+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:19:02 on 30-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT003 in P2(1)/c CELL 0.71073 14.2910 11.7090 13.3411 90.000 115.857 90.000 ZERR 4.00 0.0029 0.0023 0.0027 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI S UNIT 72 112 8 8 4 4 V = 2008.91 F(000) = 784.0 Mu = 0.23 mm-1 Cell Wt = 1458.30 Rho = 1.205 MERG 2 OMIT -3.00 55.00 OMIT 1 0 0 OMIT 6 4 5 EXTI 0.02375 FMAP 2 PLAN 10 SIZE 0.04 0.12 0.16 BOND WGHT 0.11260 0.09350 L.S. 4 TEMP -123.00 FVAR 0.36790 C1 1 -0.179343 0.021547 0.390824 11.00000 0.04941 0.04572 = 0.04338 0.00498 0.02229 0.00958 AFIX 137 H1A 2 -0.148745 0.059997 0.463318 11.00000 -1.50000 H1B 2 -0.178699 -0.061220 0.402025 11.00000 -1.50000 H1C 2 -0.251169 0.047539 0.348225 11.00000 -1.50000 AFIX 0 C2 1 -0.117360 0.049534 0.328057 11.00000 0.03514 0.02943 = 0.03559 0.00280 0.01664 0.00999 C3 1 -0.028455 0.116977 0.374938 11.00000 0.04229 0.03385 = 0.03405 -0.00211 0.01216 0.01053 AFIX 43 H3 2 -0.005650 0.144378 0.448909 11.00000 -1.20000 AFIX 0 C4 1 0.027713 0.145046 0.315382 11.00000 0.02838 0.02859 = 0.03498 -0.00331 0.00448 0.00574 AFIX 43 H4 2 0.088085 0.191459 0.348536 11.00000 -1.20000 AFIX 0 C5 1 -0.004569 0.105285 0.208267 11.00000 0.02269 0.02276 = 0.03238 -0.00211 0.00707 0.00583 C6 1 -0.093104 0.035797 0.159717 11.00000 0.02982 0.03342 = 0.03087 -0.00840 0.01238 -0.00487 AFIX 43 H6 2 -0.115274 0.007314 0.086201 11.00000 -1.20000 AFIX 0 C7 1 -0.147245 0.009581 0.220146 11.00000 0.03360 0.03889 = 0.03912 -0.00375 0.01636 -0.00567 AFIX 43 H7 2 -0.207198 -0.037475 0.187126 11.00000 -1.20000 AFIX 0 C8 1 0.236600 -0.096932 0.288918 11.00000 0.02198 0.02437 = 0.03565 0.00323 0.00644 -0.00174 C9 1 0.143944 -0.130946 0.308218 11.00000 0.03896 0.02700 = 0.04641 0.00564 0.01855 -0.00163 AFIX 137 H9A 2 0.136345 -0.077590 0.360788 11.00000 -1.50000 H9B 2 0.154244 -0.208412 0.339008 11.00000 -1.50000 H9C 2 0.081050 -0.128931 0.237396 11.00000 -1.50000 AFIX 0 C10 1 0.340235 -0.088312 0.393283 11.00000 0.03249 0.04012 = 0.03689 0.00904 0.00473 0.00044 AFIX 23 H10A 2 0.371546 -0.164700 0.417959 11.00000 -1.20000 H10B 2 0.331205 -0.050914 0.455045 11.00000 -1.20000 AFIX 0 C11 1 0.407583 -0.014411 0.354078 11.00000 0.02379 0.03496 = 0.05117 0.00604 0.00427 -0.00293 AFIX 23 H11A 2 0.433605 0.054466 0.401209 11.00000 -1.20000 H11B 2 0.467562 -0.058436 0.356199 11.00000 -1.20000 AFIX 0 C12 1 0.332545 0.018271 0.233434 11.00000 0.01688 0.03568 = 0.04018 0.00060 0.00944 -0.00024 C13 1 0.316120 -0.089613 0.164192 11.00000 0.01982 0.02920 = 0.04124 0.00101 0.00835 0.00606 C14 1 0.344268 -0.112381 0.084616 11.00000 0.03930 0.04204 = 0.06497 -0.00700 0.02559 -0.00267 AFIX 93 H14A 2 0.325063 -0.182896 0.045681 11.00000 -1.20000 H14B 2 0.383788 -0.058299 0.066115 11.00000 -1.20000 AFIX 0 C15 1 0.253120 -0.169235 0.200824 11.00000 0.02138 0.02575 = 0.04546 0.00312 0.00605 0.00491 AFIX 23 H15A 2 0.292006 -0.240203 0.233889 11.00000 -1.20000 H15B 2 0.185952 -0.189209 0.137709 11.00000 -1.20000 AFIX 0 C16 1 0.377701 0.270884 0.288638 11.00000 0.03753 0.04081 = 0.05719 -0.00577 0.01127 -0.01097 AFIX 137 H16A 2 0.396067 0.343808 0.265815 11.00000 -1.50000 H16B 2 0.430169 0.251075 0.363506 11.00000 -1.50000 H16C 2 0.309544 0.277638 0.289112 11.00000 -1.50000 AFIX 0 C17 1 0.507124 0.135092 0.202346 11.00000 0.03115 0.05899 = 0.09141 -0.00028 0.02626 -0.00942 AFIX 137 H17A 2 0.505620 0.077793 0.148119 11.00000 -1.50000 H17B 2 0.552412 0.108565 0.277800 11.00000 -1.50000 H17C 2 0.533868 0.207335 0.188173 11.00000 -1.50000 AFIX 0 C18 1 0.286870 0.201913 0.044521 11.00000 0.04427 0.04459 = 0.04724 0.00441 0.02021 -0.00649 AFIX 137 H18A 2 0.315176 0.270891 0.026338 11.00000 -1.50000 H18B 2 0.217117 0.217964 0.037943 11.00000 -1.50000 H18C 2 0.282924 0.140563 -0.007145 11.00000 -1.50000 AFIX 0 N1 3 0.145900 0.040671 0.140749 11.00000 0.01951 0.02262 = 0.02800 0.00016 0.00718 0.00211 AFIX 43 H1 2 0.137678 -0.001693 0.083004 11.00000 -1.20000 AFIX 0 N2 3 0.231941 0.023805 0.246418 11.00000 0.01758 0.02598 = 0.02887 0.00248 0.00526 -0.00166 O1 4 -0.009205 0.137608 0.013859 11.00000 0.02277 0.02754 = 0.03176 0.00530 0.00515 0.00268 O2 4 0.120350 0.243036 0.175883 11.00000 0.02726 0.02085 = 0.05497 -0.00802 0.00871 -0.00512 SI1 5 0.372616 0.157180 0.188892 11.00000 0.02286 0.03401 = 0.04838 0.00022 0.01226 -0.00724 S1 6 0.063286 0.140856 0.130291 11.00000 0.02051 0.02017 = 0.03685 -0.00078 0.00824 0.00019 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 01SOT003 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 S 1.030 C1 - C2 C2 - C3 C7 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 S1 C6 - C7 C5 C7 - C6 C2 C8 - C9 N2 C10 C15 C9 - C8 C10 - C8 C11 C11 - C12 C10 C12 - C13 N2 C11 Si1 C13 - C14 C15 C12 C14 - C13 C15 - C13 C8 C16 - Si1 C17 - Si1 C18 - Si1 N1 - N2 S1 N2 - N1 C8 C12 O1 - S1 O2 - S1 Si1 - C18 C16 C17 C12 S1 - O2 O1 N1 C5 h k l Fo^2 Sigma Why rejected 9 0 5 35.98 6.64 observed but should be systematically absent 10044 Reflections read, of which 329 rejected -16 =< h =< 17, -14 =< k =< 13, -16 =< l =< 15, Max. 2-theta = 54.98 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 65.32 1.86 3 21.10 1 7 0 77.07 1.80 4 9.92 1 8 0 195.14 5.01 3 30.36 2 8 0 240.72 5.73 3 49.48 1 9 0 174.77 5.32 2 31.85 2 10 0 152.39 4.27 2 35.10 3 11 0 195.11 5.55 2 50.81 -1 1 1 2033.65 73.88 2 506.70 0 1 1 197.75 5.30 3 51.11 -1 4 1 196.29 5.21 3 27.80 -3 11 1 83.46 3.12 2 33.13 -9 4 7 9.57 1.97 4 14.15 7 5 7 11.29 6.75 2 37.76 6 5 8 23.84 7.99 2 52.48 0 4 12 44.76 4.30 4 29.78 15 Inconsistent equivalents 3752 Unique reflections, of which 0 suppressed R(int) = 0.0857 R(sigma) = 0.1025 Friedel opposites merged Maximum memory for data reduction = 2417 / 38011 Default effective X-H distances for T = -123.0 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 = 3090 / 278367 wR2 = 0.1957 before cycle 1 for 3752 data and 223 / 223 parameters GooF = S = 1.018; Restrained GooF = 1.018 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1126 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36429 0.00154 -2.345 OSF 2 0.00360 0.00349 -5.770 EXTI Mean shift/esd = 0.205 Maximum = -5.770 for EXTI Max. shift = 0.002 A for H9B Max. dU =-0.001 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3090 / 278367 wR2 = 0.1942 before cycle 2 for 3752 data and 223 / 223 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1126 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36407 0.00139 -0.158 OSF 2 0.00397 0.00175 0.212 EXTI Mean shift/esd = 0.032 Maximum = 0.212 for EXTI Max. shift = 0.002 A for H9B Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3090 / 278367 wR2 = 0.1942 before cycle 3 for 3752 data and 223 / 223 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1126 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36404 0.00139 -0.022 OSF 2 0.00434 0.00179 0.207 EXTI Mean shift/esd = 0.004 Maximum = 0.207 for EXTI Max. shift = 0.000 A for H17A Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3090 / 278367 wR2 = 0.1942 before cycle 4 for 3752 data and 223 / 223 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1126 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36405 0.00140 0.011 OSF 2 0.00433 0.00183 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.011 for OSF Max. shift = 0.000 A for H1B Max. dU = 0.000 for C16 Largest correlation matrix elements 0.560 U13 C1 / U33 C1 0.531 U13 C17 / U11 C17 0.517 U13 C1 / U11 C1 0.554 U13 C17 / U33 C17 0.531 U13 Si1 / U11 Si1 0.516 U13 S1 / U33 S1 0.549 U13 C2 / U11 C2 0.529 U13 N1 / U33 N1 0.513 U13 C7 / U11 C7 0.547 U13 C7 / U33 C7 0.527 U13 C12 / U33 C12 0.512 U12 C2 / U23 C2 0.543 U13 C14 / U11 C14 0.527 U13 C18 / U33 C18 0.510 U13 N1 / U11 N1 0.535 U13 C9 / U33 C9 0.527 U13 C9 / U11 C9 0.509 z C1 / x C1 0.535 U13 Si1 / U33 Si1 0.520 U13 S1 / U11 S1 0.509 U13 C18 / U11 C18 0.534 U13 C14 / U33 C14 0.520 U13 C2 / U33 C2 0.508 U13 N2 / U33 N2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.1488 0.0600 0.4634 137 0.980 0.000 C1 C2 H1A H1B -0.1786 -0.0613 0.4021 137 0.980 0.000 C1 C2 H1A H1C -0.2512 0.0475 0.3483 137 0.980 0.000 C1 C2 H1A H3 -0.0056 0.1445 0.4489 43 0.950 0.000 C3 C2 C4 H4 0.0881 0.1916 0.3485 43 0.950 0.000 C4 C5 C3 H6 -0.1153 0.0074 0.0862 43 0.950 0.000 C6 C7 C5 H7 -0.2072 -0.0375 0.1872 43 0.950 0.000 C7 C6 C2 H9A 0.1365 -0.0778 0.3610 137 0.980 0.000 C9 C8 H9A H9B 0.1541 -0.2085 0.3387 137 0.980 0.000 C9 C8 H9A H9C 0.0810 -0.1286 0.2374 137 0.980 0.000 C9 C8 H9A H10A 0.3714 -0.1647 0.4178 23 0.990 0.000 C10 C8 C11 H10B 0.3311 -0.0510 0.4550 23 0.990 0.000 C10 C8 C11 H11A 0.4335 0.0545 0.4012 23 0.990 0.000 C11 C12 C10 H11B 0.4676 -0.0583 0.3562 23 0.990 0.000 C11 C12 C10 H14A 0.3251 -0.1829 0.0457 93 0.950 0.000 C14 C13 C15 H14B 0.3838 -0.0583 0.0662 93 0.950 0.000 C14 C13 C15 H15A 0.2919 -0.2402 0.2339 23 0.990 0.000 C15 C13 C8 H15B 0.1859 -0.1892 0.1376 23 0.990 0.000 C15 C13 C8 H16A 0.3959 0.3438 0.2657 137 0.980 0.000 C16 Si1 H16A H16B 0.4303 0.2511 0.3635 137 0.980 0.000 C16 Si1 H16A H16C 0.3096 0.2774 0.2893 137 0.980 0.000 C16 Si1 H16A H17A 0.5056 0.0777 0.1481 137 0.980 0.000 C17 Si1 H17A H17B 0.5524 0.1086 0.2778 137 0.980 0.000 C17 Si1 H17A H17C 0.5339 0.2073 0.1881 137 0.980 0.000 C17 Si1 H17A H18A 0.3150 0.2709 0.0261 137 0.980 0.000 C18 Si1 H18A H18B 0.2170 0.2179 0.0378 137 0.980 0.000 C18 Si1 H18A H18C 0.2828 0.1405 -0.0073 137 0.980 0.000 C18 Si1 H18A H1 0.1376 -0.0017 0.0829 43 0.880 0.000 N1 N2 S1 01SOT003 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.17932 0.02151 0.39087 1.00000 0.04909 0.04541 0.04307 0.00543 0.02254 0.00997 0.04498 0.00959 0.00034 0.00035 0.00036 0.00000 0.00272 0.00255 0.00274 0.00199 0.00226 0.00195 0.00110 H1A -0.14875 0.05996 0.46336 1.00000 0.06746 0.00000 0.00000 H1B -0.17863 -0.06126 0.40207 1.00000 0.06746 0.00000 0.00000 H1C -0.25116 0.04745 0.34826 1.00000 0.06746 0.00000 0.00000 C2 -0.11731 0.04957 0.32810 1.00000 0.03510 0.02888 0.03527 0.00306 0.01678 0.01016 0.03257 0.00837 0.00029 0.00031 0.00032 0.00000 0.00229 0.00204 0.00239 0.00174 0.00194 0.00164 0.00092 C3 -0.02841 0.11706 0.37498 1.00000 0.04176 0.03322 0.03369 -0.00195 0.01199 0.01036 0.03783 0.00856 0.00031 0.00032 0.00034 0.00000 0.00243 0.00222 0.00243 0.00177 0.00201 0.00177 0.00099 H3 -0.00561 0.14449 0.44894 1.00000 0.04539 0.00000 0.00000 C4 0.02774 0.14511 0.31540 1.00000 0.02767 0.02819 0.03420 -0.00351 0.00390 0.00576 0.03346 0.00801 0.00029 0.00030 0.00032 0.00000 0.00213 0.00205 0.00241 0.00172 0.00184 0.00154 0.00095 H4 0.08808 0.19157 0.34852 1.00000 0.04016 0.00000 0.00000 C5 -0.00451 0.10530 0.20835 1.00000 0.02219 0.02231 0.03196 -0.00238 0.00688 0.00545 0.02725 0.00739 0.00026 0.00028 0.00031 0.00000 0.00190 0.00186 0.00223 0.00157 0.00166 0.00143 0.00084 C6 -0.09309 0.03582 0.15972 1.00000 0.02883 0.03303 0.02978 -0.00829 0.01149 -0.00484 0.03101 0.00766 0.00028 0.00029 0.00032 0.00000 0.00211 0.00206 0.00226 0.00165 0.00182 0.00159 0.00089 H6 -0.11527 0.00738 0.08619 1.00000 0.03721 0.00000 0.00000 C7 -0.14722 0.00959 0.22017 1.00000 0.03292 0.03836 0.03846 -0.00339 0.01597 -0.00545 0.03644 0.00839 0.00030 0.00031 0.00033 0.00000 0.00228 0.00227 0.00262 0.00187 0.00201 0.00172 0.00098 H7 -0.20716 -0.03748 0.18717 1.00000 0.04372 0.00000 0.00000 C8 0.23652 -0.09688 0.28885 1.00000 0.02108 0.02380 0.03479 0.00310 0.00573 -0.00185 0.02887 0.00730 0.00026 0.00028 0.00031 0.00000 0.00190 0.00186 0.00233 0.00164 0.00170 0.00145 0.00088 C9 0.14391 -0.13095 0.30820 1.00000 0.03853 0.02663 0.04590 0.00616 0.01837 -0.00121 0.03703 0.00845 0.00030 0.00031 0.00034 0.00000 0.00233 0.00204 0.00263 0.00178 0.00206 0.00160 0.00098 H9A 0.13650 -0.07781 0.36103 1.00000 0.05555 0.00000 0.00000 H9B 0.15412 -0.20854 0.33868 1.00000 0.05555 0.00000 0.00000 H9C 0.08096 -0.12863 0.23745 1.00000 0.05555 0.00000 0.00000 C10 0.34014 -0.08833 0.39319 1.00000 0.03203 0.03944 0.03641 0.00873 0.00454 0.00016 0.03969 0.00809 0.00028 0.00035 0.00033 0.00000 0.00224 0.00233 0.00249 0.00185 0.00191 0.00173 0.00100 H10A 0.37143 -0.16473 0.41781 1.00000 0.04762 0.00000 0.00000 H10B 0.33112 -0.05099 0.45498 1.00000 0.04762 0.00000 0.00000 C11 0.40758 -0.01435 0.35409 1.00000 0.02337 0.03479 0.05063 0.00628 0.00444 -0.00274 0.04046 0.00833 0.00029 0.00033 0.00034 0.00000 0.00207 0.00225 0.00285 0.00191 0.00195 0.00163 0.00106 H11A 0.43354 0.05453 0.40123 1.00000 0.04856 0.00000 0.00000 H11B 0.46759 -0.05834 0.35624 1.00000 0.04856 0.00000 0.00000 C12 0.33253 0.01830 0.23342 1.00000 0.01615 0.03547 0.03937 0.00087 0.00907 0.00011 0.03142 0.00767 0.00026 0.00030 0.00032 0.00000 0.00185 0.00213 0.00246 0.00172 0.00175 0.00148 0.00091 C13 0.31609 -0.08961 0.16420 1.00000 0.01885 0.02858 0.04028 0.00098 0.00752 0.00591 0.03117 0.00775 0.00026 0.00030 0.00032 0.00000 0.00188 0.00202 0.00248 0.00171 0.00178 0.00150 0.00090 C14 0.34428 -0.11236 0.08466 1.00000 0.03869 0.04153 0.06408 -0.00653 0.02516 -0.00224 0.04712 0.00917 0.00032 0.00036 0.00038 0.00000 0.00251 0.00244 0.00329 0.00217 0.00244 0.00190 0.00116 H14A 0.32507 -0.18287 0.04571 1.00000 0.05654 0.00000 0.00000 H14B 0.38383 -0.05828 0.06620 1.00000 0.05654 0.00000 0.00000 C15 0.25303 -0.16926 0.20077 1.00000 0.02113 0.02515 0.04520 0.00327 0.00612 0.00511 0.03349 0.00798 0.00028 0.00030 0.00033 0.00000 0.00194 0.00191 0.00251 0.00174 0.00180 0.00146 0.00094 H15A 0.29190 -0.24023 0.23385 1.00000 0.04019 0.00000 0.00000 H15B 0.18587 -0.18921 0.13764 1.00000 0.04019 0.00000 0.00000 C16 0.37771 0.27081 0.28866 1.00000 0.03756 0.04052 0.05677 -0.00593 0.01169 -0.01128 0.04814 0.00840 0.00032 0.00035 0.00037 0.00000 0.00248 0.00246 0.00302 0.00210 0.00224 0.00184 0.00114 H16A 0.39588 0.34379 0.26574 1.00000 0.07221 0.00000 0.00000 H16B 0.43031 0.25108 0.36348 1.00000 0.07221 0.00000 0.00000 H16C 0.30961 0.27741 0.28930 1.00000 0.07221 0.00000 0.00000 C17 0.50714 0.13507 0.20233 1.00000 0.03064 0.05883 0.09076 -0.00135 0.02599 -0.01004 0.06025 0.01010 0.00032 0.00040 0.00046 0.00000 0.00248 0.00307 0.00401 0.00263 0.00265 0.00205 0.00138 H17A 0.50563 0.07774 0.14813 1.00000 0.09037 0.00000 0.00000 H17B 0.55244 0.10857 0.27780 1.00000 0.09037 0.00000 0.00000 H17C 0.53388 0.20730 0.18812 1.00000 0.09037 0.00000 0.00000 C18 0.28672 0.20191 0.04435 1.00000 0.04371 0.04387 0.04610 0.00491 0.01928 -0.00627 0.04467 0.00883 0.00032 0.00035 0.00034 0.00000 0.00251 0.00250 0.00279 0.00205 0.00221 0.00194 0.00108 H18A 0.31499 0.27089 0.02613 1.00000 0.06701 0.00000 0.00000 H18B 0.21697 0.21793 0.03779 1.00000 0.06701 0.00000 0.00000 H18C 0.28278 0.14054 -0.00730 1.00000 0.06701 0.00000 0.00000 N1 0.14583 0.04065 0.14063 1.00000 0.01913 0.02207 0.02758 0.00007 0.00709 0.00212 0.02404 0.00584 0.00020 0.00022 0.00024 0.00000 0.00155 0.00150 0.00176 0.00124 0.00137 0.00112 0.00069 H1 0.13761 -0.00167 0.08286 1.00000 0.02884 0.00000 0.00000 N2 0.23188 0.02374 0.24639 1.00000 0.01714 0.02546 0.02862 0.00230 0.00523 -0.00187 0.02544 0.00578 0.00021 0.00023 0.00024 0.00000 0.00154 0.00160 0.00183 0.00125 0.00137 0.00113 0.00071 O1 -0.00923 0.13760 0.01382 1.00000 0.02224 0.02710 0.03112 0.00494 0.00470 0.00239 0.02931 0.00495 0.00018 0.00018 0.00020 0.00000 0.00134 0.00135 0.00154 0.00108 0.00117 0.00099 0.00061 O2 0.12035 0.24305 0.17592 1.00000 0.02669 0.02025 0.05441 -0.00833 0.00852 -0.00546 0.03707 0.00495 0.00018 0.00019 0.00022 0.00000 0.00145 0.00133 0.00186 0.00120 0.00134 0.00102 0.00071 Si1 0.37260 0.15719 0.18889 1.00000 0.02247 0.03347 0.04801 0.00017 0.01220 -0.00726 0.03579 0.00225 0.00008 0.00009 0.00010 0.00000 0.00061 0.00064 0.00078 0.00050 0.00054 0.00042 0.00035 S1 0.06326 0.14085 0.13027 1.00000 0.02005 0.01965 0.03638 -0.00089 0.00804 0.00010 0.02689 0.00187 0.00007 0.00007 0.00008 0.00000 0.00050 0.00049 0.00062 0.00039 0.00042 0.00033 0.00030 Final Structure Factor Calculation for 01SOT003 in P2(1)/c Total number of l.s. parameters = 223 Maximum vector length = 511 Memory required = 2867 / 25039 wR2 = 0.1942 before cycle 5 for 3752 data and 0 / 223 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1126 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0691 for 2320 Fo > 4sig(Fo) and 0.1251 for all 3752 data wR2 = 0.1942, GooF = S = 1.010, Restrained GooF = 1.010 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0576 0.0403 0.0371 C1 0.0426 0.0341 0.0210 C2 0.0546 0.0331 0.0258 C3 0.0516 0.0270 0.0219 C4 0.0402 0.0249 0.0167 C5 0.0398 0.0308 0.0224 C6 0.0425 0.0373 0.0294 C7 0.0435 0.0231 0.0200 C8 0.0486 0.0386 0.0239 C9 0.0571 0.0369 0.0251 C10 0.0666 0.0326 0.0222 C11 0.0429 0.0354 0.0160 C12 0.0463 0.0311 0.0161 C13 0.0662 0.0398 0.0354 C14 0.0546 0.0286 0.0173 C15 0.0673 0.0500 0.0271 C16 0.0944 0.0620 0.0243 C17 0.0552 0.0449 0.0339 C18 0.0312 0.0229 0.0180 N1 0.0355 0.0243 0.0165 N2 0.0412 0.0279 0.0189 O1 0.0654 0.0298 0.0160 O2 0.0522 0.0368 0.0184 Si1 0.0411 0.0200 0.0196 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.025 0.035 0.047 0.059 0.077 0.103 0.148 1.000 Number in group 386. 377. 367. 394. 377. 348. 387. 365. 375. 376. GooF 0.933 0.994 0.995 0.999 1.117 1.030 1.091 1.024 0.946 0.958 K 2.650 1.557 1.223 1.123 1.047 1.022 1.005 0.991 0.998 1.028 Resolution(A) 0.77 0.84 0.88 0.92 0.97 1.04 1.12 1.23 1.41 1.77 inf Number in group 385. 375. 372. 369. 381. 377. 371. 375. 370. 377. GooF 1.096 0.901 0.953 0.947 0.956 0.996 0.925 0.927 0.983 1.335 K 0.860 0.951 1.037 1.053 1.040 1.045 1.043 1.025 1.029 1.018 R1 0.405 0.252 0.226 0.180 0.130 0.105 0.077 0.062 0.060 0.062 Recommended weighting scheme: WGHT 0.1052 0.3128 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) -5 2 1 234.35 130.95 4.51 0.054 2.51 -11 0 16 -108.00 204.98 4.29 0.067 0.81 4 8 11 -11.09 112.62 4.14 0.050 0.78 -3 5 4 50.01 4.83 3.86 0.010 1.89 -5 2 4 28.27 59.13 3.80 0.036 2.37 -2 2 7 149.52 247.95 3.78 0.074 1.78 2 0 0 76.96 40.33 3.74 0.030 6.43 0 5 4 87.10 179.49 3.64 0.063 1.85 -2 3 5 34.36 66.53 3.57 0.038 2.20 1 5 0 -9.17 12.39 3.53 0.016 2.30 5 4 0 984.29 657.84 3.52 0.120 1.93 -7 12 5 163.20 399.35 3.47 0.094 0.87 0 5 1 30.66 61.49 3.43 0.037 2.30 -13 8 2 -76.14 158.07 3.36 0.059 0.85 -4 2 4 -8.47 10.03 3.28 0.015 2.61 -13 3 7 127.50 10.65 3.26 0.015 1.05 -8 5 7 -16.81 18.49 3.18 0.020 1.30 -8 13 5 79.70 317.08 3.17 0.083 0.80 -1 6 6 40.65 0.68 3.13 0.004 1.44 7 3 5 82.11 25.14 3.07 0.023 1.17 -6 13 4 68.00 226.00 3.05 0.070 0.84 -4 3 2 123.30 83.49 2.99 0.043 2.63 3 7 6 -3.97 36.02 2.95 0.028 1.14 -8 4 14 272.46 10.19 2.88 0.015 0.90 -14 5 13 220.25 5.59 2.87 0.011 0.81 4 4 0 7586.01 5548.97 2.86 0.349 2.16 9 2 6 162.76 20.20 2.85 0.021 0.97 -14 8 9 64.47 163.05 2.83 0.060 0.82 -11 6 4 94.77 0.58 2.83 0.004 1.08 -15 0 4 14.41 197.52 2.81 0.066 0.94 -16 1 3 -138.66 115.78 2.80 0.050 0.86 0 6 3 154.25 84.85 2.77 0.043 1.75 6 4 0 937.77 689.58 2.77 0.123 1.73 3 3 0 972.95 711.81 2.77 0.125 2.89 1 3 5 58.25 92.66 2.76 0.045 1.91 4 0 10 344.81 166.81 2.76 0.061 0.99 -1 2 10 173.08 99.38 2.75 0.047 1.22 2 1 0 81.70 58.45 2.73 0.036 5.64 -2 8 7 35.73 0.86 2.72 0.004 1.15 -15 8 10 415.15 25.90 2.71 0.024 0.77 -3 1 10 40.12 0.07 2.68 0.001 1.31 -4 13 5 707.82 1036.05 2.67 0.151 0.85 -4 2 9 98.96 45.37 2.67 0.032 1.44 -2 11 1 1237.84 1721.35 2.66 0.194 1.05 -6 3 2 197.35 140.25 2.64 0.055 2.03 -2 3 7 -13.32 11.81 2.63 0.016 1.69 1 3 2 27.72 46.69 2.62 0.032 3.00 -4 2 11 1202.13 895.53 2.62 0.140 1.18 -10 11 2 146.09 258.56 2.60 0.075 0.84 13 3 2 136.88 263.07 2.59 0.076 0.89 Bond lengths and angles C1 - Distance Angles C2 1.4972 (0.0054) C1 - C2 - Distance Angles C3 1.3917 (0.0054) C7 1.3922 (0.0052) 117.65 (0.36) C1 1.4972 (0.0054) 121.35 (0.37) 121.00 (0.36) C2 - C3 C7 C3 - Distance Angles C2 1.3917 (0.0054) C4 1.3928 (0.0054) 121.18 (0.37) C3 - C2 C4 - Distance Angles C5 1.3767 (0.0050) C3 1.3928 (0.0054) 119.78 (0.35) C4 - C5 C5 - Distance Angles C4 1.3767 (0.0050) C6 1.4031 (0.0049) 120.15 (0.35) S1 1.7539 (0.0039) 120.93 (0.28) 118.92 (0.29) C5 - C4 C6 C6 - Distance Angles C7 1.3739 (0.0052) C5 1.4031 (0.0049) 118.92 (0.35) C6 - C7 C7 - Distance Angles C6 1.3739 (0.0052) C2 1.3922 (0.0052) 122.31 (0.36) C7 - C6 C8 - Distance Angles C9 1.5083 (0.0049) N2 1.5123 (0.0043) 114.38 (0.28) C10 1.5306 (0.0050) 115.77 (0.32) 98.42 (0.25) C15 1.5481 (0.0053) 114.88 (0.29) 102.90 (0.28) 108.59 (0.30) C8 - C9 N2 C10 C9 - Distance Angles C8 1.5083 (0.0049) C9 - C10 - Distance Angles C8 1.5306 (0.0050) C11 1.5458 (0.0054) 103.18 (0.30) C10 - C8 C11 - Distance Angles C12 1.5434 (0.0052) C10 1.5458 (0.0054) 103.82 (0.29) C11 - C12 C12 - Distance Angles C13 1.5215 (0.0051) N2 1.5231 (0.0043) 101.55 (0.26) C11 1.5434 (0.0052) 106.29 (0.30) 98.80 (0.28) Si1 1.9033 (0.0037) 120.52 (0.28) 115.30 (0.22) 111.74 (0.24) C12 - C13 N2 C11 C13 - Distance Angles C14 1.3161 (0.0055) C15 1.5178 (0.0052) 124.63 (0.36) C12 1.5215 (0.0051) 129.57 (0.36) 105.74 (0.31) C13 - C14 C15 C14 - Distance Angles C13 1.3161 (0.0055) C14 - C15 - Distance Angles C13 1.5178 (0.0052) C8 1.5481 (0.0053) 102.48 (0.28) C15 - C13 C16 - Distance Angles Si1 1.8608 (0.0043) C16 - C17 - Distance Angles Si1 1.8696 (0.0043) C17 - C18 - Distance Angles Si1 1.8533 (0.0042) C18 - N1 - Distance Angles N2 1.4244 (0.0038) S1 1.6266 (0.0027) 117.73 (0.22) N1 - N2 N2 - Distance Angles N1 1.4244 (0.0038) C8 1.5123 (0.0043) 112.25 (0.24) C12 1.5231 (0.0043) 110.08 (0.25) 96.56 (0.24) N2 - N1 C8 O1 - Distance Angles S1 1.4438 (0.0026) O1 - O2 - Distance Angles S1 1.4266 (0.0024) O2 - Si1 - Distance Angles C18 1.8533 (0.0042) C16 1.8608 (0.0043) 110.11 (0.21) C17 1.8696 (0.0043) 109.01 (0.22) 108.22 (0.21) C12 1.9033 (0.0037) 114.41 (0.17) 108.12 (0.19) 106.77 (0.19) Si1 - C18 C16 C17 S1 - Distance Angles O2 1.4266 (0.0024) O1 1.4438 (0.0026) 119.33 (0.15) N1 1.6266 (0.0027) 108.07 (0.15) 103.05 (0.14) C5 1.7539 (0.0039) 107.87 (0.17) 108.05 (0.16) 110.27 (0.15) S1 - O2 O1 N1 FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -1 -2 1.471 1 2 R1 = 0.1245 for 3752 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.72 at 0.0464 0.1431 0.2038 [ 0.88 A from C5 ] Deepest hole -0.56 at 0.1367 0.1463 0.1716 [ 0.95 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2953 / 39367 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0464 0.1431 0.2038 1.00000 0.05 0.72 0.88 C5 1.11 S1 1.62 C4 1.72 O2 Q2 1 0.3812 0.1599 0.1129 1.00000 0.05 0.49 1.07 SI1 1.35 C18 1.62 H18C 1.70 C17 Q3 1 0.3627 0.1532 0.2679 1.00000 0.05 0.48 1.12 SI1 1.40 C16 1.65 C12 1.67 H16B Q4 1 0.0649 0.1445 0.0412 1.00000 0.05 0.41 0.96 O1 1.20 S1 1.80 N1 1.95 H1 Q5 1 0.0108 0.1162 0.2650 1.00000 0.05 0.40 0.69 C4 0.70 C5 1.47 H4 1.78 C3 Q6 1 0.1323 0.2338 0.1068 1.00000 0.05 0.39 1.01 O2 1.59 S1 1.82 H18B 2.17 O1 Q7 1 0.3833 0.2738 0.3802 1.00000 0.05 0.35 0.84 H16B 1.19 C16 1.21 H16C 1.81 H16A Q8 1 -0.1415 -0.0055 0.4818 1.00000 0.05 0.34 0.80 H1A 1.14 C1 1.16 H1B 1.89 H1C Q9 1 0.2634 -0.1423 0.2492 1.00000 0.05 0.34 0.67 C15 0.94 C8 1.26 H15A 1.52 H15B Q10 1 0.4983 0.1257 0.1020 1.00000 0.05 0.33 0.80 H17A 1.29 C17 1.41 H17C 2.13 H17B Shortest distances between peaks (including symmetry equivalents) 1 5 1.18 4 6 1.43 2 10 1.79 3 7 1.98 2 3 2.20 1 4 2.30 1 6 2.39 7 10 2.93 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 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.48: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.55: Structure factors and derivatives 1.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.31: 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 0.16: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:19:08 Total CPU time: 5.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++