0.980 0.000 C15 N11 H15A H15B 1.1295 0.7589 0.2483 33 0.980 0.000 C15 N11 H15A H15C 1.1170 0.7985 0.1758 33 0.980 0.000 C15 N11 H15A H11 0.9431 0.8174 0.0986 147 0.840 0.000 O11 C11 H11 H21A 0.6893 0.3855 0.1512 23 0.990 0.000 C21 O21 C22 H21B 0.6881 0.2801 0.1720 23 0.990 0.000 C21 O21 C22 H22A 0.7616 0.2570 0.1643 23 0.990 0.000 C22 N21 C21 H22B 0.7071 0.2621 0.0939 23 0.990 0.000 C22 N21 C21 H23A 0.7368 0.4954 0.0629 33 0.980 0.000 C23 N21 H23A H23B 0.7126 0.4835 0.1077 33 0.980 0.000 C23 N21 H23A H23C 0.6878 0.4319 0.0347 33 0.980 0.000 C23 N21 H23A H24A 0.7900 0.2847 0.0875 33 0.980 0.000 C24 N21 H24A H24B 0.7864 0.3873 0.0584 33 0.980 0.000 C24 N21 H24A H24C 0.7385 0.3197 0.0198 33 0.980 0.000 C24 N21 H24A H25A 0.8211 0.3728 0.1990 33 0.980 0.000 C25 N21 H25A H25B 0.7853 0.4513 0.1989 33 0.980 0.000 C25 N21 H25A H25C 0.8099 0.4659 0.1549 33 0.980 0.000 C25 N21 H25A H21 0.7513 0.3057 0.2707 147 0.840 0.000 O21 C21 H21 H31A 1.0328 0.6306 0.0463 23 0.990 0.000 C31 O31 C32 H31B 0.9967 0.6860 0.0612 23 0.990 0.000 C31 O31 C32 H32A 0.9658 0.6553 -0.0526 23 0.990 0.000 C32 N31 C31 H32B 0.9650 0.5480 -0.0382 23 0.990 0.000 C32 N31 C31 H33A 0.8619 0.7031 -0.0429 33 0.980 0.000 C33 N31 H33A H33B 0.9093 0.7521 -0.0374 33 0.980 0.000 C33 N31 H33A H33C 0.9171 0.6913 0.0258 33 0.980 0.000 C33 N31 H33A H34A 0.8706 0.5680 -0.1539 33 0.980 0.000 C34 N31 H34A H34B 0.8713 0.6790 -0.1495 33 0.980 0.000 C34 N31 H34A H34C 0.8327 0.6207 -0.1398 33 0.980 0.000 C34 N31 H34A H35A 0.8901 0.4833 -0.0411 33 0.980 0.000 C35 N31 H35A H35B 0.8519 0.5576 -0.0428 33 0.980 0.000 C35 N31 H35A H35C 0.9077 0.5475 0.0250 33 0.980 0.000 C35 N31 H35A H31 0.9937 0.5265 0.0958 147 0.840 0.000 O31 C31 H31 H41A 0.8884 0.3381 0.1771 23 0.990 0.000 C41 O41 C42 H41B 0.9262 0.4213 0.2191 23 0.990 0.000 C41 O41 C42 H42A 0.9735 0.2962 0.2491 23 0.990 0.000 C42 N41 C41 H42B 0.9456 0.2592 0.1715 23 0.990 0.000 C42 N41 C41 H43A 1.0080 0.3842 0.1179 33 0.980 0.000 C43 N41 H43A H43B 0.9530 0.4073 0.1010 33 0.980 0.000 C43 N41 H43A H43C 0.9685 0.3020 0.0994 33 0.980 0.000 C43 N41 H43A H44A 1.0235 0.4590 0.2667 33 0.980 0.000 C44 N41 H44A H44B 0.9773 0.4885 0.1913 33 0.980 0.000 C44 N41 H44A H44C 1.0328 0.4802 0.2065 33 0.980 0.000 C44 N41 H44A H45A 1.0637 0.2904 0.2674 33 0.980 0.000 C45 N41 H45A H45B 1.0665 0.3394 0.2075 33 0.980 0.000 C45 N41 H45A H45C 1.0370 0.2431 0.1926 33 0.980 0.000 C45 N41 H45A H41 0.8892 0.3936 0.0880 147 0.840 0.000 O41 C41 H41 s93 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.84891 0.74457 0.06946 1.00000 0.02956 0.04440 0.02953 0.00912 0.01778 0.00791 0.03369 0.00563 0.00008 0.00018 0.00012 0.00000 0.00113 0.00136 0.00116 0.00098 0.00097 0.00096 0.00053 O2 0.79529 0.58900 0.02817 1.00000 0.03343 0.04255 0.02550 -0.00012 0.01353 0.00770 0.03522 0.00559 0.00009 0.00017 0.00012 0.00000 0.00119 0.00138 0.00112 0.00095 0.00096 0.00100 0.00056 O3 0.75505 0.66249 -0.09527 1.00000 0.04972 0.03296 0.02888 0.00192 0.02751 0.00245 0.03408 0.00570 0.00010 0.00016 0.00012 0.00000 0.00145 0.00125 0.00118 0.00091 0.00112 0.00101 0.00055 O4 0.79628 0.82717 -0.05165 1.00000 0.03408 0.04721 0.02045 -0.00247 0.01605 -0.00123 0.03335 0.00527 0.00009 0.00017 0.00011 0.00000 0.00119 0.00139 0.00104 0.00094 0.00094 0.00101 0.00054 O5 0.88274 0.89993 0.04813 1.00000 0.02814 0.04799 0.02795 -0.00208 0.01777 -0.00253 0.03345 0.00526 0.00008 0.00017 0.00012 0.00000 0.00111 0.00142 0.00114 0.00098 0.00096 0.00099 0.00054 O6 0.88107 0.59660 0.15034 1.00000 0.02618 0.04520 0.02294 0.00785 0.01156 0.01280 0.03246 0.00549 0.00008 0.00017 0.00011 0.00000 0.00106 0.00137 0.00107 0.00093 0.00089 0.00096 0.00054 O7 0.74942 0.48170 -0.08291 1.00000 0.04798 0.03315 0.03555 -0.00337 0.02904 0.00589 0.03570 0.00583 0.00010 0.00017 0.00012 0.00000 0.00138 0.00124 0.00125 0.00097 0.00113 0.00105 0.00055 O8 0.75061 0.78434 -0.18370 1.00000 0.03502 0.04624 0.02095 0.00242 0.01988 0.00411 0.03171 0.00529 0.00008 0.00017 0.00011 0.00000 0.00117 0.00142 0.00105 0.00092 0.00094 0.00101 0.00053 O9 0.80333 0.90290 0.05714 1.00000 0.03102 0.04020 0.03207 -0.00536 0.02108 0.00184 0.03247 0.00530 0.00009 0.00017 0.00012 0.00000 0.00113 0.00133 0.00118 0.00095 0.00098 0.00095 0.00053 O10 0.80221 0.68839 0.12871 1.00000 0.03024 0.05210 0.02448 0.00499 0.01900 0.01001 0.03352 0.00556 0.00008 0.00019 0.00011 0.00000 0.00113 0.00146 0.00110 0.00098 0.00096 0.00102 0.00054 Si1 0.83398 0.84523 0.03122 1.00000 0.02337 0.03752 0.01930 0.00009 0.01359 0.00196 0.02575 0.00194 0.00003 0.00006 0.00004 0.00000 0.00043 0.00052 0.00043 0.00031 0.00035 0.00033 0.00025 Si2 0.83202 0.65446 0.09400 1.00000 0.02220 0.03964 0.01774 0.00348 0.01187 0.00783 0.02606 0.00196 0.00003 0.00006 0.00004 0.00000 0.00042 0.00054 0.00042 0.00031 0.00034 0.00033 0.00026 Si3 0.74911 0.57988 -0.05256 1.00000 0.02920 0.03079 0.02028 -0.00055 0.01686 0.00460 0.02504 0.00196 0.00003 0.00006 0.00004 0.00000 0.00045 0.00049 0.00043 0.00031 0.00035 0.00033 0.00025 Si4 0.75015 0.77167 -0.11595 1.00000 0.02543 0.03585 0.01598 0.00188 0.01405 0.00474 0.02435 0.00190 0.00003 0.00006 0.00004 0.00000 0.00043 0.00051 0.00040 0.00030 0.00034 0.00032 0.00025 C11 0.99899 0.87605 0.10922 1.00000 0.03653 0.34285 0.06110 0.05064 0.01451 -0.01086 0.15329 0.01625 0.00021 0.00073 0.00034 0.00000 0.00273 0.01341 0.00376 0.00586 0.00251 0.00480 0.00441 H11A 0.97652 0.92264 0.07413 1.00000 0.18394 0.00000 0.00000 H11B 1.00533 0.82760 0.08449 1.00000 0.18394 0.00000 0.00000 C12 1.04595 0.92116 0.15506 1.00000 0.06257 0.16243 0.08271 0.06507 0.02205 0.00508 0.11194 0.01713 0.00023 0.00061 0.00037 0.00000 0.00323 0.00677 0.00425 0.00457 0.00299 0.00360 0.00278 H12A 1.03818 0.98001 0.16953 1.00000 0.13433 0.00000 0.00000 H12B 1.05983 0.93849 0.12727 1.00000 0.13433 0.00000 0.00000 C13 1.13306 0.92509 0.25286 1.00000 0.09003 0.27821 0.09823 0.00218 0.02378 -0.09687 0.17015 0.01741 0.00032 0.00090 0.00048 0.00000 0.00526 0.01184 0.00618 0.00697 0.00436 0.00713 0.00479 H13A 1.15799 0.89003 0.29409 1.00000 0.25523 0.00000 0.00000 H13B 1.12827 0.98652 0.26673 1.00000 0.25523 0.00000 0.00000 H13C 1.14506 0.93236 0.22208 1.00000 0.25523 0.00000 0.00000 C14 1.07286 0.85211 0.26844 1.00000 0.06116 0.25180 0.04781 0.04975 0.01515 -0.01151 0.12801 0.01747 0.00024 0.00073 0.00031 0.00000 0.00351 0.01082 0.00316 0.00466 0.00267 0.00478 0.00355 H14A 1.04093 0.81777 0.24447 1.00000 0.19202 0.00000 0.00000 H14B 1.06912 0.90913 0.28841 1.00000 0.19202 0.00000 0.00000 H14C 1.09944 0.81339 0.30543 1.00000 0.19202 0.00000 0.00000 C15 1.10337 0.78702 0.20424 1.00000 0.34065 0.15334 0.15041 0.03023 0.11985 0.12448 0.22271 0.03566 0.00061 0.00077 0.00065 0.00000 0.01903 0.00866 0.01114 0.00688 0.01136 0.00915 0.00692 H15A 1.07448 0.74475 0.17968 1.00000 0.33406 0.00000 0.00000 H15B 1.12950 0.75887 0.24828 1.00000 0.33406 0.00000 0.00000 H15C 1.11703 0.79852 0.17581 1.00000 0.33406 0.00000 0.00000 N11 1.08679 0.87670 0.21787 1.00000 0.03934 0.07648 0.03371 0.00990 0.00932 -0.00460 0.05548 0.00817 0.00013 0.00030 0.00017 0.00000 0.00173 0.00255 0.00172 0.00164 0.00139 0.00170 0.00094 O11 0.97137 0.83394 0.13267 1.00000 0.02434 0.10822 0.04668 0.00056 0.01026 0.00328 0.06460 0.00721 0.00010 0.00028 0.00016 0.00000 0.00128 0.00285 0.00177 0.00171 0.00125 0.00148 0.00095 H11 0.94308 0.81743 0.09859 1.00000 0.09690 0.00000 0.00000 C21 0.71042 0.32989 0.17412 1.00000 0.13073 0.18103 0.08122 0.04432 0.07145 0.01179 0.12406 0.01964 0.00032 0.00067 0.00036 0.00000 0.00650 0.00809 0.00425 0.00487 0.00443 0.00576 0.00290 H21A 0.68930 0.38550 0.15117 1.00000 0.14887 0.00000 0.00000 H21B 0.68808 0.28011 0.17202 1.00000 0.14887 0.00000 0.00000 C22 0.73280 0.29881 0.13439 1.00000 0.15774 0.08448 0.06414 0.00816 0.06895 -0.01600 0.09793 0.01741 0.00033 0.00045 0.00033 0.00000 0.00638 0.00410 0.00348 0.00298 0.00402 0.00408 0.00214 H22A 0.76160 0.25704 0.16435 1.00000 0.11751 0.00000 0.00000 H22B 0.70714 0.26206 0.09394 1.00000 0.11751 0.00000 0.00000 C23 0.71959 0.45224 0.07618 1.00000 0.30036 0.11818 0.13834 0.06912 0.15434 0.09294 0.16788 0.02981 0.00046 0.00058 0.00053 0.00000 0.01227 0.00665 0.00713 0.00591 0.00770 0.00794 0.00455 H23A 0.73677 0.49539 0.06292 1.00000 0.25183 0.00000 0.00000 H23B 0.71262 0.48355 0.10771 1.00000 0.25183 0.00000 0.00000 H23C 0.68777 0.43193 0.03469 1.00000 0.25183 0.00000 0.00000 C24 0.76787 0.33841 0.06493 1.00000 0.30709 0.13450 0.15334 0.01999 0.19263 0.03165 0.16361 0.03129 0.00053 0.00068 0.00056 0.00000 0.01470 0.00765 0.00811 0.00571 0.01015 0.00769 0.00463 H24A 0.79000 0.28466 0.08749 1.00000 0.24541 0.00000 0.00000 H24B 0.78640 0.38730 0.05841 1.00000 0.24541 0.00000 0.00000 H24C 0.73851 0.31967 0.01983 1.00000 0.24541 0.00000 0.00000 C25 0.79561 0.42008 0.17089 1.00000 0.15641 0.15220 0.14550 -0.03693 0.11550 -0.05827 0.13429 0.01957 0.00036 0.00071 0.00048 0.00000 0.00698 0.00765 0.00688 0.00560 0.00578 0.00577 0.00309 H25A 0.82106 0.37279 0.19898 1.00000 0.20143 0.00000 0.00000 H25B 0.78526 0.45127 0.19885 1.00000 0.20143 0.00000 0.00000 H25C 0.80990 0.46587 0.15489 1.00000 0.20143 0.00000 0.00000 N21 0.75056 0.37458 0.10949 1.00000 0.12252 0.05105 0.05031 0.00532 0.05651 0.00006 0.06989 0.01110 0.00020 0.00028 0.00021 0.00000 0.00387 0.00226 0.00221 0.00172 0.00248 0.00227 0.00125 O21 0.74727 0.35193 0.24591 1.00000 0.18120 0.06507 0.07616 0.00803 0.10101 -0.00693 0.09157 0.01163 0.00022 0.00026 0.00022 0.00000 0.00475 0.00229 0.00254 0.00186 0.00311 0.00256 0.00150 H21 0.75133 0.30571 0.27067 1.00000 0.13736 0.00000 0.00000 C31 1.00237 0.62421 0.04780 1.00000 0.08588 0.41704 0.39556 -0.08437 -0.03524 0.04450 0.38740 0.02772 0.00050 0.00091 0.00087 0.00000 0.00816 0.02379 0.02026 0.01721 0.01105 0.01309 0.01279 H31A 1.03282 0.63060 0.04628 1.00000 0.46488 0.00000 0.00000 H31B 0.99668 0.68603 0.06115 1.00000 0.46488 0.00000 0.00000 C32 0.95983 0.61049 -0.02525 1.00000 0.09145 0.35262 0.30257 -0.07904 0.11158 0.03990 0.24713 0.02994 0.00033 0.00120 0.00076 0.00000 0.00533 0.01679 0.01291 0.01318 0.00693 0.00843 0.00665 H32A 0.96576 0.65526 -0.05256 1.00000 0.29656 0.00000 0.00000 H32B 0.96502 0.54797 -0.03820 1.00000 0.29656 0.00000 0.00000 C33 0.89790 0.69699 -0.02475 1.00000 0.09242 0.27882 0.21847 -0.19276 0.07414 -0.02819 0.20249 0.01910 0.00034 0.00080 0.00060 0.00000 0.00535 0.01125 0.01125 0.01035 0.00683 0.00710 0.00623 H33A 0.86192 0.70310 -0.04286 1.00000 0.30373 0.00000 0.00000 H33B 0.90926 0.75208 -0.03743 1.00000 0.30373 0.00000 0.00000 H33C 0.91715 0.69133 0.02577 1.00000 0.30373 0.00000 0.00000 C34 0.86658 0.62148 -0.13106 1.00000 0.25934 0.24467 0.08596 -0.06642 0.02534 -0.01963 0.23314 0.02573 0.00058 0.00097 0.00048 0.00000 0.01288 0.01497 0.00573 0.00728 0.00710 0.01209 0.00722 H34A 0.87060 0.56799 -0.15387 1.00000 0.34972 0.00000 0.00000 H34B 0.87133 0.67905 -0.14947 1.00000 0.34972 0.00000 0.00000 H34C 0.83266 0.62072 -0.13980 1.00000 0.34972 0.00000 0.00000 C35 0.88729 0.54509 -0.02572 1.00000 0.32972 0.36736 0.39681 0.17972 0.16347 -0.10760 0.38360 0.04828 0.00082 0.00103 0.00110 0.00000 0.02249 0.01714 0.02421 0.02162 0.02251 0.02047 0.01391 H35A 0.89014 0.48326 -0.04105 1.00000 0.57540 0.00000 0.00000 H35B 0.85191 0.55758 -0.04282 1.00000 0.57540 0.00000 0.00000 H35C 0.90769 0.54750 0.02497 1.00000 0.57540 0.00000 0.00000 N31 0.90568 0.61630 -0.05343 1.00000 0.04868 0.06909 0.07633 0.00122 0.04042 0.01844 0.06151 0.01008 0.00014 0.00030 0.00023 0.00000 0.00201 0.00253 0.00264 0.00208 0.00198 0.00186 0.00103 O31 1.01718 0.56404 0.10632 1.00000 0.09674 0.39677 0.30639 -0.14327 -0.05885 0.07505 0.35564 0.02163 0.00032 0.00101 0.00066 0.00000 0.00575 0.01780 0.01347 0.01235 0.00761 0.00797 0.01004 H31 0.99373 0.52651 0.09585 1.00000 0.53346 0.00000 0.00000 C41 0.91545 0.37714 0.18056 0.50000 0.09179 0.09582 0.09513 0.04665 0.04874 0.03444 0.09562 0.03862 0.00050 0.00103 0.00071 0.00000 0.00836 0.00917 0.00892 0.00730 0.00754 0.00689 0.00414 H41A 0.88845 0.33810 0.17706 0.50000 0.11474 0.00000 0.00000 H41B 0.92620 0.42132 0.21908 0.50000 0.11474 0.00000 0.00000 C42 0.95874 0.31579 0.20058 0.50000 0.09491 0.20371 0.12972 0.08697 0.04598 0.07406 0.15103 0.05269 0.00056 0.00143 0.00104 0.00000 0.00936 0.01572 0.01252 0.01159 0.00928 0.00947 0.00658 H42A 0.97352 0.29618 0.24910 0.50000 0.18124 0.00000 0.00000 H42B 0.94556 0.25919 0.17155 0.50000 0.18124 0.00000 0.00000 C43 0.98074 0.36228 0.12247 0.50000 0.13151 0.49940 0.27558 0.19641 0.15946 0.17094 0.27718 0.06946 0.00074 0.00245 0.00114 0.00000 0.01600 0.04360 0.02057 0.02541 0.01658 0.02144 0.01573 H43A 1.00802 0.38415 0.11789 0.50000 0.41577 0.00000 0.00000 H43B 0.95300 0.40731 0.10099 0.50000 0.41577 0.00000 0.00000 H43C 0.96854 0.30197 0.09939 0.50000 0.41577 0.00000 0.00000 C44 1.00914 0.45404 0.21689 0.50000 0.28149 0.30634 0.45416 0.06911 0.11507 -0.06273 0.39301 0.09448 0.00173 0.00194 0.00246 0.00000 0.04104 0.02619 0.04879 0.03625 0.04367 0.02525 0.02508 H44A 1.02355 0.45900 0.26666 0.50000 0.58952 0.00000 0.00000 H44B 0.97727 0.48845 0.19128 0.50000 0.58952 0.00000 0.00000 H44C 1.03282 0.48019 0.20655 0.50000 0.58952 0.00000 0.00000 C45 1.04536 0.30234 0.21751 0.50000 0.13079 0.47322 0.42165 0.30193 0.15080 0.13584 0.34240 0.08797 0.00084 0.00248 0.00179 0.00000 0.01906 0.04185 0.04137 0.03719 0.02191 0.02337 0.02082 H45A 1.06365 0.29041 0.26738 0.50000 0.51360 0.00000 0.00000 H45B 1.06655 0.33943 0.20753 0.50000 0.51360 0.00000 0.00000 H45C 1.03703 0.24312 0.19260 0.50000 0.51360 0.00000 0.00000 N41 0.99953 0.35249 0.19549 0.50000 0.10197 0.29771 0.22920 0.10875 0.08094 0.05709 0.21490 0.05183 0.00059 0.00157 0.00111 0.00000 0.01091 0.02055 0.01674 0.01845 0.01263 0.01206 0.00896 O41 0.89431 0.42827 0.12050 0.50000 0.07086 0.04986 0.04057 0.00150 0.02139 0.02193 0.05860 0.01529 0.00026 0.00042 0.00030 0.00000 0.00410 0.00344 0.00314 0.00252 0.00301 0.00305 0.00167 H41 0.88917 0.39363 0.08798 0.50000 0.08790 0.00000 0.00000 Final Structure Factor Calculation for s93 in C2/c Total number of l.s. parameters = 383 Maximum vector length = 511 Memory required = 6165 / 24017 wR2 = 0.3165 before cycle 11 for 10096 data and 0 / 383 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0804 0.0200 SAME/SADI C11 C12 C21 C22 0.0731 0.0200 SAME/SADI C41 O41 C31 O31 0.0601 0.0200 SAME/SADI C25 N21 C45 N41 0.1365 0.0400 SAME/SADI C42 C45 C22 C25 0.1282 0.0400 SAME/SADI C31 N31 C41 N41 etc. 0.1668 0.0400 SAME/SADI C32 C33 C22 C23 0.1694 0.0400 SAME/SADI C32 O31 C42 O41 etc. 0.1614 0.0400 SAME/SADI C42 C44 C32 C34 etc. -0.0385 0.0100 DELU C25 N21 0.1804 0.0400 SIMU U22 C11 C12 0.3013 0.0800 SIMU U11 C15 N11 -0.1468 0.0400 SIMU U13 C31 C32 0.2835 0.0400 SIMU U22 C32 N31 0.2262 0.0400 SIMU U33 C32 N31 0.2810 0.0800 SIMU U11 C35 N31 0.2983 0.0800 SIMU U22 C35 N31 0.3205 0.0800 SIMU U33 C35 N31 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 6. 0. 0. 84. 0. 0. 0. 92. 228. 0. 0. rms sigma 0.010 0.000 0.000 0.033 0.000 0.000 0.000 0.010 0.064 0.000 0.000 rms deviation 0.011 0.000 0.000 0.068 0.000 0.000 0.000 0.011 0.083 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.324 for 410 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0961 for 7730 Fo > 4sig(Fo) and 0.1126 for all 10096 data wR2 = 0.3165, GooF = S = 1.299, Restrained GooF = 1.324 for all data Occupancy sum of asymmetric unit = 38.50 for non-hydrogen and 49.00 for hydrogen atoms Principal mean square atomic displacements U 0.0494 0.0265 0.0252 O1 0.0497 0.0305 0.0255 O2 0.0501 0.0326 0.0195 O3 0.0474 0.0347 0.0179 O4 0.0484 0.0292 0.0228 O5 0.0517 0.0275 0.0182 O6 0.0500 0.0374 0.0196 O7 0.0476 0.0337 0.0138 O8 0.0435 0.0335 0.0203 O9 0.0560 0.0273 0.0173 O10 0.0378 0.0233 0.0162 Si1 0.0427 0.0192 0.0163 Si2 0.0349 0.0262 0.0140 Si3 0.0377 0.0236 0.0117 Si4 0.3598 0.0646 0.0355 C11 may be split into 1.0000 0.8944 0.1125 and 0.9980 0.8577 0.1059 0.2156 0.0752 0.0450 C12 may be split into 1.0480 0.9317 0.1607 and 1.0439 0.9106 0.1494 0.3454 0.1160 0.0490 C13 may be split into 1.1320 0.9395 0.2571 and 1.1342 0.9107 0.2487 0.2755 0.0724 0.0362 C14 may be split into 1.0738 0.8669 0.2722 and 1.0720 0.8373 0.2647 0.4355 0.1418 0.0908 C15 may be split into 1.1087 0.7950 0.1996 and 1.0981 0.7790 0.2089 0.0857 0.0520 0.0287 N11 0.1084 0.0616 0.0238 O11 0.1980 0.1291 0.0451 C21 0.1666 0.0867 0.0405 C22 0.3395 0.1072 0.0570 C23 may be split into 0.7265 0.4587 0.0760 and 0.7126 0.4458 0.0764 0.3158 0.1289 0.0461 C24 0.2198 0.1118 0.0713 C25 0.1244 0.0531 0.0321 N21 0.1816 0.0696 0.0235 O21 0.7341 0.3603 0.0678 C31 0.4496 0.2448 0.0470 C32 0.4749 0.0884 0.0442 C33 may be split into 0.8926 0.7129 -0.0355 and 0.9032 0.6811 -0.0140 0.3770 0.2616 0.0608 C34 0.7191 0.3314 0.1003 C35 0.0801 0.0764 0.0280 N31 0.7584 0.2481 0.0605 O31 may be split into 1.0206 0.5506 0.1213 and 1.0137 0.5775 0.0913 0.1426 0.0977 0.0466 C41 0.2619 0.1441 0.0471 C42 0.6222 0.1686 0.0407 C43 may be split into 0.9871 0.3825 0.1285 and 0.9744 0.3421 0.1165 0.6497 0.3064 0.2229 C44 0.7639 0.1798 0.0834 C45 may be split into 1.0535 0.3215 0.2303 and 1.0372 0.2832 0.2047 0.3821 0.1763 0.0864 N41 0.0985 0.0413 0.0360 O41 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.015 0.022 0.030 0.040 0.052 0.067 0.090 0.134 1.000 Number in group 1014. 1103. 975. 967. 1008. 1019. 997. 999. 1003. 1011. GooF 0.853 1.374 1.482 1.520 1.562 1.400 1.312 1.182 1.048 1.079 K 7.712 2.098 1.380 1.161 1.093 1.037 1.017 1.011 1.018 1.055 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 1011. 1042. 1000. 1015. 979. 1006. 1038. 978. 1013. 1014. GooF 0.859 0.858 0.871 1.006 0.990 1.078 1.244 1.435 1.530 2.355 K 1.078 1.014 1.030 1.012 0.998 1.009 1.025 1.035 1.054 1.073 R1 0.180 0.142 0.128 0.132 0.106 0.097 0.090 0.084 0.080 0.140 Recommended weighting scheme: WGHT 0.2000 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) 3 3 1 1995.64 194.55 8.10 0.025 3.91 5 1 0 497.71 80.65 7.34 0.016 4.97 12 4 0 452.50 8.22 7.33 0.005 1.88 7 5 9 362.97 17.86 7.15 0.007 1.36 1 1 7 806.85 47.16 6.89 0.012 2.56 -7 1 8 5800.55 806.54 6.79 0.050 2.82 2 6 4 2334.08 396.18 6.75 0.035 2.04 2 6 2 279.69 17.06 6.70 0.007 2.24 -16 0 2 1506.36 318.08 6.26 0.032 1.81 -3 1 6 9317.00 2121.97 6.13 0.081 3.64 -2 2 3 6303.76 1490.75 6.05 0.068 5.25 4 2 0 15457.24 3739.46 5.99 0.108 4.87 -8 4 7 1195.29 302.12 5.74 0.031 2.36 -11 1 10 401.92 86.25 5.71 0.016 2.19 -4 6 4 4099.46 894.22 5.53 0.053 2.21 -12 4 3 893.31 193.07 5.48 0.025 2.09 -26 2 6 547.75 106.45 5.44 0.018 1.16 8 4 2 756.12 199.94 5.34 0.025 2.16 8 8 6 473.60 54.99 5.22 0.013 1.29 -12 6 17 643.22 152.40 5.10 0.022 1.18 4 4 4 5.93 887.65 5.07 0.053 2.38 1 1 3 145.36 1415.35 5.02 0.066 5.21 7 3 0 70.84 710.94 5.01 0.047 2.97 -24 4 11 387.46 63.31 4.94 0.014 1.24 3 7 0 686.41 208.92 4.94 0.026 2.00 10 4 1 544.29 160.86 4.92 0.022 2.03 1 1 8 1647.40 489.01 4.84 0.039 2.27 -9 9 7 673.41 129.26 4.81 0.020 1.41 14 4 7 288.60 47.02 4.74 0.012 1.20 4 4 13 257.30 51.43 4.71 0.013 1.23 -16 0 10 6337.03 2127.33 4.67 0.081 1.86 5 1 9 189.92 37.14 4.66 0.011 1.68 0 4 1 3270.86 1090.84 4.64 0.058 3.54 -10 4 15 391.93 116.37 4.64 0.019 1.41 -12 6 9 83.49 3.91 4.59 0.003 1.66 8 4 1 119.52 25.29 4.57 0.009 2.30 8 0 6 72.17 717.62 4.57 0.047 1.86 0 10 0 1768.63 587.87 4.55 0.043 1.44 -13 3 6 695.39 233.86 4.54 0.027 2.17 13 1 7 314.45 55.07 4.47 0.013 1.32 -11 5 2 2627.15 917.21 4.45 0.054 1.97 -2 6 2 3665.98 1296.11 4.44 0.064 2.35 -12 2 12 1207.36 395.94 4.43 0.035 1.82 1 3 7 4441.10 1585.02 4.35 0.070 2.29 -7 3 1 176.17 36.76 4.35 0.011 3.15 -5 7 9 900.07 289.65 4.32 0.030 1.60 9 1 7 148.87 38.29 4.30 0.011 1.61 4 0 2 51542.34 18684.80 4.28 0.242 4.44 -3 11 5 347.76 101.76 4.27 0.018 1.26 11 5 4 316.11 106.47 4.27 0.018 1.52 Bond lengths and angles O1 - Distance Angles Si2 1.6199 (0.0026) Si1 1.6258 (0.0026) 148.19 (0.16) O1 - Si2 O2 - Distance Angles Si2 1.6165 (0.0025) Si3 1.6256 (0.0024) 148.97 (0.17) O2 - Si2 O3 - Distance Angles Si3 1.6210 (0.0024) Si4 1.6244 (0.0025) 149.77 (0.16) O3 - Si3 O4 - Distance Angles Si4 1.6121 (0.0024) Si1 1.6282 (0.0023) 150.70 (0.17) O4 - Si4 O5 - Distance Angles Si1 1.5813 (0.0024) O5 - O6 - Distance Angles Si2 1.6073 (0.0022) O6 - O7 - Distance Angles Si3 1.5797 (0.0024) O7 - O8 - Distance Angles Si4 1.5852 (0.0021) O8 - O9 - Distance Angles Si1 1.6230 (0.0023) Si3_$2 1.6267 (0.0023) 148.50 (0.16) O9 - Si1 O10 - Distance Angles Si2 1.6158 (0.0023) Si4_$2 1.6242 (0.0023) 146.72 (0.15) O10 - Si2 Si1 - Distance Angles O5 1.5813 (0.0024) O9 1.6230 (0.0023) 110.96 (0.13) O1 1.6258 (0.0026) 110.83 (0.13) 108.00 (0.13) O4 1.6282 (0.0023) 110.89 (0.13) 108.33 (0.12) 107.70 (0.13) Si1 - O5 O9 O1 Si2 - Distance Angles O6 1.6073 (0.0022) O10 1.6158 (0.0023) 108.91 (0.12) O2 1.6165 (0.0025) 109.72 (0.14) 109.14 (0.13) O1 1.6199 (0.0026) 109.82 (0.13) 109.20 (0.14) 110.03 (0.13) Si2 - O6 O10 O2 Si3 - Distance Angles O7 1.5797 (0.0024) O3 1.6210 (0.0024) 110.71 (0.13) O2 1.6256 (0.0024) 111.14 (0.13) 107.89 (0.13) O9_$2 1.6267 (0.0023) 111.29 (0.13) 107.80 (0.13) 107.86 (0.13) Si3 - O7 O3 O2 Si4 - Distance Angles O8 1.5852 (0.0021) O4 1.6121 (0.0024) 110.96 (0.13) O10_$2 1.6242 (0.0023) 110.11 (0.12) 108.17 (0.13) O3 1.6244 (0.0025) 110.54 (0.13) 108.41 (0.13) 108.57 (0.14) Si4 - O8 O4 O10_$2 C11 - Distance Angles O11 1.3966 (0.0069) C12 1.4245 (0.0085) 122.12 (0.60) H11A 0.9900 106.80 106.80 H11B 0.9900 106.80 106.80 106.65 C11 - O11 C12 H11A C12 - Distance Angles C11 1.4245 (0.0084) N11 1.4592 (0.0062) 122.30 (0.62) H12A 0.9900 106.75 106.75 H12B 0.9900 106.75 106.75 106.63 C12 - C11 N11 H12A C13 - Distance Angles N11 1.4104 (0.0072) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - N11 H13A H13B C14 - Distance Angles N11 1.5017 (0.0070) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - N11 H14A H14B C15 - Distance Angles N11 1.4909 (0.0094) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - N11 H15A H15B N11 - Distance Angles C13 1.4104 (0.0072) C12 1.4592 (0.0062) 115.44 (0.62) C15 1.4909 (0.0094) 99.87 (0.85) 113.10 (0.69) C14 1.5017 (0.0070) 109.17 (0.58) 113.46 (0.48) 104.46 (0.69) N11 - C13 C12 C15 O11 - Distance Angles C11 1.3966 (0.0069) H11 0.8400 109.47 O11 - C11 C21 - Distance Angles O21 1.4457 (0.0080) C22 1.5049 (0.0093) 114.27 (0.65) H21A 0.9900 108.69 108.69 H21B 0.9900 108.69 108.69 107.61 C21 - O21 C22 H21A C22 - Distance Angles N21 1.4812 (0.0066) C21 1.5049 (0.0093) 115.24 (0.57) H22A 0.9900 108.46 108.46 H22B 0.9900 108.46 108.46 107.49 C22 - N21 C21 H22A C23 - Distance Angles N21 1.4055 (0.0081) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - N21 H23A H23B C24 - Distance Angles N21 1.5019 (0.0078) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - N21 H24A H24B C25 - Distance Angles N21 1.5024 (0.0087) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - N21 H25A H25B N21 - Distance Angles C23 1.4055 (0.0081) C22 1.4812 (0.0066) 119.82 (0.65) C24 1.5019 (0.0078) 107.98 (0.59) 111.86 (0.52) C25 1.5024 (0.0087) 100.78 (0.70) 108.72 (0.50) 106.42 (0.70) N21 - C23 C22 C24 O21 - Distance Angles C21 1.4457 (0.0080) H21 0.8400 109.47 O21 - C21 C31 - Distance Angles O31 1.4499 (0.0156) C32 1.4861 (0.0134) 127.42 (1.21) H31A 0.9900 105.45 105.45 H31B 0.9900 105.45 105.45 106.04 C31 - O31 C32 H31A C32 - Distance Angles N31 1.4670 (0.0086) C31 1.4861 (0.0134) 127.43 (1.11) H32A 0.9900 105.45 105.45 H32B 0.9900 105.45 105.45 106.04 C32 - N31 C31 H32A C33 - Distance Angles N31 1.4243 (0.0075) H33A 0.9800 109.47 H33B 0.9800 109.47 109.47 H33C 0.9800 109.47 109.47 109.47 C33 - N31 H33A H33B C34 - Distance Angles N31 1.5230 (0.0098) H34A 0.9800 109.47 H34B 0.9800 109.47 109.47 H34C 0.9800 109.47 109.47 109.47 C34 - N31 H34A H34B C35 - Distance Angles N31 1.4871 (0.0114) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35 - N31 H35A H35B N31 - Distance Angles C33 1.4243 (0.0075) C32 1.4670 (0.0086) 107.46 (0.74) C35 1.4871 (0.0114) 98.71 (0.74) 114.22 (1.12) C34 1.5230 (0.0098) 105.76 (0.73) 121.53 (0.89) 106.45 (0.98) N31 - C33 C32 C35 O31 - Distance Angles C31 1.4499 (0.0156) H31 0.8400 109.47 O31 - C31 C41 - Distance Angles O41 1.3768 (0.0108) C42 1.4767 (0.0134) 119.30 (1.14) H41A 0.9900 107.49 107.49 H41B 0.9900 107.49 107.49 106.99 C41 - O41 C42 H41A C42 - Distance Angles N41 1.4611 (0.0140) C41 1.4767 (0.0134) 118.11 (1.31) H42A 0.9900 107.78 107.78 H42B 0.9900 107.78 107.78 107.13 C42 - N41 C41 H42A C43 - Distance Angles N41 1.4559 (0.0154) H43A 0.9800 109.47 H43B 0.9800 109.47 109.47 H43C 0.9800 109.47 109.47 109.47 C43 - N41 H43A H43B C44 - Distance Angles N41 1.5188 (0.0156) H44A 0.9800 109.47 H44B 0.9800 109.47 109.47 H44C 0.9800 109.47 109.47 109.47 C44 - N41 H44A H44B C45 - Distance Angles N41 1.4422 (0.0149) H45A 0.9800 109.47 H45B 0.9800 109.47 109.47 H45C 0.9800 109.47 109.47 109.47 C45 - N41 H45A H45B N41 - Distance Angles C45 1.4422 (0.0149) C43 1.4559 (0.0154) 98.57 (1.64) C42 1.4611 (0.0140) 123.82 (1.70) 108.18 (1.54) C44 1.5188 (0.0156) 112.53 (1.93) 99.54 (1.82) 110.45 (1.78) N41 - C45 C43 C42 O41 - Distance Angles C41 1.3768 (0.0108) H41 0.8400 109.47 O41 - C41 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)