+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:28:43 on 28-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1016 in P-1 CELL 0.71073 7.6668 10.8424 12.6410 79.319 73.438 73.223 ZERR 2.00 0.0002 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O SI CL UNIT 28 30 4 4 2 10 V = 958.24 F(000) = 456.0 Mu = 0.83 mm-1 Cell Wt = 897.24 Rho = 1.555 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 FMAP 2 PLAN 10 SIZE 0.20 0.20 0.55 ACTA WGHT 0.04430 0.99200 L.S. 5 TEMP -153.00 FVAR 0.68585 C1 1 -0.079992 0.774872 -0.313701 11.00000 0.01486 0.02116 = 0.01617 -0.00031 -0.00738 -0.00414 AFIX 23 H1A 2 -0.048818 0.858969 -0.320726 11.00000 -1.20000 H1B 2 0.033491 0.711987 -0.350207 11.00000 -1.20000 AFIX 0 C2 1 -0.228111 0.829322 -0.476095 11.00000 0.02050 0.01543 = 0.01612 -0.00283 -0.00459 -0.00482 C3 1 -0.378685 0.843434 -0.518243 11.00000 0.02625 0.02255 = 0.01802 -0.00110 -0.01111 -0.00481 AFIX 43 H3 2 -0.371484 0.868655 -0.595148 11.00000 -1.20000 AFIX 0 C4 1 -0.544497 0.819752 -0.445124 11.00000 0.02250 0.02253 = 0.02545 -0.00236 -0.01364 -0.00510 AFIX 43 H4 2 -0.650979 0.829042 -0.472883 11.00000 -1.20000 AFIX 0 C5 1 -0.554975 0.783432 -0.334297 11.00000 0.01736 0.02251 = 0.02372 -0.00195 -0.00731 -0.00690 AFIX 43 H5 2 -0.668350 0.768651 -0.285190 11.00000 -1.20000 AFIX 0 C6 1 -0.397299 0.768328 -0.294159 11.00000 0.02124 0.01571 = 0.01657 -0.00055 -0.00611 -0.00614 C7 1 -0.113550 0.535231 -0.124148 11.00000 0.03168 0.02520 = 0.02645 0.00563 -0.01614 -0.01075 AFIX 137 H7A 2 -0.166107 0.516038 -0.044428 11.00000 -1.50000 H7B 2 0.022471 0.497252 -0.142069 11.00000 -1.50000 H7C 2 -0.171875 0.498284 -0.166175 11.00000 -1.50000 AFIX 0 C8 1 -0.283454 0.821436 -0.045927 11.00000 0.01738 0.02743 = 0.01557 0.00245 -0.00701 -0.00689 AFIX 23 H8A 2 -0.343739 0.909219 -0.076466 11.00000 -1.20000 H8B 2 -0.381625 0.784552 0.008871 11.00000 -1.20000 AFIX 0 C9 1 0.040986 0.777976 -0.048515 11.00000 0.01903 0.01806 = 0.01558 0.00216 -0.00708 -0.00666 C10 1 0.190060 0.782186 -0.006648 11.00000 0.02155 0.02581 = 0.02137 0.00128 -0.01058 -0.00665 AFIX 43 H10 2 0.316700 0.747794 -0.044431 11.00000 -1.20000 AFIX 0 C11 1 0.149310 0.836883 0.089797 11.00000 0.02955 0.02945 = 0.02129 0.00098 -0.01528 -0.00981 AFIX 43 H11 2 0.248851 0.840708 0.118835 11.00000 -1.20000 AFIX 0 C12 1 -0.037139 0.887183 0.146050 11.00000 0.03640 0.03003 = 0.01655 -0.00252 -0.01001 -0.00862 AFIX 43 H12 2 -0.064287 0.924656 0.212983 11.00000 -1.20000 AFIX 0 C13 1 -0.179714 0.881769 0.103572 11.00000 0.02737 0.02988 = 0.01569 -0.00275 -0.00459 -0.00610 AFIX 43 H13 2 -0.306869 0.915320 0.140975 11.00000 -1.20000 AFIX 0 C14 1 -0.460680 0.399965 -0.294666 11.00000 0.04238 0.02107 = 0.04021 -0.00436 -0.01645 -0.00250 N1 3 -0.235315 0.790258 -0.366235 11.00000 0.01679 0.01482 = 0.01509 -0.00113 -0.00767 -0.00358 N2 3 -0.138645 0.828174 0.007614 11.00000 0.01806 0.02193 = 0.01381 0.00091 -0.00680 -0.00588 O1 4 -0.391149 0.733334 -0.191385 11.00000 0.01932 0.02921 = 0.01510 0.00242 -0.00625 -0.01087 O2 4 0.061444 0.728806 -0.138646 11.00000 0.01519 0.02619 = 0.01739 -0.00371 -0.00590 -0.00451 SI1 5 -0.161277 0.713923 -0.161690 11.00000 0.01745 0.02064 = 0.01460 0.00121 -0.00695 -0.00696 CL1 6 -0.021903 0.861789 -0.557664 11.00000 0.02139 0.02666 = 0.01485 -0.00112 -0.00398 -0.00770 CL2 6 -0.364192 1.076334 -0.273115 11.00000 0.02058 0.01938 = 0.01954 -0.00212 -0.00734 -0.00386 CL3 6 -0.543606 0.447625 -0.159160 11.00000 0.04847 0.03562 = 0.03435 -0.00339 -0.01301 -0.01008 CL4 6 -0.262220 0.458581 -0.368041 11.00000 0.03926 0.03425 = 0.04628 -0.00841 -0.00757 -0.00407 CL5 6 -0.358185 0.544074 -0.634689 11.00000 0.05101 0.04787 = 0.04589 -0.00562 -0.02353 -0.01103 H4A 2 -0.417148 0.307118 -0.295968 11.00000 0.03748 HKLF 4 Covalent radii and connectivity table for 2008src1016 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C1 - N1 Si1 C2 - C3 N1 Cl1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - O1 N1 C5 C7 - Si1 C8 - N2 Si1 C9 - O2 N2 C10 C10 - C11 C9 C11 - C10 C12 C12 - C13 C11 C13 - N2 C12 C14 - Cl5_$1 Cl4 Cl3 N1 - C2 C6 C1 N2 - C13 C9 C8 O1 - C6 Si1 O2 - C9 Si1 Si1 - O1 C7 O2 C8 C1 Cl1 - C2 Cl2 - no bonds found Cl3 - C14 Cl4 - C14 Cl5 - C14_$1 Operators for generating equivalent atoms: $1 -x-1, -y+1, -z-1 19490 Reflections read, of which 19 rejected -9 =< h =< 9, -14 =< k =< 14, -16 =< l =< 16, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 4386 Unique reflections, of which 0 suppressed R(int) = 0.0413 R(sigma) = 0.0369 Friedel opposites merged Maximum memory for data reduction = 1993 / 43956 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 = 2590 / 277120 wR2 = 0.0992 before cycle 1 for 4386 data and 222 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68607 0.00108 0.207 OSF Mean shift/esd = 0.022 Maximum = 0.207 for OSF Max. shift = 0.005 A for H4A Max. dU = 0.000 for H4A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2590 / 277120 wR2 = 0.0992 before cycle 2 for 4386 data and 222 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68612 0.00108 0.040 OSF Mean shift/esd = 0.007 Maximum = 0.040 for OSF Max. shift = 0.002 A for H4A Max. dU = 0.000 for H4A Least-squares cycle 3 Maximum vector length = 511 Memory required = 2590 / 277120 wR2 = 0.0992 before cycle 3 for 4386 data and 222 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68612 0.00108 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.020 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H4A Least-squares cycle 4 Maximum vector length = 511 Memory required = 2590 / 277120 wR2 = 0.0992 before cycle 4 for 4386 data and 222 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68612 0.00108 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.013 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H4A Least-squares cycle 5 Maximum vector length = 511 Memory required = 2590 / 277120 wR2 = 0.0992 before cycle 5 for 4386 data and 222 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68612 0.00108 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.009 for tors H7A Max. shift = 0.000 A for H7C Max. dU = 0.000 for H4A No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0488 0.8590 -0.3207 23 0.990 0.000 C1 N1 Si1 H1B 0.0335 0.7120 -0.3502 23 0.990 0.000 C1 N1 Si1 H3 -0.3715 0.8686 -0.5952 43 0.950 0.000 C3 C2 C4 H4 -0.6510 0.8290 -0.4729 43 0.950 0.000 C4 C5 C3 H5 -0.6684 0.7686 -0.2852 43 0.950 0.000 C5 C4 C6 H7A -0.1659 0.5161 -0.0444 137 0.980 0.000 C7 Si1 H7A H7B 0.0225 0.4973 -0.1422 137 0.980 0.000 C7 Si1 H7A H7C -0.1720 0.4983 -0.1661 137 0.980 0.000 C7 Si1 H7A H8A -0.3437 0.9092 -0.0765 23 0.990 0.000 C8 N2 Si1 H8B -0.3816 0.7846 0.0089 23 0.990 0.000 C8 N2 Si1 H10 0.3167 0.7478 -0.0444 43 0.950 0.000 C10 C11 C9 H11 0.2489 0.8407 0.1188 43 0.950 0.000 C11 C10 C12 H12 -0.0643 0.9247 0.2130 43 0.950 0.000 C12 C13 C11 H13 -0.3069 0.9153 0.1410 43 0.950 0.000 C13 N2 C12 2008src1016 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.07997 0.77488 -0.31370 1.00000 0.01487 0.02118 0.01619 -0.00032 -0.00740 -0.00416 0.01696 0.00295 0.00028 0.00021 0.00017 0.00000 0.00096 0.00106 0.00100 0.00081 0.00079 0.00077 0.00041 H1A -0.04880 0.85898 -0.32072 1.00000 0.02036 0.00000 0.00000 H1B 0.03351 0.71200 -0.35020 1.00000 0.02036 0.00000 0.00000 C2 -0.22809 0.82933 -0.47609 1.00000 0.02050 0.01545 0.01614 -0.00283 -0.00459 -0.00481 0.01713 0.00297 0.00029 0.00020 0.00017 0.00000 0.00102 0.00099 0.00099 0.00078 0.00081 0.00078 0.00041 C3 -0.37870 0.84343 -0.51824 1.00000 0.02625 0.02256 0.01804 -0.00110 -0.01110 -0.00480 0.02151 0.00313 0.00031 0.00021 0.00018 0.00000 0.00114 0.00111 0.00105 0.00085 0.00089 0.00087 0.00045 H3 -0.37150 0.86865 -0.59515 1.00000 0.02582 0.00000 0.00000 C4 -0.54453 0.81974 -0.44513 1.00000 0.02252 0.02254 0.02547 -0.00237 -0.01364 -0.00510 0.02201 0.00311 0.00031 0.00021 0.00019 0.00000 0.00109 0.00112 0.00116 0.00090 0.00091 0.00086 0.00046 H4 -0.65100 0.82902 -0.47289 1.00000 0.02641 0.00000 0.00000 C5 -0.55500 0.78342 -0.33431 1.00000 0.01738 0.02253 0.02372 -0.00195 -0.00731 -0.00688 0.02040 0.00310 0.00030 0.00021 0.00019 0.00000 0.00101 0.00110 0.00111 0.00087 0.00086 0.00082 0.00044 H5 -0.66837 0.76863 -0.28520 1.00000 0.02448 0.00000 0.00000 C6 -0.39729 0.76833 -0.29416 1.00000 0.02124 0.01572 0.01658 -0.00055 -0.00611 -0.00614 0.01738 0.00298 0.00030 0.00020 0.00017 0.00000 0.00104 0.00099 0.00100 0.00079 0.00082 0.00078 0.00042 C7 -0.11350 0.53525 -0.12414 1.00000 0.03168 0.02521 0.02648 0.00563 -0.01614 -0.01076 0.02623 0.00338 0.00035 0.00023 0.00020 0.00000 0.00125 0.00119 0.00120 0.00095 0.00101 0.00096 0.00050 H7A -0.16586 0.51606 -0.04439 1.00000 0.03935 0.00000 0.00000 H7B 0.02252 0.49727 -0.14217 1.00000 0.03935 0.00000 0.00000 H7C -0.17199 0.49830 -0.16606 1.00000 0.03935 0.00000 0.00000 C8 -0.28345 0.82144 -0.04593 1.00000 0.01741 0.02744 0.01559 0.00244 -0.00702 -0.00691 0.01989 0.00307 0.00029 0.00022 0.00017 0.00000 0.00101 0.00116 0.00100 0.00085 0.00082 0.00084 0.00044 H8A -0.34373 0.90922 -0.07646 1.00000 0.02386 0.00000 0.00000 H8B -0.38162 0.78456 0.00887 1.00000 0.02386 0.00000 0.00000 C9 0.04096 0.77797 -0.04852 1.00000 0.01904 0.01807 0.01561 0.00216 -0.00708 -0.00666 0.01708 0.00299 0.00029 0.00020 0.00017 0.00000 0.00100 0.00102 0.00098 0.00079 0.00080 0.00078 0.00041 C10 0.19005 0.78218 -0.00665 1.00000 0.02157 0.02582 0.02137 0.00128 -0.01057 -0.00664 0.02217 0.00318 0.00032 0.00022 0.00019 0.00000 0.00108 0.00115 0.00110 0.00089 0.00089 0.00087 0.00046 H10 0.31669 0.74778 -0.04443 1.00000 0.02660 0.00000 0.00000 C11 0.14933 0.83689 0.08980 1.00000 0.02957 0.02945 0.02131 0.00098 -0.01528 -0.00981 0.02483 0.00325 0.00034 0.00023 0.00019 0.00000 0.00120 0.00123 0.00112 0.00093 0.00095 0.00095 0.00049 H11 0.24888 0.84073 0.11883 1.00000 0.02980 0.00000 0.00000 C12 -0.03713 0.88718 0.14605 1.00000 0.03642 0.03005 0.01654 -0.00252 -0.01001 -0.00861 0.02687 0.00345 0.00035 0.00024 0.00019 0.00000 0.00132 0.00127 0.00108 0.00092 0.00097 0.00101 0.00051 H12 -0.06429 0.92466 0.21298 1.00000 0.03225 0.00000 0.00000 C13 -0.17975 0.88175 0.10356 1.00000 0.02741 0.02989 0.01570 -0.00275 -0.00460 -0.00610 0.02469 0.00338 0.00034 0.00023 0.00019 0.00000 0.00118 0.00124 0.00104 0.00089 0.00089 0.00093 0.00048 H13 -0.30691 0.91529 0.14097 1.00000 0.02963 0.00000 0.00000 C14 -0.46071 0.39994 -0.29467 1.00000 0.04237 0.02112 0.04022 -0.00438 -0.01645 -0.00255 0.03426 0.00394 0.00040 0.00025 0.00024 0.00000 0.00150 0.00126 0.00153 0.00109 0.00123 0.00106 0.00059 N1 -0.23529 0.79027 -0.36623 1.00000 0.01680 0.01484 0.01509 -0.00113 -0.00766 -0.00358 0.01493 0.00238 0.00024 0.00016 0.00014 0.00000 0.00083 0.00083 0.00084 0.00066 0.00068 0.00064 0.00035 N2 -0.13867 0.82816 0.00761 1.00000 0.01807 0.02195 0.01382 0.00091 -0.00680 -0.00589 0.01753 0.00252 0.00024 0.00017 0.00014 0.00000 0.00087 0.00092 0.00084 0.00069 0.00069 0.00070 0.00037 O1 -0.39113 0.73334 -0.19138 1.00000 0.01934 0.02922 0.01512 0.00242 -0.00626 -0.01087 0.02042 0.00213 0.00021 0.00015 0.00012 0.00000 0.00074 0.00084 0.00073 0.00062 0.00060 0.00062 0.00033 O2 0.06143 0.72880 -0.13865 1.00000 0.01520 0.02622 0.01740 -0.00372 -0.00590 -0.00452 0.01917 0.00207 0.00020 0.00015 0.00012 0.00000 0.00071 0.00081 0.00074 0.00061 0.00058 0.00059 0.00032 Si1 -0.16127 0.71392 -0.16169 1.00000 0.01747 0.02066 0.01461 0.00121 -0.00696 -0.00696 0.01689 0.00082 0.00008 0.00006 0.00005 0.00000 0.00028 0.00030 0.00028 0.00022 0.00022 0.00022 0.00014 Cl1 -0.02190 0.86179 -0.55766 1.00000 0.02141 0.02668 0.01486 -0.00112 -0.00398 -0.00770 0.02089 0.00075 0.00007 0.00005 0.00004 0.00000 0.00026 0.00028 0.00024 0.00020 0.00019 0.00020 0.00013 Cl2 -0.36419 1.07634 -0.27311 1.00000 0.02059 0.01940 0.01956 -0.00212 -0.00734 -0.00387 0.01959 0.00073 0.00007 0.00005 0.00004 0.00000 0.00025 0.00026 0.00025 0.00019 0.00019 0.00019 0.00013 Cl3 -0.54362 0.44762 -0.15916 1.00000 0.04849 0.03564 0.03437 -0.00339 -0.01302 -0.01009 0.03906 0.00099 0.00010 0.00007 0.00006 0.00000 0.00040 0.00036 0.00036 0.00027 0.00030 0.00029 0.00017 Cl4 -0.26223 0.45858 -0.36804 1.00000 0.03928 0.03426 0.04630 -0.00841 -0.00757 -0.00407 0.04118 0.00107 0.00010 0.00007 0.00006 0.00000 0.00037 0.00036 0.00041 0.00030 0.00030 0.00027 0.00018 Cl5 -0.35819 0.54407 -0.63469 1.00000 0.05103 0.04790 0.04591 -0.00562 -0.02355 -0.01104 0.04602 0.00105 0.00011 0.00008 0.00007 0.00000 0.00044 0.00043 0.00042 0.00033 0.00034 0.00033 0.00019 H4A -0.41768 0.30680 -0.29601 1.00000 0.03752 0.04240 0.00409 0.00302 0.00243 0.00000 0.00788 Final Structure Factor Calculation for 2008src1016 in P-1 Total number of l.s. parameters = 222 Maximum vector length = 511 Memory required = 2368 / 25039 wR2 = 0.0992 before cycle 6 for 4386 data and 0 / 222 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0443 * P )^2 + 0.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0383 for 3655 Fo > 4sig(Fo) and 0.0504 for all 4386 data wR2 = 0.0992, GooF = S = 1.025, Restrained GooF = 1.025 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0220 0.0182 0.0107 C1 0.0206 0.0168 0.0140 C2 0.0283 0.0230 0.0133 C3 0.0304 0.0226 0.0130 C4 0.0244 0.0223 0.0144 C5 0.0216 0.0158 0.0148 C6 0.0396 0.0229 0.0162 C7 0.0298 0.0174 0.0124 C8 0.0226 0.0161 0.0126 C9 0.0289 0.0231 0.0145 C10 0.0353 0.0270 0.0122 C11 0.0365 0.0299 0.0142 C12 0.0310 0.0275 0.0156 C13 0.0480 0.0340 0.0208 C14 0.0191 0.0149 0.0108 N1 0.0233 0.0179 0.0114 N2 0.0318 0.0158 0.0136 O1 0.0267 0.0179 0.0130 O2 0.0230 0.0160 0.0117 Si1 0.0270 0.0208 0.0148 Cl1 0.0225 0.0195 0.0168 Cl2 0.0489 0.0355 0.0328 Cl3 0.0485 0.0440 0.0310 Cl4 0.0585 0.0478 0.0317 Cl5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.028 0.042 0.057 0.073 0.094 0.116 0.150 0.208 1.000 Number in group 446. 431. 450. 427. 446. 438. 432. 448. 430. 438. GooF 1.065 0.996 1.057 0.972 1.137 1.010 1.031 1.002 0.966 0.995 K 1.686 1.012 0.954 0.974 0.955 0.985 0.994 1.005 1.017 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 450. 446. 431. 431. 441. 430. 441. 440. 436. 440. GooF 0.943 0.917 0.912 0.912 0.912 0.874 0.827 0.856 1.133 1.676 K 0.966 0.991 1.005 1.002 1.017 1.016 1.031 1.025 1.008 0.981 R1 0.109 0.101 0.077 0.064 0.053 0.044 0.032 0.030 0.032 0.035 Recommended weighting scheme: WGHT 0.0419 0.9953 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 4 4 35.72 7.50 5.68 0.018 2.08 -3 -1 1 210.84 322.64 5.23 0.120 2.28 1 0 1 184.60 306.82 5.13 0.117 6.92 3 1 5 63.83 29.55 4.78 0.036 2.02 -2 0 1 9.81 0.11 4.76 0.002 3.20 3 1 4 1078.66 842.66 4.52 0.194 2.23 -2 -1 6 11.22 0.07 4.44 0.002 1.58 -2 3 1 118.75 74.34 4.18 0.058 2.14 -1 -3 1 45.53 82.74 4.14 0.061 3.13 -3 -3 2 273.36 198.85 3.93 0.094 1.91 0 1 2 287.47 385.29 3.91 0.131 5.47 1 4 1 36.92 16.08 3.90 0.027 2.70 2 4 4 251.64 341.46 3.86 0.124 2.18 1 1 0 7.77 0.44 3.84 0.004 6.69 -3 0 3 1343.77 1093.91 3.77 0.221 1.85 3 4 4 10.17 0.22 3.74 0.003 1.97 -3 -2 2 224.87 161.66 3.72 0.085 2.03 0 -1 6 495.78 628.73 3.63 0.168 1.93 -3 -4 1 151.20 210.56 3.60 0.097 1.90 4 0 6 128.01 86.31 3.60 0.062 1.53 1 4 0 88.95 56.02 3.60 0.050 2.65 1 -2 6 353.64 273.02 3.57 0.110 1.81 4 2 4 369.88 285.15 3.47 0.113 1.82 0 -3 4 472.09 592.20 3.47 0.163 2.15 0 0 3 -1.15 6.46 3.44 0.017 4.01 -3 2 2 34.12 16.43 3.43 0.027 1.79 2 1 3 912.52 1111.56 3.43 0.223 3.21 2 -1 6 39.00 19.50 3.41 0.030 1.85 0 3 4 215.50 288.10 3.39 0.114 2.40 8 2 3 57.46 24.59 3.33 0.033 0.95 -2 -7 5 12.89 1.15 3.27 0.007 1.16 -3 -1 2 18.85 5.95 3.26 0.016 2.07 0 4 1 9.47 0.84 3.22 0.006 2.58 0 12 3 38.99 0.03 3.21 0.001 0.86 -3 2 3 126.71 90.00 3.18 0.063 1.67 -3 -8 8 76.36 123.82 3.16 0.074 0.87 1 2 8 244.40 186.72 3.16 0.091 1.56 7 0 7 68.42 108.76 3.16 0.070 0.99 0 0 5 8.27 0.43 3.15 0.004 2.41 1 5 10 30.18 57.54 3.15 0.051 1.15 4 2 5 285.04 361.34 3.15 0.127 1.72 -3 8 8 174.75 242.71 3.14 0.104 0.84 5 4 4 7.85 0.34 3.14 0.004 1.45 9 7 5 33.39 76.11 3.10 0.058 0.82 -4 -1 1 18.62 6.88 3.09 0.018 1.74 0 -1 8 46.55 74.10 3.06 0.058 1.47 3 2 3 85.08 120.22 3.02 0.073 2.40 1 1 6 76.25 48.01 3.00 0.046 2.11 6 6 13 -8.85 13.80 2.99 0.025 0.85 -1 1 0 9644.51 11285.59 2.99 0.710 5.27 Bond lengths and angles C1 - Distance Angles N1 1.4771 (0.0025) Si1 1.8978 (0.0021) 107.44 (0.13) C1 - N1 C2 - Distance Angles C3 1.3636 (0.0030) N1 1.3648 (0.0027) 121.41 (0.19) Cl1 1.7157 (0.0021) 121.84 (0.17) 116.74 (0.15) C2 - C3 N1 C3 - Distance Angles C2 1.3636 (0.0030) C4 1.4026 (0.0032) 118.29 (0.20) C3 - C2 C4 - Distance Angles C5 1.3689 (0.0031) C3 1.4026 (0.0032) 120.88 (0.20) C4 - C5 C5 - Distance Angles C4 1.3689 (0.0031) C6 1.3969 (0.0030) 119.32 (0.20) C5 - C4 C6 - Distance Angles O1 1.2945 (0.0025) N1 1.3690 (0.0027) 116.08 (0.18) C5 1.3969 (0.0030) 124.47 (0.19) 119.46 (0.19) C6 - O1 N1 C7 - Distance Angles Si1 1.8604 (0.0023) C7 - C8 - Distance Angles N2 1.4794 (0.0026) Si1 1.8969 (0.0023) 107.37 (0.14) C8 - N2 C9 - Distance Angles O2 1.2969 (0.0026) N2 1.3600 (0.0028) 116.40 (0.18) C10 1.4046 (0.0030) 124.49 (0.20) 119.12 (0.20) C9 - O2 N2 C10 - Distance Angles C11 1.3711 (0.0033) C9 1.4046 (0.0030) 118.73 (0.21) C10 - C11 C11 - Distance Angles C10 1.3711 (0.0033) C12 1.4003 (0.0035) 120.83 (0.21) C11 - C10 C12 - Distance Angles C13 1.3679 (0.0034) C11 1.4003 (0.0035) 119.27 (0.22) C12 - C13 C13 - Distance Angles N2 1.3586 (0.0029) C12 1.3679 (0.0034) 119.68 (0.22) C13 - N2 C14 - Distance Angles Cl5_$1 1.7644 (0.0028) Cl4 1.7650 (0.0030) 111.01 (0.15) Cl3 1.7673 (0.0029) 109.89 (0.15) 110.51 (0.15) C14 - Cl5_$1 Cl4 N1 - Distance Angles C2 1.3648 (0.0026) C6 1.3690 (0.0027) 120.61 (0.17) C1 1.4771 (0.0025) 124.78 (0.17) 114.53 (0.16) N1 - C2 C6 N2 - Distance Angles C13 1.3586 (0.0029) C9 1.3600 (0.0028) 122.36 (0.19) C8 1.4794 (0.0026) 123.36 (0.18) 114.26 (0.17) N2 - C13 C9 O1 - Distance Angles C6 1.2945 (0.0025) Si1 1.8505 (0.0015) 115.61 (0.13) O1 - C6 O2 - Distance Angles C9 1.2969 (0.0026) Si1 1.8671 (0.0015) 114.64 (0.13) O2 - C9 Si1 - Distance Angles O1 1.8505 (0.0015) C7 1.8604 (0.0023) 95.80 (0.09) O2 1.8671 (0.0015) 168.99 (0.07) 95.21 (0.09) C8 1.8969 (0.0023) 89.38 (0.08) 117.99 (0.11) 85.35 (0.08) C1 1.8978 (0.0021) 86.06 (0.08) 117.15 (0.11) 89.02 (0.08) 124.85 (0.10) Si1 - O1 C7 O2 C8 Cl1 - Distance Angles C2 1.7157 (0.0021) Cl1 - Cl3 - Distance Angles C14 1.7673 (0.0029) Cl3 - Cl4 - Distance Angles C14 1.7650 (0.0030) Cl4 - Cl5 - Distance Angles C14_$1 1.7644 (0.0028) Cl5 - FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0501 for 4386 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.37 at 0.1010 0.5007 0.4340 [ 1.42 A from CL4 ] Deepest hole -0.60 at 0.2734 0.4838 0.6636 [ 0.66 A from CL5 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2503 / 23580 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1010 0.4993 -0.4340 1.00000 0.05 0.37 1.42 CL4 3.18 C14 3.22 N1 3.23 H1B Q2 1 -0.5272 0.7756 -0.3971 1.00000 0.05 0.33 0.72 C4 0.78 C5 1.47 H4 1.52 H5 Q3 1 -0.3807 0.9194 0.1615 1.00000 0.05 0.33 0.54 H13 1.48 C13 2.05 CL2 2.41 N2 Q4 1 -0.0416 0.4798 -0.2186 1.00000 0.05 0.31 1.02 H7C 1.27 H7B 1.34 C7 2.20 H7A Q5 1 -0.4584 0.8274 -0.4793 1.00000 0.05 0.30 0.70 C4 0.71 C3 1.45 H4 1.47 H3 Q6 1 -0.3142 0.8302 -0.5009 1.00000 0.05 0.29 0.57 C3 0.80 C2 1.34 H3 1.73 C4 Q7 1 -0.1303 0.6033 -0.1536 1.00000 0.05 0.28 0.75 C7 1.14 SI1 1.31 H7C 1.40 H7B Q8 1 -0.2327 0.5031 -0.0947 1.00000 0.05 0.28 0.89 H7C 0.97 H7A 1.02 C7 1.86 H7B Q9 1 -0.1113 0.7406 -0.2621 1.00000 0.05 0.28 0.70 C1 1.22 SI1 1.34 H1B 1.49 H1A Q10 1 -0.2231 0.7645 -0.0803 1.00000 0.05 0.27 0.78 C8 1.17 SI1 1.40 H8B 1.58 H8A Shortest distances between peaks (including symmetry equivalents) 5 6 1.07 2 5 1.15 7 8 1.49 4 7 1.58 4 8 1.81 7 9 1.84 1 1 1.93 2 6 1.94 7 10 1.98 9 10 2.25 4 9 2.70 1 4 2.85 8 10 2.90 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.03: Generate connectivity array 0.03: 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 0.02: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.05: Analyse other restraints etc. 25.59: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.16: Structure factors and derivatives 4.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.19: Apply other restraints 2.88: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.50: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 18:29:21 Total CPU time: 37.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++