+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:39:44 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S92 in P-1 CELL 0.71069 6.090 8.114 18.467 101.11 95.30 106.29 ZERR 2.00 0.001 0.002 0.004 0.03 0.03 0.03 LATT 1 SFAC C H N O SI BR UNIT 28 48 2 4 2 2 V = 849.03 F(000) = 360.0 Mu = 2.49 mm-1 Cell Wt = 692.68 Rho = 1.355 L.S. 4 CONF FMAP 2 PLAN 10 WGHT 0.0129 0.0000 FVAR 2.27130 BR1 6 0.28374 0.68474 0.00396 11.00000 0.03520 0.03139 = 0.03514 0.01329 -0.00365 0.00561 SI1 5 -0.09095 0.99592 -0.31841 11.00000 0.02767 0.03479 = 0.02335 0.00829 0.00252 0.01171 O1 4 -0.19706 0.57333 -0.18477 11.00000 0.02727 0.03202 = 0.03892 0.01218 -0.00598 -0.00211 AFIX 147 H1 2 -0.30029 0.49963 -0.17246 11.00000 -1.50000 AFIX 0 O2 4 0.06503 0.92518 -0.25923 11.00000 0.02641 0.02708 = 0.01856 0.00217 0.00199 0.00973 N1 3 0.39155 1.32373 -0.15537 11.00000 0.03350 0.01672 = 0.04135 0.00978 0.00190 0.00324 C1 1 0.13446 0.90489 -0.07836 11.00000 0.02284 0.02265 = 0.02493 0.00636 0.00449 0.00621 AFIX 13 H1A 2 0.21878 0.99437 -0.03339 11.00000 -1.20000 AFIX 0 C2 1 0.04431 0.71988 -0.06587 11.00000 0.02079 0.02931 = 0.02842 0.01179 0.00757 0.00553 AFIX 13 H2 2 -0.10302 0.70196 -0.04649 11.00000 -1.20000 AFIX 0 C3 1 0.01713 0.59652 -0.14038 11.00000 0.02810 0.01966 = 0.02942 0.00570 -0.00188 0.00014 AFIX 13 H3 2 0.03274 0.48284 -0.13422 11.00000 -1.20000 AFIX 0 C4 1 0.21288 0.69143 -0.17864 11.00000 0.02873 0.02834 = 0.02623 0.00885 0.00536 0.01198 AFIX 23 H4A 2 0.34609 0.64996 -0.17113 11.00000 -1.20000 H4B 2 0.16133 0.66916 -0.23189 11.00000 -1.20000 AFIX 0 C5 1 0.27611 0.88845 -0.14304 11.00000 0.01313 0.02032 = 0.02707 0.00474 0.00595 0.00649 AFIX 13 H5 2 0.44281 0.94804 -0.12861 11.00000 -1.20000 AFIX 0 C6 1 0.14187 0.99343 -0.18266 11.00000 0.02007 0.02083 = 0.01933 0.00527 0.00182 0.00297 C7 1 -0.03649 0.96438 -0.12820 11.00000 0.02652 0.02560 = 0.02261 0.00848 0.00904 0.00841 AFIX 23 H7A 2 -0.18034 0.87206 -0.14996 11.00000 -1.20000 H7B 2 -0.06574 1.07159 -0.10392 11.00000 -1.20000 AFIX 0 C8 1 0.28181 1.18043 -0.16802 11.00000 0.02297 0.03068 = 0.01816 0.01008 0.00949 0.01648 C9 1 -0.28661 1.09827 -0.26904 11.00000 0.04585 0.05437 = 0.04078 0.00725 0.00321 0.02864 AFIX 137 H9A 2 -0.35877 1.15367 -0.30154 11.00000 -1.50000 H9B 2 -0.19934 1.18513 -0.22535 11.00000 -1.50000 H9C 2 -0.40351 1.00924 -0.25454 11.00000 -1.50000 AFIX 0 C10 1 0.11014 1.16320 -0.35695 11.00000 0.04721 0.06105 = 0.04064 0.02797 0.00621 0.01233 AFIX 137 H10A 2 0.02293 1.20306 -0.39210 11.00000 -1.50000 H10B 2 0.21503 1.11157 -0.38164 11.00000 -1.50000 H10C 2 0.19641 1.26141 -0.31704 11.00000 -1.50000 AFIX 0 C11 1 -0.25237 0.79409 -0.39168 11.00000 0.02976 0.04825 = 0.02617 0.00188 -0.00160 0.01528 C12 1 -0.41880 0.66301 -0.35627 11.00000 0.05608 0.04330 = 0.04128 0.00592 -0.01294 -0.00798 AFIX 137 H12A 2 -0.33333 0.63903 -0.31532 11.00000 -1.50000 H12B 2 -0.49236 0.55522 -0.39303 11.00000 -1.50000 H12C 2 -0.53444 0.71307 -0.33840 11.00000 -1.50000 AFIX 0 C13 1 -0.39063 0.84519 -0.45260 11.00000 0.04809 0.07552 = 0.02369 0.00722 -0.00539 0.01644 AFIX 137 H13A 2 -0.28617 0.92466 -0.47538 11.00000 -1.50000 H13B 2 -0.49548 0.90179 -0.43079 11.00000 -1.50000 H13C 2 -0.47688 0.74112 -0.48978 11.00000 -1.50000 AFIX 0 C14 1 -0.08123 0.70511 -0.42765 11.00000 0.05711 0.07782 = 0.04572 -0.01522 -0.00358 0.03119 AFIX 137 H14A 2 0.03289 0.79011 -0.44514 11.00000 -1.50000 H14B 2 -0.16483 0.60932 -0.46889 11.00000 -1.50000 H14C 2 -0.00601 0.66091 -0.39113 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for S92 in P1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 BR 1.140 Br1 - C2 Si1 - O2 C9 C10 C11 O1 - C3 O2 - C6 Si1 N1 - C8 C1 - C2 C5 C7 C2 - C3 C1 Br1 C3 - O1 C2 C4 C4 - C5 C3 C5 - C4 C1 C6 C6 - O2 C8 C7 C5 C7 - C6 C1 C8 - N1 C6 C9 - Si1 C10 - Si1 C11 - C13 C12 C14 Si1 C12 - C11 C13 - C11 C14 - C11 3586 Reflections read, of which 0 rejected -6 =< h =< 4, -7 =< k =< 9, -20 =< l =< 20, Max. 2-theta = 49.74 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 8351.07 183.38 2 1072.50 1 2 2 24265.33 392.16 2 2710.00 1 -2 3 7523.76 250.11 2 1427.50 1 1 3 31126.08 465.59 2 3576.50 1 -2 9 18256.80 372.37 2 2846.00 5 Inconsistent equivalents 2347 Unique reflections, of which 0 suppressed R(int) = 0.0442 R(sigma) = 0.1177 Friedel opposites merged Maximum memory for data reduction = 2113 / 23826 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 2663 / 223242 wR2 = 0.0675 before cycle 1 for 2347 data and 178 / 178 parameters GooF = S = 0.731; Restrained GooF = 0.731 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0129 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28135 0.00282 3.561 OSF Mean shift/esd = 0.205 Maximum = 3.561 for OSF Max. shift = 0.016 A for H9C Max. dU = 0.001 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2663 / 223242 wR2 = 0.0671 before cycle 2 for 2347 data and 178 / 178 parameters GooF = S = 0.730; Restrained GooF = 0.730 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0129 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28293 0.00281 0.559 OSF Mean shift/esd = 0.068 Maximum = 0.559 for OSF Max. shift = 0.009 A for H9C Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2663 / 223242 wR2 = 0.0671 before cycle 3 for 2347 data and 178 / 178 parameters GooF = S = 0.730; Restrained GooF = 0.730 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0129 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28300 0.00281 0.026 OSF Mean shift/esd = 0.004 Maximum = -0.062 for tors H9A Max. shift = 0.002 A for H9B Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2663 / 223242 wR2 = 0.0672 before cycle 4 for 2347 data and 178 / 178 parameters GooF = S = 0.730; Restrained GooF = 0.730 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0129 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28300 0.00282 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.013 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for C10 Largest correlation matrix elements 0.548 U12 C9 / U22 C9 0.529 U12 C8 / U22 C8 0.520 U12 C14 / U22 C14 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 -0.2999 0.4979 -0.1732 147 0.820 0.000 O1 C3 H1 H1A 0.2194 0.9945 -0.0334 13 0.980 0.000 C1 C2 C5 C7 H2 -0.1028 0.7023 -0.0465 13 0.980 0.000 C2 C3 C1 Br1 H3 0.0328 0.4829 -0.1342 13 0.980 0.000 C3 O1 C2 C4 H4A 0.3459 0.6501 -0.1712 23 0.970 0.000 C4 C5 C3 H4B 0.1610 0.6696 -0.2318 23 0.970 0.000 C4 C5 C3 H5 0.4430 0.9481 -0.1285 13 0.980 0.000 C5 C4 C1 C6 H7A -0.1800 0.8716 -0.1501 23 0.970 0.000 C7 C6 C1 H7B -0.0660 1.0712 -0.1041 23 0.970 0.000 C7 C6 C1 H9A -0.3555 1.1565 -0.3012 137 0.960 0.000 C9 Si1 H9A H9B -0.2003 1.1828 -0.2247 137 0.960 0.000 C9 Si1 H9A H9C -0.4063 1.0088 -0.2559 137 0.960 0.000 C9 Si1 H9A H10A 0.0232 1.2019 -0.3927 137 0.960 0.000 C10 Si1 H10A H10B 0.2167 1.1124 -0.3810 137 0.960 0.000 C10 Si1 H10A H10C 0.1948 1.2624 -0.3172 137 0.960 0.000 C10 Si1 H10A H12A -0.3329 0.6383 -0.3155 137 0.960 0.000 C12 C11 H12A H12B -0.4922 0.5551 -0.3932 137 0.960 0.000 C12 C11 H12A H12C -0.5341 0.7125 -0.3382 137 0.960 0.000 C12 C11 H12A H13A -0.2862 0.9239 -0.4757 137 0.960 0.000 C13 C11 H13A H13B -0.4951 0.9022 -0.4309 137 0.960 0.000 C13 C11 H13A H13C -0.4775 0.7407 -0.4897 137 0.960 0.000 C13 C11 H13A H14A 0.0316 0.7896 -0.4457 137 0.960 0.000 C14 C11 H14A H14B -0.1656 0.6085 -0.4686 137 0.960 0.000 C14 C11 H14A H14C -0.0050 0.6618 -0.3911 137 0.960 0.000 C14 C11 H14A S92 in P1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.28374 0.68472 0.00396 1.00000 0.03561 0.03183 0.03570 0.01346 -0.00370 0.00574 0.03515 0.00105 0.00008 0.00007 0.00003 0.00000 0.00028 0.00031 0.00033 0.00025 0.00020 0.00021 0.00017 Si1 -0.09097 0.99588 -0.31844 1.00000 0.02805 0.03518 0.02356 0.00827 0.00269 0.01191 0.02832 0.00273 0.00019 0.00018 0.00007 0.00000 0.00071 0.00089 0.00082 0.00069 0.00055 0.00063 0.00035 O1 -0.19725 0.57344 -0.18476 1.00000 0.02659 0.03283 0.04000 0.01247 -0.00640 -0.00197 0.03566 0.00627 0.00043 0.00043 0.00017 0.00000 0.00168 0.00228 0.00218 0.00174 0.00149 0.00151 0.00086 H1 -0.29994 0.49787 -0.17321 1.00000 0.05349 0.00000 0.00000 O2 0.06502 0.92505 -0.25922 1.00000 0.02675 0.02726 0.01831 0.00228 0.00203 0.00996 0.02426 0.00572 0.00040 0.00037 0.00015 0.00000 0.00156 0.00195 0.00184 0.00150 0.00123 0.00139 0.00073 N1 0.39168 1.32366 -0.15523 1.00000 0.03492 0.01629 0.04099 0.00990 0.00264 0.00266 0.03157 0.00807 0.00056 0.00051 0.00021 0.00000 0.00227 0.00252 0.00279 0.00214 0.00183 0.00194 0.00101 C1 0.13521 0.90497 -0.07834 1.00000 0.02272 0.02293 0.02583 0.00674 0.00454 0.00658 0.02369 0.00926 0.00062 0.00057 0.00024 0.00000 0.00235 0.00282 0.00286 0.00227 0.00188 0.00202 0.00108 H1A 0.21942 0.99449 -0.03336 1.00000 0.02843 0.00000 0.00000 C2 0.04454 0.72001 -0.06592 1.00000 0.02100 0.02947 0.02907 0.01252 0.00753 0.00564 0.02588 0.00920 0.00065 0.00058 0.00024 0.00000 0.00236 0.00302 0.00300 0.00249 0.00192 0.00209 0.00115 H2 -0.10275 0.70234 -0.04653 1.00000 0.03105 0.00000 0.00000 C3 0.01708 0.59660 -0.14032 1.00000 0.02864 0.01967 0.02907 0.00533 -0.00209 -0.00002 0.02783 0.00886 0.00063 0.00060 0.00024 0.00000 0.00258 0.00285 0.00304 0.00242 0.00205 0.00208 0.00118 H3 0.03280 0.48295 -0.13416 1.00000 0.03340 0.00000 0.00000 C4 0.21271 0.69172 -0.17857 1.00000 0.02729 0.02980 0.02699 0.00982 0.00546 0.01274 0.02662 0.00940 0.00065 0.00057 0.00025 0.00000 0.00254 0.00310 0.00290 0.00246 0.00197 0.00223 0.00115 H4A 0.34588 0.65015 -0.17118 1.00000 0.03195 0.00000 0.00000 H4B 0.16099 0.66965 -0.23180 1.00000 0.03195 0.00000 0.00000 C5 0.27626 0.88858 -0.14291 1.00000 0.01201 0.02049 0.02758 0.00450 0.00644 0.00684 0.01955 0.00872 0.00062 0.00054 0.00023 0.00000 0.00219 0.00274 0.00284 0.00222 0.00181 0.00192 0.00104 H5 0.44300 0.94807 -0.12855 1.00000 0.02346 0.00000 0.00000 C6 0.14192 0.99341 -0.18274 1.00000 0.02041 0.02045 0.01945 0.00534 0.00202 0.00269 0.02081 0.00875 0.00062 0.00057 0.00023 0.00000 0.00231 0.00273 0.00276 0.00218 0.00182 0.00196 0.00105 C7 -0.03638 0.96413 -0.12835 1.00000 0.02618 0.02634 0.02232 0.00886 0.00869 0.00907 0.02393 0.00895 0.00061 0.00057 0.00022 0.00000 0.00245 0.00295 0.00280 0.00236 0.00195 0.00212 0.00111 H7A -0.18003 0.87159 -0.15010 1.00000 0.02871 0.00000 0.00000 H7B -0.06602 1.07122 -0.10412 1.00000 0.02871 0.00000 0.00000 C8 0.28193 1.18047 -0.16806 1.00000 0.02338 0.03144 0.01824 0.01054 0.01046 0.01725 0.02131 0.01003 0.00067 0.00064 0.00023 0.00000 0.00253 0.00327 0.00268 0.00242 0.00190 0.00235 0.00107 C9 -0.28674 1.09828 -0.26914 1.00000 0.04678 0.05504 0.04051 0.00697 0.00341 0.02765 0.04567 0.01049 0.00071 0.00066 0.00027 0.00000 0.00297 0.00391 0.00348 0.00299 0.00240 0.00284 0.00144 H9A -0.35550 1.15650 -0.30118 1.00000 0.06851 0.00000 0.00000 H9B -0.20032 1.18280 -0.22470 1.00000 0.06851 0.00000 0.00000 H9C -0.40625 1.00881 -0.25589 1.00000 0.06851 0.00000 0.00000 C10 0.11027 1.16340 -0.35700 1.00000 0.04664 0.06311 0.04066 0.02846 0.00600 0.01350 0.04852 0.01088 0.00070 0.00070 0.00028 0.00000 0.00304 0.00432 0.00358 0.00322 0.00243 0.00289 0.00154 H10A 0.02322 1.20194 -0.39271 1.00000 0.07279 0.00000 0.00000 H10B 0.21673 1.11236 -0.38102 1.00000 0.07279 0.00000 0.00000 H10C 0.19479 1.26241 -0.31717 1.00000 0.07279 0.00000 0.00000 C11 -0.25222 0.79425 -0.39157 1.00000 0.02955 0.04832 0.02697 0.00223 -0.00065 0.01582 0.03536 0.00981 0.00070 0.00067 0.00026 0.00000 0.00271 0.00361 0.00304 0.00267 0.00211 0.00252 0.00129 C12 -0.41850 0.66263 -0.35629 1.00000 0.05796 0.04385 0.04104 0.00555 -0.01296 -0.00808 0.05458 0.01011 0.00075 0.00069 0.00028 0.00000 0.00333 0.00395 0.00372 0.00310 0.00261 0.00284 0.00162 H12A -0.33286 0.63830 -0.31547 1.00000 0.08187 0.00000 0.00000 H12B -0.49215 0.55507 -0.39317 1.00000 0.08187 0.00000 0.00000 H12C -0.53409 0.71252 -0.33824 1.00000 0.08187 0.00000 0.00000 C13 -0.39072 0.84503 -0.45270 1.00000 0.04868 0.07523 0.02268 0.00687 -0.00572 0.01505 0.05105 0.01024 0.00071 0.00072 0.00025 0.00000 0.00315 0.00453 0.00324 0.00304 0.00232 0.00298 0.00158 H13A -0.28623 0.92388 -0.47573 1.00000 0.07657 0.00000 0.00000 H13B -0.49507 0.90224 -0.43094 1.00000 0.07657 0.00000 0.00000 H13C -0.47752 0.74074 -0.48969 1.00000 0.07657 0.00000 0.00000 C14 -0.08150 0.70503 -0.42769 1.00000 0.05702 0.08001 0.04578 -0.01493 -0.00393 0.03183 0.06359 0.01129 0.00078 0.00075 0.00030 0.00000 0.00362 0.00504 0.00405 0.00349 0.00281 0.00345 0.00183 H14A 0.03162 0.78963 -0.44571 1.00000 0.09538 0.00000 0.00000 H14B -0.16563 0.60852 -0.46859 1.00000 0.09538 0.00000 0.00000 H14C -0.00500 0.66182 -0.39109 1.00000 0.09538 0.00000 0.00000 Final Structure Factor Calculation for S92 in P1 Total number of l.s. parameters = 178 Maximum vector length = 511 Memory required = 2485 / 25039 wR2 = 0.0671 before cycle 5 for 2347 data and 0 / 178 parameters GooF = S = 0.730; Restrained GooF = 0.730 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0129 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0343 for 1666 Fo > 4sig(Fo) and 0.0515 for all 2347 data wR2 = 0.0671, GooF = S = 0.730, Restrained GooF = 0.730 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0510 0.0300 0.0244 Br1 0.0354 0.0278 0.0218 Si1 0.0560 0.0309 0.0201 O1 0.0302 0.0246 0.0180 O2 0.0443 0.0359 0.0145 N1 0.0260 0.0233 0.0217 C1 0.0343 0.0260 0.0173 C2 0.0396 0.0267 0.0172 C3 0.0325 0.0257 0.0217 C4 0.0285 0.0205 0.0096 C5 0.0258 0.0190 0.0176 C6 0.0294 0.0249 0.0175 C7 0.0360 0.0168 0.0112 C8 0.0642 0.0402 0.0326 C9 0.0721 0.0466 0.0268 C10 0.0526 0.0302 0.0234 C11 0.0906 0.0477 0.0254 C12 0.0786 0.0550 0.0195 C13 0.1084 0.0481 0.0343 C14 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.055 0.074 0.094 0.119 0.142 0.169 0.210 0.278 1.000 Number in group 238. 231. 241. 235. 234. 232. 235. 235. 230. 236. GooF 0.352 0.378 0.490 0.574 0.553 0.562 0.591 0.712 0.839 1.520 K 2.289 1.059 0.994 0.988 0.982 1.003 1.003 1.005 0.995 1.014 Resolution(A) 0.84 0.92 0.96 1.01 1.07 1.14 1.22 1.35 1.54 1.95 inf Number in group 250. 222. 246. 223. 234. 235. 232. 234. 237. 234. GooF 0.425 0.443 0.422 0.486 0.474 0.598 0.604 0.653 1.025 1.455 K 1.009 1.029 1.023 1.022 1.023 1.022 1.014 0.999 1.003 1.001 R1 0.094 0.083 0.074 0.067 0.059 0.054 0.040 0.034 0.037 0.035 Recommended weighting scheme: WGHT 0.0106 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) 0 -3 7 2174.56 2856.70 7.78 0.397 2.05 3 -2 4 6238.81 5700.34 7.16 0.561 1.78 0 0 5 2794.84 3369.31 7.05 0.431 3.58 -1 1 1 12999.03 12094.72 6.95 0.817 5.20 2 0 7 2163.08 2453.34 5.66 0.368 1.78 0 -1 5 1961.59 2310.88 5.61 0.357 3.57 0 -2 1 1510.72 1776.37 5.02 0.313 3.89 3 -2 3 2798.61 2567.39 4.79 0.376 1.85 -1 -1 10 2178.20 2615.31 4.73 0.380 1.80 0 0 3 595.15 737.86 4.63 0.202 5.97 2 -3 4 6201.05 5762.09 4.47 0.564 2.10 -3 2 12 4075.71 3463.41 4.33 0.437 1.21 -1 1 7 1919.00 2235.42 4.18 0.351 2.30 -2 0 3 548.88 640.25 4.10 0.188 2.77 0 0 6 8056.83 7481.06 4.07 0.642 2.98 2 -3 5 1116.75 1285.45 4.05 0.266 2.00 2 -2 8 2277.86 2073.12 4.01 0.338 1.75 1 1 9 2743.62 2313.66 3.90 0.357 1.64 -2 0 6 6376.12 5906.72 3.84 0.571 2.26 -2 2 2 1430.22 1291.18 3.82 0.267 2.60 0 2 4 803.32 1001.83 3.80 0.235 2.61 -1 -2 3 5780.59 5346.80 3.77 0.543 2.81 -2 3 0 197.31 262.64 3.60 0.120 2.28 -1 -2 11 1325.57 1610.95 3.60 0.298 1.59 0 2 0 666.91 803.82 3.57 0.211 3.79 1 1 12 3617.35 3101.60 3.52 0.414 1.30 1 -5 6 2827.27 3257.04 3.50 0.424 1.53 -1 -3 6 1933.19 2215.67 3.49 0.350 1.95 -3 2 2 2445.84 2322.77 3.41 0.358 1.95 2 -1 9 3566.02 3190.30 3.33 0.419 1.61 0 -1 8 712.38 869.88 3.33 0.219 2.29 -2 0 2 577.83 631.03 3.32 0.187 2.88 0 -3 1 7969.53 7478.22 3.29 0.642 2.59 1 -4 11 4070.14 3603.60 3.25 0.446 1.39 1 2 1 602.06 738.04 3.24 0.202 2.67 -1 1 5 2298.31 2519.58 3.21 0.373 2.97 2 0 3 351.68 410.98 3.19 0.151 2.45 3 -1 5 2005.58 1803.01 3.13 0.315 1.69 -3 0 2 108.15 146.72 3.10 0.090 1.94 3 0 2 1676.00 1799.90 3.08 0.315 1.82 -1 -1 6 198.83 247.06 3.04 0.117 2.72 0 1 5 5289.04 4945.78 3.01 0.522 2.98 -1 -1 1 8880.63 8568.64 2.97 0.687 4.15 -1 2 2 2379.27 2571.46 2.96 0.377 3.30 -1 -4 4 1824.60 2082.40 2.92 0.339 1.69 -2 -2 1 2897.30 3091.45 2.88 0.413 2.06 1 -2 4 3424.53 3196.75 2.87 0.420 3.06 2 3 1 1589.57 1810.15 2.87 0.316 1.62 0 -1 6 1519.35 1352.09 2.87 0.273 3.02 -1 1 3 1074.04 1192.34 2.84 0.256 4.00 Selected torsion angles -30.77 ( 0.38) C9 - Si1 - O2 - C6 88.51 ( 0.37) C10 - Si1 - O2 - C6 -151.51 ( 0.33) C11 - Si1 - O2 - C6 -29.47 ( 0.38) C5 - C1 - C2 - C3 67.43 ( 0.43) C7 - C1 - C2 - C3 86.98 ( 0.32) C5 - C1 - C2 - Br1 -176.12 ( 0.29) C7 - C1 - C2 - Br1 -83.31 ( 0.39) C1 - C2 - C3 - O1 160.99 ( 0.26) Br1 - C2 - C3 - O1 32.94 ( 0.38) C1 - C2 - C3 - C4 -82.76 ( 0.33) Br1 - C2 - C3 - C4 94.66 ( 0.39) O1 - C3 - C4 - C5 -23.84 ( 0.40) C2 - C3 - C4 - C5 5.89 ( 0.39) C3 - C4 - C5 - C1 -91.28 ( 0.41) C3 - C4 - C5 - C6 14.11 ( 0.38) C2 - C1 - C5 - C4 -102.54 ( 0.33) C7 - C1 - C5 - C4 130.42 ( 0.31) C2 - C1 - C5 - C6 13.76 ( 0.30) C7 - C1 - C5 - C6 -56.88 ( 0.42) Si1 - O2 - C6 - C8 73.44 ( 0.47) Si1 - O2 - C6 - C7 177.27 ( 0.24) Si1 - O2 - C6 - C5 -27.62 ( 0.50) C4 - C5 - C6 - O2 -135.41 ( 0.35) C1 - C5 - C6 - O2 -153.84 ( 0.37) C4 - C5 - C6 - C8 98.37 ( 0.37) C1 - C5 - C6 - C8 93.86 ( 0.39) C4 - C5 - C6 - C7 -13.93 ( 0.31) C1 - C5 - C6 - C7 132.64 ( 0.37) O2 - C6 - C7 - C1 -97.33 ( 0.34) C8 - C6 - C7 - C1 13.69 ( 0.31) C5 - C6 - C7 - C1 -120.89 ( 0.39) C2 - C1 - C7 - C6 -13.94 ( 0.32) C5 - C1 - C7 - C6 -158.48 (17.33) O2 - C6 - C8 - N1 67.46 (17.46) C7 - C6 - C8 - N1 -29.46 (17.56) C5 - C6 - C8 - N1 -176.15 ( 0.29) O2 - Si1 - C11 - C13 64.48 ( 0.38) C9 - Si1 - C11 - C13 -58.69 ( 0.36) C10 - Si1 - C11 - C13 63.55 ( 0.33) O2 - Si1 - C11 - C12 -55.82 ( 0.37) C9 - Si1 - C11 - C12 -179.00 ( 0.30) C10 - Si1 - C11 - C12 -56.60 ( 0.37) O2 - Si1 - C11 - C14 -175.97 ( 0.33) C9 - Si1 - C11 - C14 60.85 ( 0.39) C10 - Si1 - C11 - C14 FMAP and GRID set by program FMAP 2 1 28 GRID -4.000 -2 -1 4.000 2 1 R1 = 0.0493 for 2347 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.8359 0.0454 0.0131 [ 0.61 A from H1A ] Deepest hole -0.33 at 0.1856 0.7191 0.0329 [ 0.90 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2537 / 25300 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1641 0.9546 -0.0131 1.00000 0.05 0.49 0.61 H1A 1.17 C1 1.87 C2 2.16 H2 Q2 1 0.4792 1.3736 -0.3078 1.00000 0.05 0.42 1.69 H10C 2.17 H12A 2.28 H9A 2.34 H10B Q3 1 -0.6422 0.6346 -0.3240 1.00000 0.05 0.31 0.87 H12C 1.51 C12 1.76 H12B 1.87 H12A Q4 1 -0.1198 0.5692 -0.1681 1.00000 0.05 0.25 0.55 O1 0.88 C3 1.07 H1 1.47 H3 Q5 1 0.0300 0.9592 -0.0994 1.00000 0.05 0.25 0.65 C7 0.97 C1 1.22 H7B 1.42 H7A Q6 1 -0.4849 0.5482 -0.2613 1.00000 0.05 0.24 1.57 H12A 2.06 H1 2.08 O1 2.16 C12 Q7 1 -0.3434 0.3186 -0.2029 1.00000 0.05 0.24 1.39 H1 1.60 H9B 1.91 N1 1.96 O1 Q8 1 0.3986 0.5870 -0.1324 1.00000 0.05 0.23 1.03 H4A 1.84 C4 2.08 N1 2.14 H3 Q9 1 0.2276 0.9559 -0.1561 1.00000 0.05 0.23 0.76 C5 0.84 C6 1.39 H5 1.67 C1 Q10 1 -0.3528 0.5201 -0.1358 1.00000 0.05 0.23 0.80 H1 1.41 O1 1.84 N1 2.14 H2 Shortest distances between peaks (including symmetry equivalents) 2 6 1.45 4 10 1.57 5 9 1.67 1 5 1.73 8 10 1.75 3 6 1.80 7 10 1.87 4 7 2.05 2 7 2.31 1 1 2.38 6 10 2.45 2 3 2.49 6 8 2.53 1 5 2.56 6 7 2.62 4 6 2.63 1 9 2.70 Time profile in seconds ----------------------- 0.19: 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. 0.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.61: Structure factors and derivatives 0.70: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:39:46 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++