+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 16:11:07 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S93 in Pbca CELL 0.71073 17.4597 17.3538 28.3363 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0007 0.0014 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O SI UNIT 192 288 144 96 V = 8585.67 F(000) = 3936.0 Mu = 0.43 mm-1 Cell Wt = 7596.86 Rho = 1.469 MERG 2 SHEL 7 0.84 DFIX 1.3 0.02 C11 C12 ANIS SI1 SI4 SI2 SI6 SI3 SI10 SI9 SI7 SI11 SI8 SI12 SI5 O1 O12 O6 O4 ANIS O14 O11 O10 O13 O3 O8 O5 O7 O9 O15 O2 O16 O17 C7 O18 C2 C5 C13 ANIS C24 C17 C1 C8 C3 C6 C21 C14 C11 C23 C18 C16 C22 C20 C15 C9 C12 ANIS C19 C10 C4 FMAP 2 PLAN 10 SIZE 0.10 0.20 0.25 ACTA BOND $H WGHT 0.08080 250.39850 L.S. 20 TEMP -153.00 FVAR 0.03200 SI1 4 0.053610 0.580754 0.072108 11.00000 0.02739 0.02385 = 0.03783 -0.00636 -0.00404 -0.00103 SI4 4 -0.148655 0.697720 0.175676 11.00000 0.02399 0.02769 = 0.02820 0.00077 -0.00400 -0.00151 SI2 4 0.136546 0.608394 0.168554 11.00000 0.02806 0.02730 = 0.03826 -0.00143 -0.00435 -0.00665 SI6 4 -0.088767 0.758382 0.010462 11.00000 0.02397 0.03884 = 0.04147 0.00488 -0.00075 0.00376 SI3 4 -0.004435 0.644967 0.233426 11.00000 0.02551 0.02572 = 0.03727 0.00780 -0.00649 -0.00276 SI10 4 0.049637 0.818804 0.241615 11.00000 0.02845 0.02841 = 0.04047 0.00234 -0.00255 -0.00356 SI9 4 0.175522 0.781924 0.166720 11.00000 0.02793 0.02544 = 0.03947 0.00242 -0.00379 0.00004 SI7 4 0.080581 0.706084 -0.003366 11.00000 0.03251 0.02774 = 0.04199 0.00123 0.00201 -0.00199 SI11 4 -0.085917 0.870336 0.178030 11.00000 0.03182 0.02522 = 0.03860 -0.00162 -0.00137 0.00228 SI8 4 0.131740 0.838277 0.065269 11.00000 0.02713 0.03102 = 0.03313 0.00885 -0.00083 0.00284 SI12 4 -0.035598 0.897429 0.073295 11.00000 0.03107 0.02799 = 0.04006 0.01016 0.00379 0.00094 SI5 4 -0.119108 0.624456 0.077052 11.00000 0.02587 0.03983 = 0.02712 -0.00310 -0.00142 -0.00278 O1 3 0.112807 0.596123 0.114223 11.00000 0.03534 0.03149 = 0.03134 -0.00102 -0.00679 -0.00568 O12 3 0.126876 0.770088 0.026253 11.00000 0.03013 0.03053 = 0.04550 -0.00580 0.00016 -0.00377 O6 3 -0.128894 0.684501 0.034552 11.00000 0.02513 0.04249 = 0.05675 0.00705 0.00287 0.00537 O4 3 -0.157643 0.660769 0.124042 11.00000 0.01533 0.04502 = 0.03920 -0.00508 -0.00240 -0.00528 O14 3 0.125324 0.819042 0.207300 11.00000 0.02501 0.02386 = 0.08172 0.01646 0.00214 0.00459 O11 3 -0.007648 0.733988 -0.011226 11.00000 0.03917 0.04116 = 0.04474 -0.01477 0.00511 0.00767 O10 3 -0.124091 0.785098 0.169844 11.00000 0.01755 0.03462 = 0.05724 0.00838 0.00058 0.00675 O13 3 0.136209 0.798744 0.116625 11.00000 0.04621 0.04520 = 0.02250 0.00768 0.00663 0.00519 O3 3 -0.083050 0.650985 0.203923 11.00000 0.03632 0.03234 = 0.06475 0.00395 -0.00620 0.00253 O8 3 0.178229 0.689446 0.173614 11.00000 0.04195 0.02165 = 0.04092 0.00665 -0.01136 0.00349 O5 3 -0.027993 0.617479 0.087952 11.00000 0.03247 0.03981 = 0.03586 0.00562 0.01123 0.01741 O7 3 0.081275 0.627118 0.026363 11.00000 0.04393 0.04815 = 0.03800 0.02048 0.00491 0.00571 O9 3 0.022811 0.729709 0.250149 11.00000 0.03303 0.03524 = 0.04883 0.00210 0.00085 -0.00001 O15 3 -0.018810 0.864358 0.217016 11.00000 0.04938 0.02062 = 0.03955 0.00128 -0.01066 0.00441 O2 3 0.062056 0.606016 0.199317 11.00000 0.04759 0.02750 = 0.03631 0.00296 -0.00237 0.00860 O16 3 -0.048850 0.900205 0.129223 11.00000 0.05204 0.02224 = 0.03145 0.00111 0.00509 0.00882 O17 3 0.054570 0.895265 0.062788 11.00000 0.01945 0.04969 = 0.04312 0.00049 -0.00691 0.00087 C7 1 -0.240960 0.686327 0.205661 11.00000 0.03222 AFIX 43 H7 2 -0.243014 0.700450 0.238028 11.00000 -1.20000 AFIX 0 O18 3 -0.075617 0.823331 0.050840 11.00000 0.04523 0.04190 = 0.05571 -0.00530 0.00747 -0.00249 C2 1 0.082723 0.424429 0.083546 11.00000 0.04562 AFIX 93 H2A 2 0.115540 0.437907 0.108982 11.00000 -1.20000 H2B 2 0.076123 0.371856 0.075132 11.00000 -1.20000 AFIX 0 C5 1 -0.021832 0.585215 0.285426 11.00000 0.04228 AFIX 43 H5 2 -0.035045 0.532695 0.280613 11.00000 -1.20000 AFIX 0 C13 1 0.128238 0.691387 -0.061162 11.00000 0.04493 AFIX 43 H13 2 0.106169 0.656467 -0.083110 11.00000 -1.20000 AFIX 0 C24 1 -0.101998 1.043066 0.068319 11.00000 0.04800 AFIX 93 H24A 2 -0.105466 1.040671 0.101745 11.00000 -1.20000 H24B 2 -0.120116 1.087255 0.051980 11.00000 -1.20000 AFIX 0 C17 1 0.272907 0.822676 0.167755 11.00000 0.03688 AFIX 43 H17 2 0.279336 0.875527 0.159966 11.00000 -1.20000 AFIX 0 C1 1 0.047278 0.477289 0.060530 11.00000 0.03402 AFIX 43 H1 2 0.015046 0.461278 0.035363 11.00000 -1.20000 AFIX 0 C8 1 -0.304080 0.660661 0.186751 11.00000 0.04547 AFIX 93 H8A 2 -0.304843 0.645820 0.154484 11.00000 -1.20000 H8B 2 -0.349307 0.656800 0.205240 11.00000 -1.20000 AFIX 0 C3 1 0.203215 0.531670 0.187158 11.00000 0.04448 AFIX 43 H3 2 0.180142 0.484257 0.196032 11.00000 -1.20000 AFIX 0 C6 1 -0.017335 0.609652 0.327778 11.00000 0.05651 AFIX 93 H6A 2 -0.004245 0.661882 0.333760 11.00000 -1.20000 H6B 2 -0.027075 0.575627 0.353347 11.00000 -1.20000 AFIX 0 C21 1 -0.157388 0.940934 0.198896 11.00000 0.04094 AFIX 43 H21 2 -0.143074 0.992391 0.206183 11.00000 -1.20000 AFIX 0 C14 1 0.190830 0.727306 -0.072602 11.00000 0.05499 AFIX 93 H14A 2 0.213637 0.762419 -0.051060 11.00000 -1.20000 H14B 2 0.213790 0.718458 -0.102510 11.00000 -1.20000 AFIX 0 C11 1 -0.154376 0.797405 -0.036520 11.00000 0.05630 AFIX 43 H11 2 -0.207124 0.802048 -0.028801 11.00000 -1.20000 AFIX 0 C23 1 -0.072359 0.985684 0.044861 11.00000 0.03940 AFIX 43 H23 2 -0.069551 0.989506 0.011461 11.00000 -1.20000 AFIX 0 C18 1 0.334956 0.781457 0.178938 11.00000 0.05400 AFIX 93 H18A 2 0.330000 0.728497 0.186857 11.00000 -1.20000 H18B 2 0.384024 0.805115 0.178970 11.00000 -1.20000 AFIX 0 C16 1 0.215023 0.976606 0.057555 11.00000 0.04671 AFIX 93 H16A 2 0.170242 1.001919 0.068615 11.00000 -1.20000 H16B 2 0.259600 1.005680 0.050308 11.00000 -1.20000 AFIX 0 C22 1 -0.229383 0.917558 0.203399 11.00000 0.04608 AFIX 93 H22A 2 -0.242759 0.865902 0.195965 11.00000 -1.20000 H22B 2 -0.267549 0.952480 0.214056 11.00000 -1.20000 AFIX 0 C20 1 0.039369 0.923684 0.315087 11.00000 0.05436 AFIX 93 H20A 2 -0.000222 0.948577 0.297868 11.00000 -1.20000 H20B 2 0.054737 0.943266 0.344928 11.00000 -1.20000 AFIX 0 C15 1 0.215312 0.899162 0.052125 11.00000 0.03837 AFIX 43 H15 2 0.260748 0.875118 0.041016 11.00000 -1.20000 AFIX 0 C9 1 -0.162855 0.529901 0.061423 11.00000 0.04223 AFIX 43 H9 2 -0.151180 0.506446 0.031997 11.00000 -1.20000 AFIX 0 C12 1 -0.134219 0.817935 -0.077430 11.00000 0.14476 AFIX 93 H12A 2 -0.082020 0.814251 -0.086619 11.00000 -1.20000 H12B 2 -0.171254 0.837064 -0.099017 11.00000 -1.20000 AFIX 0 C19 1 0.072899 0.862122 0.297615 11.00000 0.03079 AFIX 43 H19 2 0.112244 0.838785 0.315836 11.00000 -1.20000 AFIX 0 C10 1 -0.208763 0.496281 0.090293 11.00000 0.06584 AFIX 93 H10A 2 -0.220515 0.519636 0.119738 11.00000 -1.20000 H10B 2 -0.230943 0.448076 0.082187 11.00000 -1.20000 AFIX 0 C4 1 0.274810 0.533733 0.189652 11.00000 0.05620 AFIX 93 H4A 2 0.301537 0.579417 0.181284 11.00000 -1.20000 H4B 2 0.302384 0.489613 0.199911 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for S93 in Pbca C 0.770 H 0.320 O 0.660 SI 1.170 Si1 - O7 O1 O5 C1 Si4 - O10 O4 O3 C7 Si2 - O2 O8 O1 C3 Si6 - O11 O6 O18 C11 Si3 - O3 O9 O2 C5 Si10 - O15 O9 O14 C19 Si9 - O14 O13 O8 C17 Si7 - O7 O12 O11 C13 Si11 - O16 O15 O10 C21 Si8 - O13 O12 O17 C15 Si12 - O18 O16 O17 C23 Si5 - O6 O4 O5 C9 O1 - Si1 Si2 O12 - Si7 Si8 O6 - Si5 Si6 O4 - Si4 Si5 O14 - Si9 Si10 O11 - Si6 Si7 O10 - Si4 Si11 O13 - Si9 Si8 O3 - Si3 Si4 O8 - Si2 Si9 O5 - Si1 Si5 O7 - Si1 Si7 O9 - Si3 Si10 O15 - Si10 Si11 O2 - Si2 Si3 O16 - Si12 Si11 O17 - Si12 Si8 C7 - C8 Si4 O18 - Si12 Si6 C2 - C1 C5 - C6 Si3 C13 - C14 Si7 C24 - C23 C17 - C18 Si9 C1 - C2 Si1 C8 - C7 C3 - C4 Si2 C6 - C5 C21 - C22 Si11 C14 - C13 C11 - C12 Si6 C23 - C24 Si12 C18 - C17 C16 - C15 C22 - C21 C20 - C19 C15 - C16 Si8 C9 - C10 Si5 C12 - C11 C19 - C20 Si10 C10 - C9 C4 - C3 h k l Fo^2 Sigma Why rejected 1 14 0 14.30 3.07 observed but should be systematically absent 3 12 0 8.37 2.09 observed but should be systematically absent 0 9 20 3.92 0.98 observed but should be systematically absent 0 9 4 3.96 0.99 observed but should be systematically absent 0 7 10 8.20 0.91 observed but should be systematically absent 0 7 8 3.77 0.94 observed but should be systematically absent 0 7 6 10.38 1.89 observed but should be systematically absent 0 7 4 4.91 0.98 observed but should be systematically absent 3 6 0 7.22 1.03 observed but should be systematically absent 3 6 0 8.41 2.10 observed but should be systematically absent 0 5 4 5.66 0.94 observed but should be systematically absent 9 4 0 11.61 1.94 observed but should be systematically absent 9 4 0 10.81 1.09 observed but should be systematically absent 9 4 0 14.85 2.79 observed but should be systematically absent 7 4 0 5.59 0.93 observed but should be systematically absent 7 4 0 5.43 1.09 observed but should be systematically absent 0 3 24 11.96 2.99 observed but should be systematically absent 0 3 10 8.07 1.01 observed but should be systematically absent 0 3 10 7.17 1.03 observed but should be systematically absent 0 3 8 18.20 1.02 observed but should be systematically absent 0 3 8 20.83 2.09 observed but should be systematically absent 0 3 2 4.85 0.97 observed but should be systematically absent 9 2 0 4.22 1.05 observed but should be systematically absent 9 2 0 6.09 1.02 observed but should be systematically absent 9 2 0 7.88 1.75 observed but should be systematically absent 0 1 16 6.96 1.00 observed but should be systematically absent 0 1 16 7.97 1.00 observed but should be systematically absent 0 1 8 13.18 1.02 observed but should be systematically absent 0 1 8 14.91 1.99 observed but should be systematically absent 14 0 3 5.03 1.01 observed but should be systematically absent 12 0 7 17.88 4.26 observed but should be systematically absent 12 0 7 17.16 3.44 observed but should be systematically absent 12 0 5 11.98 2.57 observed but should be systematically absent 10 0 7 10.12 1.69 observed but should be systematically absent 6 0 15 4.24 1.06 observed but should be systematically absent 6 0 13 6.43 1.07 observed but should be systematically absent 6 0 3 3.96 0.79 observed but should be systematically absent 6 0 1 5.08 1.02 observed but should be systematically absent 6 0 1 6.30 0.79 observed but should be systematically absent 6 0 1 6.08 1.01 observed but should be systematically absent 6 0 1 7.58 1.68 observed but should be systematically absent 4 0 11 5.18 1.04 observed but should be systematically absent 2 0 13 9.06 1.01 observed but should be systematically absent 2 0 13 13.11 1.01 observed but should be systematically absent 2 0 13 6.17 1.03 observed but should be systematically absent 6 0 1 6.08 1.01 observed but should be systematically absent 6 0 1 6.17 1.03 observed but should be systematically absent 6 0 1 7.05 0.78 observed but should be systematically absent 6 0 1 7.61 1.69 observed but should be systematically absent 12 0 5 10.31 2.06 observed but should be systematically absent ** etc. ** 41553 Reflections read, of which 6194 rejected -20 =< h =< 17, -20 =< k =< 19, -28 =< l =< 33, Max. 2-theta = 50.04 71 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 2 1 3.42 0.43 11 3.77 4 1 2 4.73 0.34 12 2.91 3 10 5 27.57 0.78 6 7.12 0 4 6 102.33 3.93 2 20.45 4 Inconsistent equivalents 7552 Unique reflections, of which 0 suppressed R(int) = 0.3375 R(sigma) = 0.3341 Friedel opposites merged Maximum memory for data reduction = 4338 / 75055 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 = 5689 / 640511 wR2 = 0.3839 before cycle 1 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.055; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03203 0.00015 0.198 OSF Mean shift/su = 0.292 Maximum = -2.715 for U11 C22 Max. shift = 0.024 A for C12 Max. dU =-0.005 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3792 before cycle 2 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.039 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.041; Restrained GooF = 1.042 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03207 0.00015 0.250 OSF Mean shift/su = 0.143 Maximum = 1.576 for U33 C10 Max. shift = 0.009 A for C17 Max. dU = 0.009 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3784 before cycle 3 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.180 OSF Mean shift/su = 0.050 Maximum = 0.669 for U33 C10 Max. shift = 0.005 A for C17 Max. dU = 0.006 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 4 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.035 OSF Mean shift/su = 0.020 Maximum = 0.298 for U33 C10 Max. shift = 0.004 A for C12 Max. dU = 0.003 for C12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 5 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.035 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.011 OSF Mean shift/su = 0.010 Maximum = 0.195 for U33 C12 Max. shift = 0.003 A for C11 Max. dU = 0.002 for C12 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 6 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.003 OSF Mean shift/su = 0.006 Maximum = -0.131 for U11 C12 Max. shift = 0.003 A for C11 Max. dU = 0.001 for C12 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 7 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.004 Maximum = -0.126 for U11 C12 Max. shift = 0.003 A for C11 Max. dU = 0.001 for C12 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 8 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 -0.001 OSF Mean shift/su = 0.004 Maximum = -0.117 for U11 C12 Max. shift = 0.003 A for C11 Max. dU = 0.001 for C12 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 9 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 -0.002 OSF Mean shift/su = 0.003 Maximum = -0.104 for U11 C12 Max. shift = 0.002 A for C11 Max. dU = 0.001 for C12 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 10 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 -0.002 OSF Mean shift/su = 0.003 Maximum = -0.091 for U11 C12 Max. shift = 0.002 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 11 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.003 Maximum = -0.078 for U11 C12 Max. shift = 0.002 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 12 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 -0.001 OSF Mean shift/su = 0.002 Maximum = -0.066 for U11 C12 Max. shift = 0.002 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 13 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 -0.001 OSF Mean shift/su = 0.002 Maximum = -0.056 for U11 C12 Max. shift = 0.002 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 14 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.002 Maximum = -0.047 for U11 C12 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 15 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.002 Maximum = -0.040 for U11 C12 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 16 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3782 before cycle 16 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = -0.034 for U11 C12 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 17 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 17 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = -0.029 for U11 C12 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 18 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3782 before cycle 18 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = -0.025 for U12 C11 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 19 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3782 before cycle 19 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = -0.022 for U12 C11 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 20 Maximum vector length = 511 Memory required = 5689 / 640511 wR2 = 0.3783 before cycle 20 for 7552 data and 487 / 487 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.03210 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = -0.020 for U12 C11 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C12 Largest correlation matrix elements 0.527 z C12 / z C11 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 -0.2431 0.7005 0.2378 43 0.950 0.000 C7 C8 Si4 H2A 0.1160 0.4378 0.1091 93 0.950 0.000 C2 C1 Si1 H2B 0.0766 0.3716 0.0753 93 0.950 0.000 C2 C1 Si1 H5 -0.0349 0.5329 0.2809 43 0.950 0.000 C5 C6 Si3 H13 0.1069 0.6564 -0.0830 43 0.950 0.000 C13 C14 Si7 H24A -0.1072 1.0399 0.1020 93 0.950 0.000 C24 C23 Si12 H24B -0.1207 1.0876 0.0526 93 0.950 0.000 C24 C23 Si12 H17 0.2779 0.8751 0.1597 43 0.950 0.000 C17 C18 Si9 H1 0.0153 0.4607 0.0356 43 0.950 0.000 C1 C2 Si1 H8A -0.3052 0.6460 0.1545 93 0.950 0.000 C8 C7 Si4 H8B -0.3494 0.6571 0.2053 93 0.950 0.000 C8 C7 Si4 H3 0.1809 0.4848 0.1971 43 0.950 0.000 C3 C4 Si2 H6A -0.0042 0.6620 0.3346 93 0.950 0.000 C6 C5 Si3 H6B -0.0270 0.5756 0.3539 93 0.950 0.000 C6 C5 Si3 H21 -0.1442 0.9922 0.2059 43 0.950 0.000 C21 C22 Si11 H14A 0.2135 0.7630 -0.0511 93 0.950 0.000 C14 C13 Si7 H14B 0.2140 0.7187 -0.1024 93 0.950 0.000 C14 C13 Si7 H11 -0.2090 0.8033 -0.0280 43 0.950 0.000 C11 C12 Si6 H23 -0.0684 0.9908 0.0116 43 0.950 0.000 C23 C24 Si12 H18A 0.3303 0.7292 0.1866 93 0.950 0.000 C18 C17 Si9 H18B 0.3831 0.8065 0.1783 93 0.950 0.000 C18 C17 Si9 H16A 0.1704 1.0011 0.0687 93 0.950 0.000 C16 C15 Si8 H16B 0.2596 1.0048 0.0501 93 0.950 0.000 C16 C15 Si8 H22A -0.2434 0.8659 0.1960 93 0.950 0.000 C22 C21 Si11 H22B -0.2680 0.9527 0.2138 93 0.950 0.000 C22 C21 Si11 H20A -0.0007 0.9478 0.2975 93 0.950 0.000 C20 C19 Si10 H20B 0.0545 0.9432 0.3445 93 0.950 0.000 C20 C19 Si10 H15 0.2605 0.8743 0.0406 43 0.950 0.000 C15 C16 Si8 H9 -0.1504 0.5070 0.0321 43 0.950 0.000 C9 C10 Si5 H12A -0.0827 0.8126 -0.0857 93 0.950 0.001 C12 C11 Si6 H12B -0.1712 0.8369 -0.0989 93 0.950 0.001 C12 C11 Si6 H19 0.1128 0.8387 0.3154 43 0.950 0.000 C19 C20 Si10 H10A -0.2207 0.5200 0.1194 93 0.950 0.000 C10 C9 Si5 H10B -0.2304 0.4486 0.0816 93 0.950 0.000 C10 C9 Si5 H4A 0.3019 0.5790 0.1805 93 0.950 0.000 C4 C3 Si2 H4B 0.3026 0.4897 0.2000 93 0.950 0.000 C4 C3 Si2 S93 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.05352 0.58080 0.07210 1.00000 0.02762 0.02451 0.03763 -0.00579 -0.00352 -0.00046 0.02992 0.00790 0.00025 0.00027 0.00017 0.00000 0.00249 0.00279 0.00300 0.00241 0.00221 0.00212 0.00120 Si4 -0.14865 0.69779 0.17573 1.00000 0.02446 0.02803 0.02812 0.00046 -0.00386 -0.00142 0.02687 0.00774 0.00024 0.00027 0.00016 0.00000 0.00237 0.00279 0.00272 0.00231 0.00209 0.00202 0.00114 Si2 0.13655 0.60839 0.16860 1.00000 0.02883 0.02663 0.03813 -0.00090 -0.00432 -0.00642 0.03120 0.00795 0.00025 0.00028 0.00017 0.00000 0.00255 0.00283 0.00302 0.00244 0.00231 0.00216 0.00121 Si6 -0.08873 0.75840 0.01047 1.00000 0.02408 0.03871 0.04016 0.00469 -0.00036 0.00312 0.03431 0.00872 0.00025 0.00030 0.00018 0.00000 0.00244 0.00325 0.00314 0.00258 0.00229 0.00230 0.00129 Si3 -0.00448 0.64496 0.23338 1.00000 0.02586 0.02686 0.03654 0.00811 -0.00648 -0.00285 0.02975 0.00795 0.00025 0.00027 0.00017 0.00000 0.00245 0.00280 0.00294 0.00237 0.00228 0.00209 0.00119 Si10 0.04964 0.81880 0.24160 1.00000 0.02843 0.02895 0.04213 0.00254 -0.00279 -0.00322 0.03317 0.00832 0.00026 0.00028 0.00018 0.00000 0.00256 0.00294 0.00309 0.00253 0.00233 0.00220 0.00125 Si9 0.17547 0.78194 0.16672 1.00000 0.02818 0.02498 0.03935 0.00190 -0.00308 -0.00014 0.03084 0.00817 0.00025 0.00027 0.00018 0.00000 0.00249 0.00293 0.00312 0.00245 0.00228 0.00210 0.00124 Si7 0.08057 0.70608 -0.00337 1.00000 0.03323 0.02799 0.04143 0.00105 0.00184 -0.00273 0.03421 0.00857 0.00027 0.00029 0.00018 0.00000 0.00265 0.00291 0.00311 0.00249 0.00240 0.00226 0.00126 Si11 -0.08589 0.87037 0.17801 1.00000 0.03214 0.02537 0.03850 -0.00105 -0.00148 0.00243 0.03200 0.00837 0.00026 0.00028 0.00018 0.00000 0.00262 0.00286 0.00303 0.00239 0.00233 0.00219 0.00123 Si8 0.13168 0.83837 0.06531 1.00000 0.02789 0.03070 0.03421 0.00906 -0.00109 0.00246 0.03093 0.00839 0.00025 0.00028 0.00017 0.00000 0.00255 0.00298 0.00292 0.00243 0.00222 0.00220 0.00122 Si12 -0.03569 0.89732 0.07334 1.00000 0.03125 0.03000 0.03991 0.01024 0.00369 0.00082 0.03372 0.00883 0.00026 0.00029 0.00018 0.00000 0.00262 0.00300 0.00311 0.00256 0.00233 0.00223 0.00126 Si5 -0.11901 0.62439 0.07704 1.00000 0.02579 0.03942 0.02779 -0.00350 -0.00124 -0.00301 0.03100 0.00798 0.00026 0.00029 0.00016 0.00000 0.00246 0.00326 0.00278 0.00246 0.00216 0.00222 0.00123 O1 0.11302 0.59619 0.11411 1.00000 0.03585 0.03137 0.03200 -0.00250 -0.00667 -0.00697 0.03307 0.01779 0.00059 0.00064 0.00037 0.00000 0.00644 0.00708 0.00677 0.00584 0.00541 0.00539 0.00284 O12 0.12716 0.77024 0.02621 1.00000 0.02970 0.03015 0.04801 -0.00555 0.00048 -0.00343 0.03595 0.01850 0.00058 0.00064 0.00040 0.00000 0.00609 0.00718 0.00752 0.00619 0.00574 0.00544 0.00293 O6 -0.12890 0.68453 0.03429 1.00000 0.02596 0.04145 0.05550 0.00738 0.00441 0.00556 0.04097 0.02038 0.00058 0.00069 0.00042 0.00000 0.00620 0.00806 0.00821 0.00668 0.00596 0.00569 0.00318 O4 -0.15758 0.66069 0.12404 1.00000 0.01545 0.04559 0.03875 -0.00705 -0.00042 -0.00461 0.03326 0.01771 0.00053 0.00066 0.00038 0.00000 0.00551 0.00783 0.00718 0.00623 0.00503 0.00514 0.00292 O14 0.12526 0.81903 0.20726 1.00000 0.02562 0.02506 0.08220 0.01978 0.00244 0.00482 0.04429 0.02121 0.00059 0.00065 0.00046 0.00000 0.00616 0.00720 0.00962 0.00685 0.00657 0.00537 0.00339 O11 -0.00745 0.73399 -0.01105 1.00000 0.04108 0.04094 0.04326 -0.01463 0.00367 0.00632 0.04176 0.01951 0.00062 0.00069 0.00041 0.00000 0.00681 0.00762 0.00781 0.00634 0.00604 0.00603 0.00316 O10 -0.12397 0.78520 0.16992 1.00000 0.01850 0.03440 0.05710 0.00746 -0.00103 0.00684 0.03667 0.01938 0.00056 0.00064 0.00041 0.00000 0.00550 0.00739 0.00791 0.00649 0.00564 0.00514 0.00299 O13 0.13617 0.79873 0.11667 1.00000 0.04671 0.04566 0.02101 0.00496 0.00635 0.00653 0.03779 0.01998 0.00064 0.00068 0.00036 0.00000 0.00721 0.00797 0.00634 0.00591 0.00560 0.00605 0.00303 O3 -0.08310 0.65120 0.20391 1.00000 0.03704 0.03115 0.06167 0.00307 -0.00639 0.00198 0.04329 0.02015 0.00063 0.00068 0.00043 0.00000 0.00679 0.00752 0.00865 0.00665 0.00638 0.00575 0.00326 O8 0.17818 0.68959 0.17342 1.00000 0.04141 0.02050 0.04044 0.00686 -0.01086 0.00288 0.03411 0.01877 0.00061 0.00062 0.00039 0.00000 0.00667 0.00658 0.00728 0.00586 0.00574 0.00524 0.00289 O5 -0.02785 0.61775 0.08800 1.00000 0.03395 0.04173 0.03323 0.00645 0.01177 0.01707 0.03630 0.02047 0.00059 0.00067 0.00038 0.00000 0.00649 0.00798 0.00693 0.00594 0.00543 0.00566 0.00306 O7 0.08119 0.62718 0.02644 1.00000 0.04358 0.04603 0.03926 0.01631 0.00415 0.00582 0.04296 0.02138 0.00064 0.00071 0.00041 0.00000 0.00708 0.00847 0.00743 0.00647 0.00602 0.00618 0.00324 O9 0.02300 0.72996 0.25021 1.00000 0.03387 0.03125 0.04992 -0.00010 0.00245 -0.00092 0.03835 0.01940 0.00059 0.00065 0.00042 0.00000 0.00640 0.00720 0.00782 0.00633 0.00582 0.00544 0.00304 O15 -0.01892 0.86432 0.21688 1.00000 0.04966 0.02270 0.03700 0.00277 -0.01088 0.00643 0.03645 0.01893 0.00063 0.00062 0.00039 0.00000 0.00732 0.00685 0.00702 0.00561 0.00590 0.00564 0.00299 O2 0.06190 0.60575 0.19937 1.00000 0.04796 0.02948 0.03671 0.00100 -0.00453 0.01057 0.03805 0.01964 0.00064 0.00065 0.00039 0.00000 0.00726 0.00727 0.00711 0.00602 0.00587 0.00582 0.00302 O16 -0.04883 0.90020 0.12915 1.00000 0.05386 0.02310 0.03204 0.00060 0.00304 0.00810 0.03633 0.01959 0.00064 0.00063 0.00038 0.00000 0.00746 0.00676 0.00697 0.00570 0.00581 0.00578 0.00295 O17 0.05474 0.89549 0.06277 1.00000 0.01935 0.04822 0.04248 0.00017 -0.00712 -0.00063 0.03668 0.01870 0.00056 0.00069 0.00039 0.00000 0.00569 0.00801 0.00739 0.00635 0.00522 0.00545 0.00303 C7 -0.24104 0.68638 0.20546 1.00000 0.03622 0.02906 0.03904 -0.01881 0.01432 0.01092 0.03477 0.03102 0.00095 0.00096 0.00062 0.00000 0.01075 0.01099 0.01107 0.00902 0.00899 0.00846 0.00454 H7 -0.24308 0.70051 0.23783 1.00000 0.04173 0.00000 0.00000 O18 -0.07551 0.82344 0.05087 1.00000 0.04595 0.03930 0.05598 -0.00702 0.00759 0.00088 0.04708 0.02107 0.00066 0.00071 0.00044 0.00000 0.00742 0.00821 0.00845 0.00685 0.00654 0.00632 0.00337 C2 0.08314 0.42419 0.08368 1.00000 0.04219 0.04770 0.05271 -0.01180 -0.02211 0.02011 0.04753 0.03325 0.00101 0.00119 0.00067 0.00000 0.01104 0.01348 0.01314 0.01094 0.01020 0.01022 0.00540 H2A 0.11600 0.43779 0.10906 1.00000 0.05704 0.00000 0.00000 H2B 0.07663 0.37158 0.07531 1.00000 0.05704 0.00000 0.00000 C5 -0.02172 0.58546 0.28568 1.00000 0.02757 0.03488 0.06977 0.00988 0.00506 -0.00565 0.04407 0.03593 0.00092 0.00114 0.00076 0.00000 0.01002 0.01207 0.01556 0.01124 0.00987 0.00845 0.00517 H5 -0.03491 0.53293 0.28088 1.00000 0.05289 0.00000 0.00000 C13 0.12872 0.69155 -0.06111 1.00000 0.04806 0.03369 0.05676 -0.01607 0.00633 -0.00150 0.04617 0.03344 0.00107 0.00109 0.00069 0.00000 0.01175 0.01173 0.01311 0.01032 0.01039 0.00975 0.00509 H13 0.10694 0.65641 -0.08304 1.00000 0.05541 0.00000 0.00000 C24 -0.10281 1.04313 0.06868 1.00000 0.04189 0.03751 0.06968 0.01115 0.00000 0.00991 0.04969 0.03431 0.00100 0.00115 0.00077 0.00000 0.01170 0.01256 0.01508 0.01179 0.01079 0.00969 0.00547 H24A -0.10719 1.03989 0.10204 1.00000 0.05963 0.00000 0.00000 H24B -0.12070 1.08763 0.05256 1.00000 0.05963 0.00000 0.00000 C17 0.27190 0.82223 0.16755 1.00000 0.02655 0.01475 0.07849 -0.00245 0.01118 -0.01808 0.03993 0.02920 0.00093 0.00099 0.00069 0.00000 0.00989 0.00986 0.01461 0.01000 0.00973 0.00794 0.00493 H17 0.27790 0.87509 0.15966 1.00000 0.04792 0.00000 0.00000 C1 0.04753 0.47687 0.06069 1.00000 0.02427 0.04132 0.04435 -0.01702 0.00962 -0.00247 0.03665 0.03052 0.00093 0.00105 0.00066 0.00000 0.00914 0.01202 0.01169 0.01000 0.00864 0.00876 0.00466 H1 0.01527 0.46067 0.03558 1.00000 0.04398 0.00000 0.00000 C8 -0.30425 0.66086 0.18673 1.00000 0.02395 0.05633 0.06749 0.00655 0.01634 0.01704 0.04926 0.03766 0.00098 0.00113 0.00076 0.00000 0.00997 0.01415 0.01445 0.01154 0.01011 0.00968 0.00555 H8A -0.30524 0.64597 0.15448 1.00000 0.05911 0.00000 0.00000 H8B -0.34938 0.65713 0.20533 1.00000 0.05911 0.00000 0.00000 C3 0.20386 0.53191 0.18755 1.00000 0.07068 0.02723 0.04136 -0.00845 0.00086 0.00981 0.04642 0.03418 0.00120 0.00110 0.00064 0.00000 0.01545 0.01163 0.01234 0.00964 0.01083 0.01040 0.00527 H3 0.18085 0.48481 0.19708 1.00000 0.05570 0.00000 0.00000 C6 -0.01724 0.60978 0.32843 1.00000 0.06011 0.06301 0.05174 -0.01011 0.00409 0.00519 0.05828 0.03871 0.00109 0.00135 0.00080 0.00000 0.01380 0.01569 0.01467 0.01262 0.01144 0.01165 0.00586 H6A -0.00419 0.66198 0.33455 1.00000 0.06994 0.00000 0.00000 H6B -0.02697 0.57557 0.35390 1.00000 0.06994 0.00000 0.00000 C21 -0.15835 0.94063 0.19873 1.00000 0.06328 0.03960 0.02919 -0.01175 0.00996 0.00538 0.04402 0.03343 0.00110 0.00113 0.00060 0.00000 0.01377 0.01263 0.01096 0.00947 0.00974 0.00994 0.00514 H21 -0.14423 0.99217 0.20593 1.00000 0.05283 0.00000 0.00000 C14 0.19095 0.72764 -0.07256 1.00000 0.07171 0.05593 0.05113 -0.00647 0.03849 -0.01972 0.05959 0.03874 0.00118 0.00119 0.00075 0.00000 0.01463 0.01461 0.01375 0.01191 0.01175 0.01202 0.00623 H14A 0.21354 0.76300 -0.05108 1.00000 0.07151 0.00000 0.00000 H14B 0.21400 0.71875 -0.10244 1.00000 0.07151 0.00000 0.00000 C11 -0.15636 0.79790 -0.03591 1.00000 0.08470 0.10451 0.02592 0.01339 0.01185 -0.02472 0.07171 0.04449 0.00158 0.00169 0.00072 0.00000 0.01803 0.02183 0.01222 0.01363 0.01186 0.01524 0.00830 H11 -0.20896 0.80332 -0.02801 1.00000 0.08605 0.00000 0.00000 C23 -0.07214 0.98630 0.04494 1.00000 0.01922 0.06509 0.04602 0.01966 -0.00252 0.01046 0.04344 0.03442 0.00088 0.00121 0.00070 0.00000 0.00936 0.01524 0.01229 0.01132 0.00867 0.00945 0.00528 H23 -0.06838 0.99084 0.01161 1.00000 0.05213 0.00000 0.00000 C18 0.33442 0.78214 0.17854 1.00000 0.04603 0.05945 0.06508 -0.00668 0.01029 -0.02999 0.05685 0.03270 0.00112 0.00128 0.00071 0.00000 0.01253 0.01524 0.01490 0.01229 0.01103 0.01162 0.00611 H18A 0.33031 0.72916 0.18660 1.00000 0.06822 0.00000 0.00000 H18B 0.38314 0.80651 0.17833 1.00000 0.06822 0.00000 0.00000 C16 0.21508 0.97576 0.05746 1.00000 0.02560 0.06727 0.05810 -0.00940 0.00442 -0.00765 0.05032 0.03245 0.00101 0.00126 0.00067 0.00000 0.00967 0.01650 0.01355 0.01194 0.00946 0.00996 0.00560 H16A 0.17041 1.00107 0.06870 1.00000 0.06039 0.00000 0.00000 H16B 0.25962 1.00482 0.05011 1.00000 0.06039 0.00000 0.00000 C22 -0.22995 0.91759 0.20328 1.00000 0.00898 0.07116 0.07933 -0.03939 0.00911 0.00352 0.05316 0.03130 0.00087 0.00125 0.00068 0.00000 0.00884 0.01557 0.01560 0.01267 0.00934 0.00917 0.00616 H22A -0.24344 0.86591 0.19598 1.00000 0.06379 0.00000 0.00000 H22B -0.26803 0.95267 0.21385 1.00000 0.06379 0.00000 0.00000 C20 0.03914 0.92333 0.31471 1.00000 0.05051 0.07722 0.04439 -0.00337 0.00423 -0.02176 0.05738 0.03539 0.00114 0.00134 0.00072 0.00000 0.01248 0.01781 0.01319 0.01234 0.01049 0.01215 0.00609 H20A -0.00072 0.94780 0.29750 1.00000 0.06885 0.00000 0.00000 H20B 0.05446 0.94320 0.34449 1.00000 0.06885 0.00000 0.00000 C15 0.21525 0.89852 0.05193 1.00000 0.04795 0.01729 0.05592 0.01228 0.00164 -0.01536 0.04039 0.03057 0.00103 0.00102 0.00066 0.00000 0.01122 0.01047 0.01273 0.00969 0.00957 0.00868 0.00481 H15 0.26050 0.87433 0.04065 1.00000 0.04847 0.00000 0.00000 C9 -0.16242 0.53043 0.06150 1.00000 0.03812 0.06223 0.03559 -0.00721 0.00748 -0.01234 0.04532 0.03263 0.00103 0.00121 0.00068 0.00000 0.01107 0.01471 0.01177 0.01043 0.00926 0.01074 0.00520 H9 -0.15040 0.50699 0.03212 1.00000 0.05438 0.00000 0.00000 C12 -0.13499 0.81741 -0.07690 1.00000 0.08406 0.11226 0.30279 -0.08998 -0.05120 -0.00290 0.16637 0.05115 0.00182 0.00186 0.00101 0.00000 0.02351 0.03150 0.05899 0.03829 0.03305 0.02145 0.01906 H12A -0.08270 0.81256 -0.08568 1.00000 0.19964 0.00000 0.00000 H12B -0.17123 0.83692 -0.09886 1.00000 0.19964 0.00000 0.00000 C19 0.07321 0.86180 0.29726 1.00000 0.03505 0.01826 0.03950 -0.00556 -0.00650 -0.00025 0.03094 0.02773 0.00094 0.00097 0.00060 0.00000 0.00982 0.00980 0.01100 0.00872 0.00864 0.00800 0.00421 H19 0.11284 0.83874 0.31538 1.00000 0.03712 0.00000 0.00000 C10 -0.20845 0.49677 0.08994 1.00000 0.03901 0.03397 0.15745 0.01390 -0.03271 0.00692 0.07681 0.04082 0.00114 0.00123 0.00106 0.00000 0.01238 0.01332 0.02572 0.01535 0.01562 0.01027 0.00832 H10A -0.22065 0.51998 0.11936 1.00000 0.09217 0.00000 0.00000 H10B -0.23044 0.44856 0.08164 1.00000 0.09217 0.00000 0.00000 C4 0.27507 0.53366 0.18952 1.00000 0.03547 0.03143 0.12026 0.01546 -0.00833 -0.00718 0.06239 0.03621 0.00112 0.00119 0.00083 0.00000 0.01177 0.01256 0.02064 0.01296 0.01241 0.00957 0.00672 H4A 0.30187 0.57897 0.18051 1.00000 0.07486 0.00000 0.00000 H4B 0.30261 0.48969 0.20005 1.00000 0.07486 0.00000 0.00000 Final Structure Factor Calculation for S93 in Pbca Total number of l.s. parameters = 487 Maximum vector length = 511 Memory required = 5202 / 22995 wR2 = 0.3783 before cycle 21 for 7552 data and 0 / 487 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0808 * P )^2 + 250.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1434 for 3039 Fo > 4sig(Fo) and 0.3015 for all 7552 data wR2 = 0.3783, GooF = S = 1.037, Restrained GooF = 1.037 for all data Occupancy sum of asymmetric unit = 54.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0406 0.0274 0.0218 Si1 0.0310 0.0277 0.0219 Si4 0.0401 0.0330 0.0205 Si2 0.0443 0.0353 0.0233 Si6 0.0439 0.0235 0.0219 Si3 0.0434 0.0307 0.0255 Si10 0.0404 0.0274 0.0247 Si9 0.0418 0.0342 0.0266 Si7 0.0390 0.0324 0.0246 Si11 0.0417 0.0290 0.0221 Si8 0.0471 0.0307 0.0234 Si12 0.0408 0.0282 0.0240 Si5 0.0427 0.0342 0.0223 O1 0.0497 0.0323 0.0259 O12 0.0598 0.0390 0.0240 O6 0.0504 0.0347 0.0147 O4 0.0886 0.0272 0.0171 O14 0.0570 0.0440 0.0244 O11 0.0594 0.0350 0.0156 O10 0.0547 0.0396 0.0191 O13 0.0634 0.0367 0.0297 O3 0.0520 0.0336 0.0167 O8 0.0610 0.0300 0.0179 O5 0.0621 0.0408 0.0260 O7 0.0503 0.0338 0.0309 O9 0.0565 0.0335 0.0194 O15 0.0536 0.0365 0.0240 O2 0.0563 0.0316 0.0211 O16 0.0483 0.0445 0.0173 O17 0.0554 0.0441 0.0048 C7 0.0616 0.0443 0.0354 O18 0.0837 0.0382 0.0206 C2 0.0726 0.0370 0.0226 C5 0.0671 0.0461 0.0253 C13 0.0735 0.0480 0.0277 C24 0.0814 0.0371 0.0013 C17 0.0620 0.0288 0.0191 C1 0.0796 0.0545 0.0136 C8 0.0728 0.0449 0.0215 C3 0.0697 0.0617 0.0435 C6 0.0662 0.0472 0.0187 C21 0.1086 0.0501 0.0201 C14 0.1215 0.0741 0.0195 C11 0.0784 0.0368 0.0151 C23 0.0892 0.0598 0.0216 C18 0.0747 0.0522 0.0240 C16 0.1150 0.0382 0.0062 C22 0.0900 0.0445 0.0377 C20 0.0605 0.0528 0.0079 C15 0.0701 0.0369 0.0290 C9 0.3469 0.0974 0.0548 C12 may be split into -0.1375 0.8124 -0.0688 and -0.1325 0.8225 -0.0850 0.0449 0.0312 0.0167 C19 0.1669 0.0420 0.0216 C10 0.1239 0.0380 0.0253 C4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.027 0.034 0.043 0.055 0.072 0.104 1.000 Number in group 823. 727. 793. 726. 716. 755. 766. 750. 744. 752. GooF 1.074 1.046 1.080 1.006 1.065 1.039 1.081 0.984 0.948 1.027 K 30.520 5.023 2.326 1.497 1.372 1.257 1.162 1.071 1.052 0.983 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.79 inf Number in group 805. 728. 732. 762. 760. 749. 752. 752. 754. 758. GooF 0.816 0.832 0.822 0.863 0.827 0.916 1.030 1.293 1.284 1.438 K 1.481 1.264 1.165 1.167 1.064 1.038 1.035 1.061 1.050 1.016 R1 0.565 0.511 0.466 0.409 0.329 0.297 0.194 0.165 0.147 0.125 Recommended weighting scheme: WGHT 0.0679 244.5761 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)/su Fc/Fc(max) Resolution(A) 1 4 8 9668.93 1426.88 6.95 0.044 2.71 1 3 20 7403.54 3.61 6.67 0.002 1.37 9 7 8 5267.62 2.93 6.11 0.002 1.40 7 4 12 5457.25 232.02 5.95 0.018 1.59 7 6 14 5644.78 219.87 5.95 0.017 1.38 3 2 6 7923.98 1356.01 5.81 0.043 3.38 4 9 4 42278.54 18342.55 5.67 0.157 1.71 2 4 3 12241.81 3812.03 5.67 0.072 3.59 2 8 11 4904.71 1.30 5.48 0.001 1.63 11 2 6 4526.43 259.98 5.47 0.019 1.48 6 5 6 5964.92 649.54 5.46 0.030 2.02 10 4 13 4399.01 0.05 5.41 0.000 1.30 11 2 8 7902.04 1702.33 5.35 0.048 1.43 10 4 6 3718.70 98.79 5.24 0.012 1.53 9 7 12 11427.13 2166.11 5.19 0.054 1.28 3 10 6 11078.05 2166.79 5.17 0.054 1.57 1 6 12 12115.74 3707.40 5.16 0.071 1.82 5 8 8 6114.06 637.40 5.14 0.029 1.63 2 6 1 17049.03 2178.57 5.03 0.054 2.73 2 8 13 4086.34 65.65 5.02 0.009 1.51 3 7 15 7728.73 898.00 4.85 0.035 1.45 7 6 8 3836.86 326.38 4.74 0.021 1.67 8 9 9 5877.25 407.52 4.72 0.023 1.31 8 1 8 3421.94 149.08 4.70 0.014 1.85 5 12 1 6574.92 862.47 4.69 0.034 1.33 4 8 3 3782.80 205.40 4.63 0.017 1.90 2 5 2 3977.39 442.71 4.61 0.024 3.14 2 5 6 12732.57 4840.98 4.54 0.081 2.66 7 2 6 3159.99 107.20 4.53 0.012 2.14 8 9 4 5073.80 684.49 4.51 0.030 1.42 4 7 2 3482.67 17.24 4.50 0.005 2.13 7 6 2 2379.82 7.50 4.39 0.003 1.87 10 3 7 4389.09 829.50 4.30 0.033 1.54 4 12 2 7555.29 1534.16 4.27 0.045 1.37 2 5 15 10809.53 3985.19 4.26 0.073 1.63 7 10 6 15776.76 6018.24 4.25 0.090 1.36 2 10 5 5634.62 860.87 4.25 0.034 1.63 3 6 1 6021.61 994.66 4.22 0.037 2.58 4 5 10 3871.13 630.16 4.21 0.029 1.96 4 2 4 7512.95 2702.18 4.20 0.060 3.42 7 2 9 6494.07 1524.64 4.19 0.045 1.91 9 11 2 3213.82 3.54 4.18 0.002 1.22 9 4 12 2829.50 99.52 4.18 0.012 1.42 10 8 6 3370.88 180.69 4.18 0.016 1.31 3 7 3 3033.34 139.76 4.12 0.014 2.22 9 7 9 3634.77 1.46 4.03 0.001 1.37 10 8 9 3930.42 620.69 4.03 0.029 1.25 3 1 9 6284.73 2125.50 3.98 0.054 2.73 3 5 17 2911.08 0.05 3.94 0.000 1.45 5 1 7 4505.92 982.11 3.94 0.036 2.61 Bond lengths and angles Si1 - Distance Angles O7 1.5986 (0.0122) O1 1.6023 (0.0112) 108.75 (0.63) O5 1.6225 (0.0109) 106.88 (0.62) 107.19 (0.62) C1 1.8353 (0.0184) 111.67 (0.77) 109.37 (0.77) 112.79 (0.70) Si1 - O7 O1 O5 Si4 - Distance Angles O10 1.5855 (0.0120) O4 1.6073 (0.0117) 108.37 (0.65) O3 1.6129 (0.0121) 109.76 (0.61) 108.61 (0.65) C7 1.8307 (0.0167) 113.00 (0.69) 106.90 (0.69) 110.07 (0.75) Si4 - O10 O4 O3 Si2 - Distance Angles O2 1.5688 (0.0122) O8 1.5914 (0.0118) 110.96 (0.66) O1 1.6117 (0.0115) 108.47 (0.61) 108.36 (0.63) C3 1.8524 (0.0193) 110.19 (0.80) 108.65 (0.79) 110.20 (0.73) Si2 - O2 O8 O1 Si6 - Distance Angles O11 1.6017 (0.0117) O6 1.6096 (0.0124) 109.58 (0.65) O18 1.6242 (0.0133) 109.04 (0.63) 108.65 (0.67) C11 1.8950 (0.0257) 112.56 (0.91) 107.90 (0.90) 109.03 (1.02) Si6 - O11 O6 O18 Si3 - Distance Angles O3 1.6104 (0.0120) O9 1.6228 (0.0121) 110.07 (0.63) O2 1.6538 (0.0121) 108.83 (0.64) 109.75 (0.62) C5 1.8311 (0.0197) 108.51 (0.72) 108.87 (0.84) 110.79 (0.75) Si3 - O3 O9 O2 Si10 - Distance Angles O15 1.5961 (0.0116) O9 1.6287 (0.0121) 108.66 (0.61) O14 1.6400 (0.0124) 110.02 (0.63) 108.73 (0.62) C19 1.7928 (0.0174) 110.62 (0.74) 109.13 (0.73) 109.64 (0.73) Si10 - O15 O9 O14 Si9 - Distance Angles O14 1.5820 (0.0131) O13 1.6022 (0.0116) 109.36 (0.62) O8 1.6144 (0.0117) 109.56 (0.64) 107.28 (0.64) C17 1.8231 (0.0157) 110.27 (0.75) 109.70 (0.79) 110.62 (0.74) Si9 - O14 O13 O8 Si7 - Distance Angles O7 1.6089 (0.0125) O12 1.6137 (0.0117) 108.12 (0.65) O11 1.6260 (0.0120) 109.28 (0.65) 109.90 (0.63) C13 1.8567 (0.0194) 110.12 (0.77) 108.86 (0.75) 110.51 (0.76) Si7 - O7 O12 O11 Si11 - Distance Angles O16 1.6135 (0.0119) O15 1.6098 (0.0116) 108.46 (0.62) O10 1.6367 (0.0122) 109.42 (0.64) 109.39 (0.60) C21 1.8525 (0.0183) 109.55 (0.74) 108.79 (0.74) 111.19 (0.76) Si11 - O16 O15 O10 Si8 - Distance Angles O13 1.6118 (0.0115) O12 1.6222 (0.0121) 107.94 (0.64) O17 1.6709 (0.0116) 109.34 (0.62) 111.33 (0.61) C15 1.8336 (0.0169) 113.01 (0.75) 108.20 (0.77) 107.05 (0.74) Si8 - O13 O12 O17 Si12 - Distance Angles O18 1.5913 (0.0131) O16 1.5990 (0.0120) 111.00 (0.67) O17 1.6075 (0.0110) 109.79 (0.66) 109.02 (0.64) C23 1.8540 (0.0190) 110.33 (0.79) 110.74 (0.81) 105.83 (0.72) Si12 - O18 O16 O17 Si5 - Distance Angles O6 1.6083 (0.0126) O4 1.6200 (0.0116) 108.80 (0.64) O5 1.6257 (0.0114) 107.16 (0.60) 106.11 (0.58) C9 1.8513 (0.0207) 110.39 (0.78) 111.59 (0.75) 112.58 (0.77) Si5 - O6 O4 O5 O1 - Distance Angles Si1 1.6023 (0.0112) Si2 1.6117 (0.0115) 154.01 (0.77) O1 - Si1 O12 - Distance Angles Si7 1.6137 (0.0117) Si8 1.6222 (0.0121) 151.91 (0.75) O12 - Si7 O6 - Distance Angles Si5 1.6083 (0.0126) Si6 1.6096 (0.0124) 141.80 (0.78) O6 - Si5 O4 - Distance Angles Si4 1.6073 (0.0117) Si5 1.6200 (0.0116) 149.83 (0.68) O4 - Si4 O14 - Distance Angles Si9 1.5820 (0.0131) Si10 1.6400 (0.0123) 151.16 (0.85) O14 - Si9 O11 - Distance Angles Si6 1.6017 (0.0116) Si7 1.6260 (0.0120) 149.91 (0.84) O11 - Si6 O10 - Distance Angles Si4 1.5855 (0.0120) Si11 1.6367 (0.0122) 163.70 (0.82) O10 - Si4 O13 - Distance Angles Si9 1.6022 (0.0116) Si8 1.6118 (0.0115) 153.87 (0.84) O13 - Si9 O3 - Distance Angles Si3 1.6104 (0.0120) Si4 1.6129 (0.0121) 153.56 (0.84) O3 - Si3 O8 - Distance Angles Si2 1.5914 (0.0118) Si9 1.6144 (0.0117) 148.81 (0.75) O8 - Si2 O5 - Distance Angles Si1 1.6225 (0.0109) Si5 1.6257 (0.0114) 146.33 (0.82) O5 - Si1 O7 - Distance Angles Si1 1.5986 (0.0122) Si7 1.6089 (0.0125) 148.36 (0.85) O7 - Si1 O9 - Distance Angles Si3 1.6228 (0.0121) Si10 1.6287 (0.0121) 154.27 (0.85) O9 - Si3 O15 - Distance Angles Si10 1.5961 (0.0116) Si11 1.6098 (0.0116) 151.32 (0.80) O15 - Si10 O2 - Distance Angles Si2 1.5688 (0.0122) Si3 1.6538 (0.0121) 153.40 (0.83) O2 - Si2 O16 - Distance Angles Si12 1.5990 (0.0120) Si11 1.6135 (0.0119) 153.67 (0.83) O16 - Si12 O17 - Distance Angles Si12 1.6075 (0.0110) Si8 1.6709 (0.0116) 142.50 (0.82) O17 - Si12 C7 - Distance Angles C8 1.3023 (0.0236) Si4 1.8307 (0.0166) 126.58 (1.47) H7 0.9500 116.71 116.71 C7 - C8 Si4 O18 - Distance Angles Si12 1.5913 (0.0131) Si6 1.6242 (0.0133) 154.69 (0.86) O18 - Si12 C2 - Distance Angles C1 1.2833 (0.0237) H2A 0.9500 120.00 H2B 0.9500 120.00 120.00 C2 - C1 H2A C5 - Distance Angles C6 1.2850 (0.0260) Si3 1.8311 (0.0197) 124.59 (1.74) H5 0.9500 117.71 117.71 C5 - C6 Si3 C13 - Distance Angles C14 1.2954 (0.0244) Si7 1.8567 (0.0193) 122.33 (1.60) H13 0.9500 118.84 118.83 C13 - C14 Si7 C24 - Distance Angles C23 1.3085 (0.0254) H24A 0.9500 120.00 H24B 0.9500 120.00 120.00 C24 - C23 H24A C17 - Distance Angles C18 1.3315 (0.0252) Si9 1.8231 (0.0156) 124.03 (1.41) H17 0.9500 117.98 117.98 C17 - C18 Si9 C1 - Distance Angles C2 1.2833 (0.0237) Si1 1.8353 (0.0183) 125.66 (1.55) H1 0.9500 117.17 117.17 C1 - C2 Si1 C8 - Distance Angles C7 1.3023 (0.0236) H8A 0.9500 120.00 H8B 0.9500 120.00 120.00 C8 - C7 H8A C3 - Distance Angles C4 1.2449 (0.0240) Si2 1.8524 (0.0192) 128.99 (1.77) H3 0.9500 115.51 115.51 C3 - C4 Si2 C6 - Distance Angles C5 1.2850 (0.0260) H6A 0.9500 120.00 H6B 0.9500 120.00 120.00 C6 - C5 H6A C21 - Distance Angles C22 1.3187 (0.0237) Si11 1.8525 (0.0183) 118.60 (1.54) H21 0.9500 120.70 120.70 C21 - C22 Si11 C14 - Distance Angles C13 1.2954 (0.0243) H14A 0.9500 120.00 H14B 0.9500 120.00 120.00 C14 - C13 H14A C11 - Distance Angles C12 1.2660 (0.0191) Si6 1.8950 (0.0257) 123.32 (2.72) H11 0.9500 118.35 118.33 C11 - C12 Si6 C23 - Distance Angles C24 1.3085 (0.0254) Si12 1.8540 (0.0190) 123.03 (1.58) H23 0.9500 118.49 118.49 C23 - C24 Si12 C18 - Distance Angles C17 1.3315 (0.0252) H18A 0.9500 120.00 H18B 0.9500 120.00 120.00 C18 - C17 H18A C16 - Distance Angles C15 1.3496 (0.0251) H16A 0.9500 120.00 H16B 0.9500 120.00 120.00 C16 - C15 H16A C22 - Distance Angles C21 1.3187 (0.0238) H22A 0.9500 120.00 H22B 0.9500 120.00 120.00 C22 - C21 H22A C20 - Distance Angles C19 1.3185 (0.0253) H20A 0.9500 120.00 H20B 0.9500 120.00 120.00 C20 - C19 H20A C15 - Distance Angles C16 1.3496 (0.0251) Si8 1.8336 (0.0169) 122.65 (1.52) H15 0.9500 118.67 118.67 C15 - C16 Si8 C9 - Distance Angles C10 1.2793 (0.0277) Si5 1.8513 (0.0207) 120.63 (1.79) H9 0.9500 119.68 119.68 C9 - C10 Si5 C12 - Distance Angles C11 1.2660 (0.0190) H12A 0.9500 120.03 H12B 0.9500 119.97 120.00 C12 - C11 H12A C19 - Distance Angles C20 1.3185 (0.0253) Si10 1.7928 (0.0174) 124.30 (1.50) H19 0.9500 117.85 117.85 C19 - C20 Si10 C10 - Distance Angles C9 1.2793 (0.0277) H10A 0.9500 120.00 H10B 0.9500 120.00 120.00 C10 - C9 H10A C4 - Distance Angles C3 1.2449 (0.0240) H4A 0.9500 120.00 H4B 0.9500 120.00 120.00 C4 - C3 H4A FMAP and GRID set by program FMAP 2 1 20 GRID -1.471 -2 -1 1.471 2 1 R1 = 0.3007 for 7552 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.98 at 0.2085 0.1634 0.0501 [ 0.85 A from H11 ] Deepest hole -0.73 at 0.2230 0.1787 0.3548 [ 1.33 A from O4 ] Mean = 0.00, Rms deviation from mean = 0.16 e/A^3, Highest memory used = 5746 / 51937 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2085 0.8366 -0.0501 1.00000 0.05 0.98 0.85 H11 1.20 C11 1.53 H12B 1.53 C12 Q2 1 -0.0133 0.7572 0.2897 1.00000 0.05 0.68 1.37 O9 2.05 SI10 2.09 H6A 2.20 H18B Q3 1 0.1689 0.8885 0.0816 1.00000 0.05 0.64 1.18 SI8 1.18 C15 1.85 C16 1.93 O13 Q4 1 0.0563 0.5996 0.1320 1.00000 0.05 0.64 1.11 O1 1.73 SI1 1.75 SI2 1.91 O2 Q5 1 0.1447 0.9180 0.1053 1.00000 0.05 0.63 1.80 SI8 1.83 H16A 1.98 C15 2.02 O17 Q6 1 -0.0551 1.0199 0.1493 1.00000 0.05 0.62 1.65 H24A 1.73 H6B 2.10 C6 2.16 O16 Q7 1 0.0779 0.7438 0.0915 1.00000 0.05 0.61 1.57 O13 2.03 SI8 2.09 O12 2.71 O1 Q8 1 0.1275 0.7473 0.0846 1.00000 0.05 0.58 1.28 O13 1.67 SI8 1.70 O12 2.54 SI9 Q9 1 0.0694 0.8602 0.1567 1.00000 0.05 0.56 1.88 O14 1.94 O13 2.30 O15 2.31 O16 Q10 1 0.0513 0.8538 0.3316 1.00000 0.05 0.54 1.05 C19 1.20 H19 1.31 C20 1.59 H20B Shortest distances between peaks (including symmetry equivalents) 7 8 0.89 3 5 0.94 5 9 2.20 2 10 2.34 3 8 2.56 7 9 2.74 4 7 2.78 3 9 2.79 3 7 2.98 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 0.02: 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. 1.63: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 18.81: Structure factors and derivatives 43.08: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 3.33: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 16:12:17 Total CPU time: 67.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++