+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0909 started at 13:34:02 on 25-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0909 in P2(1)/c CELL 0.71073 7.6666 18.2992 8.9265 90.000 114.370 90.000 ZERR 2.00 0.0004 0.0014 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 32 48 4 6 4 8 V = 1140.74 F(000) = 508.0 Mu = 0.64 mm-1 Cell Wt = 980.70 Rho = 1.428 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x+3, -y+1, -z+2 FREE O1 O1_$1 DFIX -0.1 0.02 O1 O1_$1 EQIV_$2 x+1, y, z HTAB O2 CL1_$2 FMAP 2 PLAN 10 SIZE 0.07 0.14 0.21 ACTA BOND $H WGHT 0.05020 2.79340 L.S. 8 TEMP -153.00 FVAR 0.50204 MOLE 1 C2 1 1.245673 0.660267 0.823956 11.00000 0.03787 0.02003 = 0.02279 0.00003 0.01639 -0.00032 C3 1 1.065774 0.672236 0.695524 11.00000 0.03876 0.02201 = 0.02650 -0.00150 0.01314 -0.00245 AFIX 43 H3 2 1.052757 0.673537 0.585008 11.00000 -1.20000 AFIX 0 C4 1 0.909407 0.682017 0.729076 11.00000 0.03387 0.02475 = 0.03679 -0.00014 0.00879 -0.00123 AFIX 43 H4 2 0.787314 0.690653 0.642343 11.00000 -1.20000 AFIX 0 C5 1 0.929851 0.679252 0.892699 11.00000 0.03288 0.02923 = 0.04243 -0.00184 0.02309 -0.00238 AFIX 43 H5 2 0.822027 0.686502 0.917650 11.00000 -1.20000 AFIX 0 C6 1 1.104372 0.666179 1.014449 11.00000 0.04184 0.02257 = 0.03255 -0.00154 0.02481 -0.00339 AFIX 43 H6 2 1.118379 0.664112 1.125187 11.00000 -1.20000 AFIX 0 C7 1 1.450299 0.640205 1.117027 11.00000 0.03402 0.02523 = 0.01816 0.00088 0.01145 0.00041 AFIX 23 H7A 2 1.457588 0.665227 1.217775 11.00000 -1.20000 H7B 2 1.553589 0.659876 1.089257 11.00000 -1.20000 AFIX 0 C9 1 1.290031 0.497834 1.204892 11.00000 0.04844 0.02180 = 0.03616 0.00029 0.02190 0.00317 AFIX 137 H9A 2 1.172485 0.495277 1.103497 11.00000 -1.50000 H9B 2 1.267924 0.528474 1.285423 11.00000 -1.50000 H9C 2 1.326694 0.448548 1.249851 11.00000 -1.50000 AFIX 0 C10 1 1.719156 0.532164 1.343196 11.00000 0.03671 0.03398 = 0.02664 -0.00033 0.01234 -0.00400 AFIX 23 H10A 2 1.707414 0.557390 1.436716 11.00000 -1.20000 H10B 2 1.749394 0.480178 1.373479 11.00000 -1.20000 AFIX 0 N1 3 1.262168 0.655814 0.980188 11.00000 0.03169 0.01864 = 0.02116 -0.00120 0.01352 -0.00110 O1 4 1.520463 0.502544 1.003286 10.50000 0.02183 O2 4 1.406840 0.650188 0.806856 11.00000 0.03597 0.04157 = 0.01883 0.00375 0.01672 0.00706 AFIX 147 H2 2 1.384251 0.650107 0.706423 11.00000 -1.50000 AFIX 0 SI1 5 1.488544 0.538704 1.158450 11.00000 0.03571 0.02447 = 0.01924 0.00009 0.01252 0.00178 CL1 6 0.382872 0.668743 0.480489 11.00000 0.03963 0.03294 = 0.02130 0.00082 0.01738 0.00161 CL2 6 1.908575 0.572668 1.304379 11.00000 0.03196 0.09025 = 0.04549 0.00427 0.01651 -0.00593 HKLF 4 Covalent radii and connectivity table for 2008src0909 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C2 - O2 N1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 N1 C7 - N1 Si1 C9 - Si1 C10 - Cl2 Si1 N1 - C2 C6 C7 O1 - Si1_$1 Si1 O2 - C2 Si1 - O1_$1 O1 C10 C9 C7 Cl1 - no bonds found Cl2 - C10 Operators for generating equivalent atoms: $1 -x+3, -y+1, -z+2 $2 x+1, y, z h k l Fo^2 Sigma Why rejected 2 0 1 10.08 1.69 observed but should be systematically absent 2 0 1 9.96 1.12 observed but should be systematically absent 3 0 1 7.61 1.78 observed but should be systematically absent 3 0 1 17.68 4.07 observed but should be systematically absent 4 0 1 9.92 1.94 observed but should be systematically absent 14312 Reflections read, of which 306 rejected -9 =< h =< 9, -23 =< k =< 23, -11 =< l =< 11, Max. 2-theta = 54.96 5 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 3 6 8 -13.59 5.99 2 47.11 2 7 8 -1.91 3.84 2 19.53 2 Inconsistent equivalents 2606 Unique reflections, of which 0 suppressed R(int) = 0.0855 R(sigma) = 0.0742 Friedel opposites merged Maximum memory for data reduction = 1569 / 26004 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 = 1927 / 159765 wR2 = 0.1604 before cycle 1 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.001 Maximum = -0.008 for U12 Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 2 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.001 OSF Mean shift/su = 0.000 Maximum = -0.003 for U12 Cl1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 3 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 4 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Cl1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C6 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 5 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Cl1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 6 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Cl1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 7 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Cl1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for O2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1927 / 159765 wR2 = 0.1604 before cycle 8 for 2606 data and 124 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50204 0.00157 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Cl1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C3 Largest correlation matrix elements 0.624 U13 C6 / U11 C6 0.564 U13 C9 / U11 C9 0.536 U13 C7 / U11 C7 0.623 U13 C6 / U33 C6 0.562 U13 O2 / U11 O2 0.536 U13 Cl2 / U11 Cl2 0.605 U13 C5 / U11 C5 0.558 U13 C2 / U33 C2 0.535 U13 Si1 / U11 Si1 0.602 U13 C5 / U33 C5 0.551 U13 N1 / U11 N1 0.533 U13 C7 / U33 C7 0.597 U13 Cl1 / U33 Cl1 0.549 U13 C9 / U33 C9 0.530 U13 Cl2 / U33 Cl2 0.597 U13 Cl1 / U11 Cl1 0.547 U13 Si1 / U33 Si1 0.512 U13 C3 / U33 C3 -0.583 U11 O1 / x O1 0.547 U13 C2 / U11 C2 0.507 U13 C10 / U33 C10 0.579 U13 O2 / U33 O2 0.538 U13 N1 / U33 N1 0.503 U13 C3 / U11 C3 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 1.0528 0.6735 0.5850 43 0.950 0.000 C3 C4 C2 H4 0.7873 0.6907 0.6423 43 0.950 0.000 C4 C3 C5 H5 0.8220 0.6865 0.9177 43 0.950 0.000 C5 C6 C4 H6 1.1184 0.6641 1.1252 43 0.950 0.000 C6 C5 N1 H7A 1.4576 0.6652 1.2178 23 0.990 0.000 C7 N1 Si1 H7B 1.5536 0.6599 1.0893 23 0.990 0.000 C7 N1 Si1 H9A 1.1725 0.4953 1.1035 137 0.980 0.000 C9 Si1 H9A H9B 1.2679 0.5285 1.2854 137 0.980 0.000 C9 Si1 H9A H9C 1.3267 0.4485 1.2499 137 0.980 0.000 C9 Si1 H9A H10A 1.7074 0.5574 1.4367 23 0.990 0.000 C10 Cl2 Si1 H10B 1.7494 0.4802 1.3735 23 0.990 0.000 C10 Cl2 Si1 H2 1.3843 0.6501 0.7064 147 0.840 0.000 O2 C2 H2 2008src0909 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 1.24567 0.66027 0.82396 1.00000 0.03787 0.02003 0.02279 0.00003 0.01639 -0.00032 0.02561 0.00802 0.00057 0.00020 0.00045 0.00000 0.00219 0.00190 0.00182 0.00149 0.00170 0.00164 0.00082 C3 1.06577 0.67224 0.69552 1.00000 0.03876 0.02201 0.02650 -0.00150 0.01314 -0.00245 0.02920 0.00816 0.00058 0.00021 0.00048 0.00000 0.00232 0.00206 0.00192 0.00160 0.00179 0.00170 0.00088 H3 1.05276 0.67354 0.58501 1.00000 0.03503 0.00000 0.00000 C4 0.90941 0.68202 0.72908 1.00000 0.03387 0.02475 0.03679 -0.00014 0.00879 -0.00123 0.03372 0.00872 0.00061 0.00022 0.00052 0.00000 0.00225 0.00216 0.00226 0.00177 0.00190 0.00172 0.00095 H4 0.78731 0.69065 0.64234 1.00000 0.04046 0.00000 0.00000 C5 0.92985 0.67925 0.89270 1.00000 0.03288 0.02923 0.04243 -0.00184 0.02309 -0.00238 0.03235 0.00875 0.00059 0.00023 0.00052 0.00000 0.00222 0.00224 0.00237 0.00184 0.00200 0.00174 0.00093 H5 0.82203 0.68650 0.91765 1.00000 0.03881 0.00000 0.00000 C6 1.10437 0.66618 1.01445 1.00000 0.04184 0.02257 0.03255 -0.00154 0.02481 -0.00339 0.02918 0.00847 0.00058 0.00021 0.00049 0.00000 0.00235 0.00203 0.00209 0.00165 0.00193 0.00176 0.00088 H6 1.11838 0.66411 1.12519 1.00000 0.03502 0.00000 0.00000 C7 1.45030 0.64021 1.11703 1.00000 0.03401 0.02523 0.01816 0.00088 0.01145 0.00041 0.02557 0.00781 0.00055 0.00021 0.00043 0.00000 0.00216 0.00205 0.00175 0.00148 0.00165 0.00162 0.00083 H7A 1.45759 0.66523 1.21778 1.00000 0.03069 0.00000 0.00000 H7B 1.55359 0.65988 1.08926 1.00000 0.03069 0.00000 0.00000 C9 1.29003 0.49783 1.20489 1.00000 0.04844 0.02180 0.03616 0.00029 0.02190 0.00317 0.03399 0.00909 0.00063 0.00022 0.00052 0.00000 0.00265 0.00210 0.00220 0.00175 0.00207 0.00184 0.00097 H9A 1.17248 0.49528 1.10350 1.00000 0.05099 0.00000 0.00000 H9B 1.26792 0.52847 1.28542 1.00000 0.05099 0.00000 0.00000 H9C 1.32669 0.44855 1.24985 1.00000 0.05099 0.00000 0.00000 C10 1.71916 0.53216 1.34320 1.00000 0.03671 0.03398 0.02664 -0.00033 0.01234 -0.00400 0.03269 0.00844 0.00059 0.00024 0.00048 0.00000 0.00229 0.00233 0.00200 0.00177 0.00181 0.00184 0.00093 H10A 1.70741 0.55739 1.43672 1.00000 0.03923 0.00000 0.00000 H10B 1.74939 0.48018 1.37348 1.00000 0.03923 0.00000 0.00000 N1 1.26217 0.65581 0.98019 1.00000 0.03169 0.01864 0.02116 -0.00120 0.01352 -0.00110 0.02296 0.00630 0.00045 0.00016 0.00036 0.00000 0.00173 0.00155 0.00151 0.00121 0.00136 0.00129 0.00067 O1 1.52046 0.50254 1.00329 0.50000 0.02183 0.01871 0.00117 0.00054 0.00120 0.00000 0.00114 O2 1.40684 0.65019 0.80686 1.00000 0.03597 0.04157 0.01883 0.00375 0.01672 0.00706 0.03033 0.00589 0.00038 0.00016 0.00031 0.00000 0.00156 0.00173 0.00125 0.00119 0.00120 0.00127 0.00066 H2 1.38425 0.65011 0.70642 1.00000 0.04549 0.00000 0.00000 Si1 1.48854 0.53870 1.15845 1.00000 0.03571 0.02447 0.01924 0.00009 0.01252 0.00178 0.02608 0.00226 0.00016 0.00006 0.00012 0.00000 0.00063 0.00057 0.00051 0.00042 0.00046 0.00046 0.00029 Cl1 0.38287 0.66874 0.48049 1.00000 0.03963 0.03294 0.02130 0.00082 0.01738 0.00161 0.02970 0.00203 0.00014 0.00005 0.00011 0.00000 0.00056 0.00056 0.00045 0.00038 0.00041 0.00043 0.00027 Cl2 1.90858 0.57267 1.30438 1.00000 0.03196 0.09025 0.04549 0.00427 0.01651 -0.00593 0.05572 0.00273 0.00017 0.00009 0.00015 0.00000 0.00062 0.00108 0.00069 0.00066 0.00054 0.00062 0.00040 Final Structure Factor Calculation for 2008src0909 in P2(1)/c Total number of l.s. parameters = 124 Maximum vector length = 511 Memory required = 1803 / 25039 wR2 = 0.1604 before cycle 9 for 2606 data and 0 / 124 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0502 * P )^2 + 2.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0631 for 1824 Fo > 4sig(Fo) and 0.0978 for all 2606 data wR2 = 0.1604, GooF = S = 1.065, Restrained GooF = 1.065 for all data Occupancy sum of asymmetric unit = 13.50 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0379 0.0201 0.0189 C2 0.0398 0.0263 0.0215 C3 0.0454 0.0312 0.0246 C4 0.0447 0.0291 0.0232 C5 0.0454 0.0225 0.0196 C6 0.0345 0.0253 0.0169 C7 0.0490 0.0317 0.0213 C9 0.0404 0.0312 0.0264 C10 0.0318 0.0193 0.0178 N1 0.0465 0.0313 0.0133 O2 0.0363 0.0242 0.0177 Si1 0.0400 0.0326 0.0165 Cl1 0.0919 0.0453 0.0300 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.030 0.040 0.054 0.068 0.086 0.110 0.163 1.000 Number in group 278. 244. 273. 247. 280. 256. 254. 255. 260. 259. GooF 0.935 0.938 0.970 1.023 1.118 1.118 1.206 1.160 1.164 0.976 K 3.191 1.319 1.026 0.992 0.965 0.989 0.980 1.019 1.019 1.022 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.67 inf Number in group 266. 264. 252. 262. 264. 261. 256. 259. 261. 261. GooF 0.847 0.873 0.899 1.013 0.929 1.011 1.044 1.009 1.242 1.577 K 0.997 1.003 1.041 1.031 1.066 1.033 1.009 0.996 1.021 1.017 R1 0.247 0.196 0.156 0.154 0.119 0.094 0.081 0.053 0.051 0.049 Recommended weighting scheme: WGHT 0.0502 2.7935 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) 5 3 0 69.04 11.62 5.00 0.019 1.36 1 3 3 338.14 176.13 4.90 0.073 2.10 -1 4 4 182.93 79.58 4.89 0.049 1.99 -5 1 2 88.83 21.92 4.61 0.026 1.52 -2 5 3 78.34 182.06 4.43 0.074 2.21 1 5 1 195.01 94.08 4.38 0.053 2.83 4 2 2 154.36 65.75 4.20 0.044 1.39 -3 2 2 721.23 512.49 3.75 0.124 2.43 1 2 1 12.50 55.76 3.72 0.041 4.01 -3 0 4 226.96 123.22 3.67 0.061 1.99 -8 5 6 436.67 261.64 3.67 0.089 0.90 -2 3 3 1030.43 776.49 3.50 0.153 2.52 -2 7 3 607.25 833.78 3.50 0.158 1.90 -3 9 2 80.50 23.18 3.35 0.026 1.58 0 3 1 21.32 1.03 3.31 0.006 4.88 0 1 3 211.43 130.97 3.26 0.063 2.68 -2 1 3 36.96 88.35 3.25 0.051 2.73 4 6 2 515.35 728.36 3.23 0.148 1.28 -1 1 1 3661.75 4528.74 3.18 0.369 6.44 -3 3 3 81.01 154.25 3.11 0.068 2.15 5 1 0 42.70 10.15 3.10 0.017 1.39 0 4 2 769.19 584.83 3.08 0.132 3.04 0 4 4 438.32 601.23 3.07 0.134 1.86 4 8 3 66.58 132.67 2.99 0.063 1.10 3 0 0 242.64 159.52 2.98 0.069 2.33 -1 4 5 847.20 654.11 2.98 0.140 1.64 -1 2 4 57.64 23.50 2.97 0.027 2.15 0 13 4 180.47 296.31 2.91 0.094 1.16 -5 5 3 93.76 19.61 2.87 0.024 1.41 -4 6 7 192.14 301.58 2.87 0.095 1.14 -2 6 1 50.65 103.43 2.85 0.056 2.39 -7 3 1 88.05 150.93 2.78 0.067 1.03 -5 1 1 455.03 605.38 2.75 0.135 1.48 -4 6 4 490.81 362.43 2.75 0.104 1.50 1 7 1 66.62 31.56 2.74 0.031 2.26 -4 6 3 401.37 287.50 2.73 0.093 1.59 5 7 0 18.51 0.14 2.73 0.002 1.23 -3 2 4 66.92 124.37 2.72 0.061 1.95 -6 13 6 373.96 246.91 2.69 0.086 0.89 -4 5 4 627.90 799.77 2.63 0.155 1.56 -1 11 1 2447.71 2026.81 2.61 0.247 1.62 -8 7 4 391.16 270.45 2.61 0.090 0.90 0 1 5 100.70 160.00 2.59 0.069 1.62 -4 15 2 87.66 155.84 2.56 0.068 1.03 3 5 3 47.53 17.50 2.54 0.023 1.38 1 7 2 328.74 230.93 2.54 0.083 1.97 3 1 5 10.08 48.22 2.52 0.038 1.13 0 10 1 843.99 674.49 2.52 0.142 1.79 -5 3 6 281.01 395.52 2.50 0.109 1.24 -2 8 10 18.18 75.89 2.47 0.048 0.82 Bond lengths and angles C2 - Distance Angles O2 1.3190 (0.0046) N1 1.3498 (0.0045) 114.72 (0.33) C3 1.3999 (0.0056) 125.49 (0.33) 119.75 (0.35) C2 - O2 N1 C3 - Distance Angles C4 1.3621 (0.0058) C2 1.3999 (0.0056) 119.97 (0.37) H3 0.9500 120.01 120.01 C3 - C4 C2 C4 - Distance Angles C3 1.3621 (0.0058) C5 1.4041 (0.0058) 119.56 (0.39) H4 0.9500 120.22 120.22 C4 - C3 C5 C5 - Distance Angles C6 1.3522 (0.0060) C4 1.4041 (0.0058) 119.42 (0.38) H5 0.9500 120.29 120.29 C5 - C6 C4 C6 - Distance Angles C5 1.3522 (0.0060) N1 1.3778 (0.0048) 120.94 (0.36) H6 0.9500 119.53 119.53 C6 - C5 N1 C7 - Distance Angles N1 1.4832 (0.0048) Si1 1.8929 (0.0039) 111.68 (0.25) H7A 0.9900 109.28 109.28 H7B 0.9900 109.28 109.28 107.95 C7 - N1 Si1 H7A C9 - Distance Angles Si1 1.8890 (0.0043) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - Si1 H9A H9B C10 - Distance Angles Cl2 1.7871 (0.0042) Si1 1.8584 (0.0042) 110.66 (0.21) H10A 0.9900 109.51 109.51 H10B 0.9900 109.51 109.51 108.08 C10 - Cl2 Si1 H10A N1 - Distance Angles C2 1.3498 (0.0045) C6 1.3778 (0.0048) 120.30 (0.34) C7 1.4832 (0.0048) 120.48 (0.31) 119.22 (0.30) N1 - C2 C6 O1 - Distance Angles Si1_$1 1.6052 (0.0099) Si1 1.6419 (0.0098) 169.16 (0.56) O1 - Si1_$1 O2 - Distance Angles C2 1.3190 (0.0046) H2 0.8400 109.47 O2 - C2 Si1 - Distance Angles O1_$1 1.6052 (0.0099) O1 1.6419 (0.0098) 10.84 (0.56) C10 1.8584 (0.0042) 116.10 (0.35) 107.71 (0.34) C9 1.8890 (0.0043) 105.76 (0.32) 116.08 (0.32) 109.72 (0.19) C7 1.8929 (0.0039) 109.88 (0.38) 107.20 (0.37) 104.51 (0.18) 110.95 (0.18) Si1 - O1_$1 O1 C10 C9 Cl2 - Distance Angles C10 1.7871 (0.0043) Cl2 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.04 2.863(3) 165.7 O2-H2...Cl1_$2 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 24 -2 2.500 1 2 R1 = 0.0971 for 2606 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.33 at 0.3901 0.4476 0.8243 [ 0.91 A from SI1 ] Deepest hole -0.55 at 0.0837 0.3934 0.6508 [ 0.73 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2144 / 28055 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.6099 0.5524 1.1757 1.00000 0.05 1.33 0.91 SI1 1.43 C10 1.67 O1 1.80 O1 Q2 1 1.4705 0.5003 1.3032 1.00000 0.05 0.54 1.30 C9 1.38 H9C 1.53 SI1 1.58 H9B Q3 1 1.3461 0.5185 1.1755 1.00000 0.05 0.42 0.70 C9 1.22 SI1 1.29 H9A 1.36 H9B Q4 1 1.6791 0.5741 1.5228 1.00000 0.05 0.36 0.93 H10A 1.91 C10 2.09 H9C 2.37 H10B Q5 1 1.5744 0.5183 1.2697 1.00000 0.05 0.35 1.01 SI1 1.06 C10 1.46 H10B 1.59 H10A Q6 1 1.4437 0.5974 1.1636 1.00000 0.05 0.33 0.90 C7 1.13 SI1 1.32 H7A 1.71 H7B Q7 1 1.1219 0.4626 1.2593 1.00000 0.05 0.32 1.60 H9B 1.63 H9C 1.68 C9 1.70 H9A Q8 1 0.9803 0.7214 0.5119 1.00000 0.05 0.31 1.10 H3 1.74 C3 2.04 H5 2.06 C5 Q9 1 0.2762 0.6705 0.4873 1.00000 0.05 0.30 0.84 CL1 1.82 H2 2.22 H3 2.63 O2 Q10 1 1.7656 0.4368 1.5185 1.00000 0.05 0.30 1.48 H10B 1.98 H9B 2.24 CL1 2.27 C10 Shortest distances between peaks (including symmetry equivalents) 2 5 1.01 1 5 1.16 2 3 1.19 1 6 1.48 3 5 1.60 3 6 1.65 5 6 1.79 9 10 1.99 4 7 2.03 1 2 2.08 1 3 2.11 2 6 2.13 4 5 2.30 3 7 2.37 2 4 2.37 8 9 2.54 2 10 2.56 5 10 2.57 7 10 2.58 4 10 2.60 2 7 2.63 2 4 2.66 1 4 2.95 4 6 2.99 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.66: 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 0.73: Structure factors and derivatives 0.59: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0909 finished at 13:34:05 Total CPU time: 2.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++