+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:28:28 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL DIRDIF output for 01SRC073 CELL 0.71073 9.2498 9.7081 17.7378 93.616 90.610 104.258 ZERR 4.00 0.0018 0.0019 0.0035 0.030 0.030 0.030 LATT 1 SFAC C H N CL SN SI UNIT 36 60 8 12 4 4 V = 1540.12 F(000) = 792.0 Mu = 2.24 mm-1 Cell Wt = 1617.44 Rho = 1.744 MERG 2 OMIT -3.00 55.00 OMIT 0 1 0 OMIT 0 0 2 OMIT 1 0 0 OMIT -1 1 0 OMIT 0 -1 6 OMIT -4 -1 4 EXTI 0.00715 FMAP 2 PLAN 10 SIZE 0.10 0.12 0.20 BOND WGHT 0.04400 L.S. 4 TEMP -123.00 FVAR 0.33470 C1 1 0.003420 0.262501 0.260400 11.00000 0.02018 0.01712 = 0.02700 -0.00108 -0.00032 0.00166 C2 1 -0.128294 0.291397 0.288614 11.00000 0.02339 0.02785 = 0.03372 -0.00295 0.00497 0.00569 AFIX 43 H2 2 -0.151549 0.283249 0.340437 11.00000 -1.20000 AFIX 0 C3 1 -0.222248 0.331818 0.238707 11.00000 0.02022 0.02949 = 0.05260 -0.00828 -0.00214 0.00786 AFIX 43 H3 2 -0.311555 0.352306 0.256713 11.00000 -1.20000 AFIX 0 C4 1 -0.190323 0.343603 0.162541 11.00000 0.02621 0.02432 = 0.05229 0.00179 -0.01231 0.00593 AFIX 43 H4 2 -0.256736 0.372188 0.129133 11.00000 -1.20000 AFIX 0 C5 1 -0.061404 0.313354 0.136204 11.00000 0.02574 0.02605 = 0.03438 0.00435 -0.00604 0.00318 C6 1 -0.015915 0.318182 0.055277 11.00000 0.04021 0.05319 = 0.03415 0.01441 -0.00536 0.00806 AFIX 137 H6A 2 0.086881 0.375632 0.052632 11.00000 -1.50000 H6B 2 -0.082660 0.360844 0.026433 11.00000 -1.50000 H6C 2 -0.022258 0.221225 0.033910 11.00000 -1.50000 AFIX 0 C7 1 0.040750 0.291428 0.453941 11.00000 0.04321 0.04583 = 0.02959 -0.00253 0.00423 0.00822 AFIX 137 H7A 2 0.037025 0.383946 0.435988 11.00000 -1.50000 H7B 2 0.082005 0.304830 0.505761 11.00000 -1.50000 H7C 2 -0.060248 0.228916 0.452948 11.00000 -1.50000 AFIX 0 C8 1 0.139231 0.021328 0.412783 11.00000 0.05685 0.04058 = 0.03618 0.01275 -0.00075 0.01001 AFIX 137 H8A 2 0.033423 -0.029009 0.408650 11.00000 -1.50000 H8B 2 0.177090 0.017330 0.464204 11.00000 -1.50000 H8C 2 0.195652 -0.023981 0.376689 11.00000 -1.50000 AFIX 0 C9 1 0.358447 0.312292 0.407751 11.00000 0.03328 0.05901 = 0.04403 -0.00561 -0.00489 0.00646 AFIX 137 H9A 2 0.425245 0.255631 0.387516 11.00000 -1.50000 H9B 2 0.378987 0.334303 0.462075 11.00000 -1.50000 H9C 2 0.374974 0.401157 0.382115 11.00000 -1.50000 AFIX 0 C10 1 -0.623643 -0.280955 0.236769 11.00000 0.02337 0.01673 = 0.02768 -0.00066 -0.00105 0.00350 C11 1 -0.769236 -0.321785 0.206445 11.00000 0.02789 0.03039 = 0.03342 -0.00227 -0.00487 0.00518 AFIX 43 H11 2 -0.787819 -0.325002 0.153506 11.00000 -1.20000 AFIX 0 C12 1 -0.883890 -0.356883 0.255032 11.00000 0.01935 0.02882 = 0.05288 -0.00324 -0.00354 0.00424 AFIX 43 H12 2 -0.983439 -0.384770 0.235263 11.00000 -1.20000 AFIX 0 C13 1 -0.858985 -0.352950 0.332854 11.00000 0.02480 0.03214 = 0.04384 -0.00056 0.01092 0.00588 AFIX 43 H13 2 -0.940329 -0.378086 0.365726 11.00000 -1.20000 AFIX 0 C14 1 -0.714964 -0.312156 0.361260 11.00000 0.03306 0.02713 = 0.03382 0.00089 0.00875 0.01001 C15 1 -0.672213 -0.299266 0.443801 11.00000 0.04106 0.05191 = 0.03222 0.00169 0.00976 0.01210 AFIX 137 H15A 2 -0.593632 -0.348968 0.451790 11.00000 -1.50000 H15B 2 -0.759634 -0.341980 0.472769 11.00000 -1.50000 H15C 2 -0.635478 -0.198441 0.460701 11.00000 -1.50000 AFIX 0 C16 1 -0.303146 -0.323358 0.082645 11.00000 0.04286 0.04075 = 0.04013 -0.00032 0.01079 0.01472 AFIX 137 H16A 2 -0.215611 -0.293980 0.116918 11.00000 -1.50000 H16B 2 -0.272025 -0.308945 0.030491 11.00000 -1.50000 H16C 2 -0.350767 -0.424315 0.087419 11.00000 -1.50000 AFIX 0 C17 1 -0.352575 -0.023394 0.097462 11.00000 0.05967 0.02843 = 0.03942 0.00717 0.01609 0.00471 AFIX 137 H17A 2 -0.426950 0.031421 0.107730 11.00000 -1.50000 H17B 2 -0.317397 -0.010015 0.045880 11.00000 -1.50000 H17C 2 -0.268141 0.009674 0.133443 11.00000 -1.50000 AFIX 0 C18 1 -0.602943 -0.276199 0.042232 11.00000 0.05060 0.04715 = 0.02580 0.00093 -0.00352 0.01528 AFIX 137 H18A 2 -0.651434 -0.375921 0.049825 11.00000 -1.50000 H18B 2 -0.570773 -0.267747 -0.010100 11.00000 -1.50000 H18C 2 -0.673604 -0.217334 0.052517 11.00000 -1.50000 AFIX 0 N1 3 0.114946 0.218267 0.295631 11.00000 0.02244 0.02639 = 0.02325 0.00226 0.00236 0.00890 N2 3 0.029682 0.272332 0.185345 11.00000 0.02312 0.02378 = 0.02718 0.00362 0.00086 0.00670 N3 3 -0.488314 -0.239525 0.202700 11.00000 0.02181 0.02434 = 0.02480 -0.00088 -0.00119 0.00059 N4 3 -0.602027 -0.277841 0.312649 11.00000 0.02185 0.02500 = 0.02760 0.00157 0.00233 0.00714 CL1 4 0.147668 0.014679 0.099934 11.00000 0.05147 0.04073 = 0.03952 -0.01399 0.00423 0.01052 CL2 4 0.403178 0.077252 0.251298 11.00000 0.04119 0.04383 = 0.05078 0.00836 0.00254 0.02763 CL3 4 0.397128 0.380561 0.153157 11.00000 0.02814 0.03295 = 0.05718 0.01469 0.01176 0.00562 CL4 4 -0.302948 -0.387953 0.361211 11.00000 0.03791 0.03740 = 0.04314 0.00562 -0.00323 0.01603 CL5 4 -0.123996 -0.114482 0.249070 11.00000 0.02358 0.05042 = 0.04938 0.00086 0.00300 -0.00360 CL6 4 -0.344351 -0.011659 0.391366 11.00000 0.04442 0.03343 = 0.03764 -0.01257 -0.00832 0.00691 SN1 5 0.229330 0.185996 0.198835 11.00000 0.02273 0.02262 = 0.02541 0.00227 0.00434 0.00813 SN2 5 -0.358366 -0.199704 0.301483 11.00000 0.02113 0.02556 = 0.02454 -0.00168 -0.00237 0.00339 SI1 6 0.160965 0.209213 0.391677 11.00000 0.02841 0.02966 = 0.02287 0.00169 -0.00049 0.00485 SI2 6 -0.438075 -0.214775 0.107541 11.00000 0.03241 0.02193 = 0.02374 0.00084 0.00214 0.00631 HKLF 4 Covalent radii and connectivity table for DIRDIF output for 01SRC073 C 0.770 H 0.320 N 0.700 CL 0.990 SN 1.400 SI 1.170 C1 - N2 N1 C2 Sn1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - N2 C4 C6 C6 - C5 C7 - Si1 C8 - Si1 C9 - Si1 C10 - N4 N3 C11 Sn2 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - N4 C13 C15 C15 - C14 C16 - Si2 C17 - Si2 C18 - Si2 N1 - C1 Si1 Sn1 N2 - C5 C1 Sn1 N3 - C10 Si2 Sn2 N4 - C14 C10 Sn2 Cl1 - Sn1 Cl2 - Sn1 Cl3 - Sn1 Cl4 - Sn2 Cl5 - Sn2 Cl6 - Sn2 Sn1 - N1 N2 Cl1 Cl3 Cl2 C1 Sn2 - N3 N4 Cl6 Cl4 Cl5 C10 Si1 - N1 C8 C7 C9 Si2 - N3 C17 C18 C16 23545 Reflections read, of which 24 rejected -12 =< h =< 11, -12 =< k =< 12, -23 =< l =< 23, Max. 2-theta = 54.92 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 4 0 1685.76 50.27 2 356.36 -1 0 1 139.50 3.04 6 38.17 1 0 1 115.47 3.54 4 28.03 -3 1 1 74.82 1.05 5 9.96 -9 3 1 149.68 3.03 5 24.56 -3 0 2 78.02 0.29 7 13.50 -2 0 2 8.83 0.13 4 2.28 -1 0 2 320.99 0.42 5 388.70 -6 2 2 548.39 6.56 5 68.37 -7 3 2 291.16 0.85 5 88.93 -6 3 2 47.76 1.07 3 18.37 -8 4 2 183.35 1.28 5 52.90 -3 2 3 77.57 0.42 6 14.49 -7 4 3 132.90 2.89 5 17.00 -8 5 3 31.49 0.99 5 6.21 -2 1 4 57.55 0.43 2 167.89 -3 2 4 77.82 0.42 6 13.10 -6 4 4 142.75 1.44 6 17.72 -4 -1 6 43.08 0.51 7 4.35 -3 2 6 563.54 9.77 3 163.89 -4 -1 7 191.98 1.35 7 21.10 -5 4 7 672.96 1.01 5 325.59 -6 5 7 59.81 0.80 6 9.18 -4 3 8 105.71 4.46 2 46.34 1 -1 9 519.89 11.44 3 59.11 1 -1 10 1373.39 26.03 4 136.02 -6 -2 11 67.10 1.37 3 25.85 3 2 12 473.76 13.63 2 122.85 28 Inconsistent equivalents 6924 Unique reflections, of which 0 suppressed R(int) = 0.0809 R(sigma) = 0.0559 Friedel opposites merged Maximum memory for data reduction = 2911 / 69469 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 = 3755 / 374742 wR2 = 0.0822 before cycle 1 for 6924 data and 298 / 298 parameters GooF = S = 0.992; Restrained GooF = 0.992 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0440 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33321 0.00047 -3.167 OSF 2 0.00288 0.00047 -9.077 EXTI Mean shift/esd = 0.271 Maximum = -9.077 for EXTI Max. shift = 0.012 A for H8B Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3755 / 374742 wR2 = 0.0812 before cycle 2 for 6924 data and 298 / 298 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0440 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33282 0.00045 -0.860 OSF 2 0.00215 0.00039 -1.863 EXTI Mean shift/esd = 0.085 Maximum = -1.863 for EXTI Max. shift = 0.008 A for H17A Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3755 / 374742 wR2 = 0.0812 before cycle 3 for 6924 data and 298 / 298 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0440 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33282 0.00045 0.004 OSF 2 0.00217 0.00037 0.038 EXTI Mean shift/esd = 0.006 Maximum = 0.118 for tors H17A Max. shift = 0.003 A for H17C Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3755 / 374742 wR2 = 0.0812 before cycle 4 for 6924 data and 298 / 298 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0440 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33282 0.00045 0.007 OSF 2 0.00218 0.00037 0.037 EXTI Mean shift/esd = 0.002 Maximum = 0.043 for tors H17A Max. shift = 0.001 A for H17C Max. dU = 0.000 for C3 Largest correlation matrix elements 0.602 U11 Sn2 / U11 Sn1 0.569 EXTI / OSF 0.558 U33 Sn2 / U33 Sn1 0.600 U11 Sn2 / OSF 0.569 U33 Sn1 / OSF 0.534 U12 Cl2 / U22 Cl2 0.597 U11 Sn1 / OSF 0.565 U22 Sn2 / OSF 0.516 U12 Cl2 / U11 Cl2 0.581 U22 Sn1 / OSF 0.559 U33 Sn2 / OSF 0.513 U22 Sn2 / U22 Sn1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.1519 0.2828 0.3404 43 0.950 0.000 C2 C3 C1 H3 -0.3115 0.3523 0.2566 43 0.950 0.000 C3 C2 C4 H4 -0.2568 0.3721 0.1293 43 0.950 0.000 C4 C5 C3 H6A 0.0866 0.3759 0.0526 137 0.980 0.000 C6 C5 H6A H6B -0.0831 0.3598 0.0263 137 0.980 0.000 C6 C5 H6A H6C -0.0215 0.2210 0.0341 137 0.980 0.000 C6 C5 H6A H7A 0.0370 0.3838 0.4361 137 0.980 0.000 C7 Si1 H7A H7B 0.0815 0.3042 0.5058 137 0.980 0.000 C7 Si1 H7A H7C -0.0605 0.2287 0.4527 137 0.980 0.000 C7 Si1 H7A H8A 0.0336 -0.0295 0.4076 137 0.980 0.000 C8 Si1 H8A H8B 0.1751 0.0172 0.4645 137 0.980 0.000 C8 Si1 H8A H8C 0.1972 -0.0235 0.3773 137 0.980 0.000 C8 Si1 H8A H9A 0.4251 0.2558 0.3867 137 0.980 0.000 C9 Si1 H9A H9B 0.3796 0.3330 0.4619 137 0.980 0.000 C9 Si1 H9A H9C 0.3748 0.4015 0.3825 137 0.980 0.000 C9 Si1 H9A H11 -0.7879 -0.3250 0.1536 43 0.950 0.000 C11 C12 C10 H12 -0.9833 -0.3845 0.2353 43 0.950 0.000 C12 C11 C13 H13 -0.9404 -0.3780 0.3657 43 0.950 0.000 C13 C14 C12 H15A -0.5938 -0.3491 0.4518 137 0.980 0.000 C15 C14 H15A H15B -0.7594 -0.3409 0.4729 137 0.980 0.000 C15 C14 H15A H15C -0.6345 -0.1980 0.4605 137 0.980 0.000 C15 C14 H15A H16A -0.2145 -0.2922 0.1164 137 0.980 0.000 C16 Si2 H16A H16B -0.2733 -0.3102 0.0303 137 0.980 0.000 C16 Si2 H16A H16C -0.3496 -0.4239 0.0886 137 0.980 0.000 C16 Si2 H16A H17A -0.4260 0.0318 0.1089 137 0.980 0.000 C17 Si2 H17A H17B -0.3192 -0.0097 0.0456 137 0.980 0.000 C17 Si2 H17A H17C -0.2666 0.0091 0.1327 137 0.980 0.000 C17 Si2 H17A H18A -0.6517 -0.3755 0.0499 137 0.980 0.000 C18 Si2 H18A H18B -0.5704 -0.2679 -0.0101 137 0.980 0.000 C18 Si2 H18A H18C -0.6731 -0.2167 0.0523 137 0.980 0.000 C18 Si2 H18A DIRDIF output for 01SRC073 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.00348 0.26245 0.26032 1.00000 0.02010 0.01692 0.02704 -0.00119 -0.00048 0.00174 0.02197 0.00459 0.00026 0.00024 0.00014 0.00000 0.00112 0.00116 0.00130 0.00097 0.00103 0.00091 0.00050 C2 -0.12850 0.29116 0.28861 1.00000 0.02281 0.02765 0.03412 -0.00316 0.00512 0.00537 0.02854 0.00515 0.00028 0.00028 0.00016 0.00000 0.00121 0.00137 0.00148 0.00112 0.00114 0.00104 0.00058 H2 -0.15189 0.28282 0.34041 1.00000 0.03425 0.00000 0.00000 C3 -0.22225 0.33169 0.23862 1.00000 0.01988 0.02968 0.05148 -0.00779 -0.00163 0.00774 0.03388 0.00534 0.00029 0.00028 0.00018 0.00000 0.00121 0.00148 0.00188 0.00131 0.00127 0.00107 0.00066 H3 -0.31155 0.35225 0.25660 1.00000 0.04065 0.00000 0.00000 C4 -0.19040 0.34350 0.16267 1.00000 0.02639 0.02412 0.05281 0.00131 -0.01282 0.00628 0.03459 0.00544 0.00030 0.00028 0.00018 0.00000 0.00133 0.00139 0.00193 0.00129 0.00134 0.00109 0.00067 H4 -0.25683 0.37214 0.12930 1.00000 0.04151 0.00000 0.00000 C5 -0.06140 0.31322 0.13620 1.00000 0.02498 0.02600 0.03454 0.00421 -0.00576 0.00306 0.02903 0.00516 0.00028 0.00028 0.00016 0.00000 0.00124 0.00135 0.00149 0.00113 0.00116 0.00104 0.00057 C6 -0.01592 0.31790 0.05529 1.00000 0.04068 0.05345 0.03337 0.01463 -0.00572 0.00830 0.04263 0.00617 0.00034 0.00035 0.00016 0.00000 0.00162 0.00195 0.00160 0.00141 0.00136 0.00144 0.00073 H6A 0.08661 0.37594 0.05260 1.00000 0.06394 0.00000 0.00000 H6B -0.08313 0.35984 0.02634 1.00000 0.06394 0.00000 0.00000 H6C -0.02153 0.22098 0.03409 1.00000 0.06394 0.00000 0.00000 C7 0.04054 0.29116 0.45393 1.00000 0.04281 0.04570 0.02985 -0.00280 0.00430 0.00825 0.04014 0.00598 0.00035 0.00033 0.00017 0.00000 0.00162 0.00178 0.00150 0.00130 0.00133 0.00137 0.00070 H7A 0.03702 0.38385 0.43613 1.00000 0.06021 0.00000 0.00000 H7B 0.08151 0.30419 0.50580 1.00000 0.06021 0.00000 0.00000 H7C -0.06051 0.22872 0.45273 1.00000 0.06021 0.00000 0.00000 C8 0.13916 0.02128 0.41274 1.00000 0.05724 0.03978 0.03649 0.01238 -0.00124 0.01015 0.04442 0.00654 0.00038 0.00032 0.00018 0.00000 0.00196 0.00175 0.00170 0.00137 0.00154 0.00148 0.00076 H8A 0.03357 -0.02948 0.40759 1.00000 0.06662 0.00000 0.00000 H8B 0.17510 0.01718 0.46453 1.00000 0.06662 0.00000 0.00000 H8C 0.19721 -0.02351 0.37730 1.00000 0.06662 0.00000 0.00000 C9 0.35853 0.31204 0.40759 1.00000 0.03380 0.05879 0.04323 -0.00559 -0.00540 0.00663 0.04656 0.00607 0.00033 0.00037 0.00019 0.00000 0.00154 0.00211 0.00183 0.00154 0.00142 0.00144 0.00079 H9A 0.42513 0.25576 0.38670 1.00000 0.06984 0.00000 0.00000 H9B 0.37961 0.33297 0.46193 1.00000 0.06984 0.00000 0.00000 H9C 0.37476 0.40147 0.38250 1.00000 0.06984 0.00000 0.00000 C10 -0.62350 -0.28081 0.23682 1.00000 0.02292 0.01650 0.02778 -0.00054 -0.00087 0.00330 0.02278 0.00477 0.00027 0.00025 0.00014 0.00000 0.00117 0.00117 0.00132 0.00098 0.00104 0.00093 0.00051 C11 -0.76930 -0.32172 0.20651 1.00000 0.02751 0.03041 0.03385 -0.00247 -0.00501 0.00520 0.03118 0.00514 0.00028 0.00027 0.00017 0.00000 0.00136 0.00148 0.00151 0.00119 0.00122 0.00112 0.00061 H11 -0.78793 -0.32502 0.15357 1.00000 0.03742 0.00000 0.00000 C12 -0.88379 -0.35670 0.25508 1.00000 0.01972 0.02885 0.05191 -0.00295 -0.00376 0.00440 0.03406 0.00541 0.00029 0.00029 0.00018 0.00000 0.00124 0.00146 0.00188 0.00130 0.00128 0.00106 0.00066 H12 -0.98334 -0.38453 0.23530 1.00000 0.04087 0.00000 0.00000 C13 -0.85905 -0.35282 0.33282 1.00000 0.02473 0.03223 0.04376 -0.00089 0.01084 0.00587 0.03386 0.00561 0.00030 0.00029 0.00017 0.00000 0.00129 0.00151 0.00173 0.00126 0.00129 0.00112 0.00065 H13 -0.94042 -0.37795 0.36567 1.00000 0.04063 0.00000 0.00000 C14 -0.71485 -0.31201 0.36124 1.00000 0.03199 0.02696 0.03404 0.00071 0.00896 0.00963 0.03059 0.00552 0.00030 0.00028 0.00016 0.00000 0.00139 0.00137 0.00150 0.00114 0.00124 0.00110 0.00060 C15 -0.67191 -0.29886 0.44378 1.00000 0.04130 0.05219 0.03150 0.00203 0.00959 0.01236 0.04150 0.00617 0.00036 0.00034 0.00016 0.00000 0.00154 0.00197 0.00161 0.00140 0.00136 0.00139 0.00073 H15A -0.59379 -0.34909 0.45182 1.00000 0.06224 0.00000 0.00000 H15B -0.75942 -0.34089 0.47285 1.00000 0.06224 0.00000 0.00000 H15C -0.63450 -0.19802 0.46050 1.00000 0.06224 0.00000 0.00000 C16 -0.30287 -0.32308 0.08276 1.00000 0.04290 0.04033 0.04003 -0.00056 0.01054 0.01486 0.04036 0.00638 0.00035 0.00032 0.00018 0.00000 0.00164 0.00169 0.00173 0.00136 0.00144 0.00137 0.00071 H16A -0.21447 -0.29217 0.11637 1.00000 0.06054 0.00000 0.00000 H16B -0.27332 -0.31021 0.03027 1.00000 0.06054 0.00000 0.00000 H16C -0.34964 -0.42387 0.08857 1.00000 0.06054 0.00000 0.00000 C17 -0.35238 -0.02336 0.09754 1.00000 0.06007 0.02795 0.03932 0.00689 0.01578 0.00449 0.04326 0.00651 0.00040 0.00030 0.00018 0.00000 0.00198 0.00152 0.00173 0.00129 0.00159 0.00138 0.00077 H17A -0.42603 0.03177 0.10894 1.00000 0.06489 0.00000 0.00000 H17B -0.31920 -0.00967 0.04565 1.00000 0.06489 0.00000 0.00000 H17C -0.26656 0.00906 0.13273 1.00000 0.06489 0.00000 0.00000 C18 -0.60277 -0.27591 0.04223 1.00000 0.05097 0.04701 0.02622 0.00059 -0.00380 0.01548 0.04093 0.00604 0.00036 0.00034 0.00016 0.00000 0.00182 0.00184 0.00148 0.00130 0.00137 0.00147 0.00071 H18A -0.65167 -0.37548 0.04995 1.00000 0.06140 0.00000 0.00000 H18B -0.57045 -0.26787 -0.01010 1.00000 0.06140 0.00000 0.00000 H18C -0.67313 -0.21666 0.05234 1.00000 0.06140 0.00000 0.00000 N1 0.11493 0.21818 0.29565 1.00000 0.02193 0.02616 0.02337 0.00227 0.00262 0.00866 0.02331 0.00407 0.00022 0.00022 0.00012 0.00000 0.00098 0.00110 0.00106 0.00085 0.00087 0.00084 0.00044 N2 0.02955 0.27214 0.18542 1.00000 0.02283 0.02379 0.02687 0.00371 0.00108 0.00666 0.02425 0.00410 0.00022 0.00022 0.00012 0.00000 0.00102 0.00108 0.00112 0.00087 0.00091 0.00085 0.00045 N3 -0.48827 -0.23940 0.20267 1.00000 0.02196 0.02405 0.02496 -0.00109 -0.00143 0.00072 0.02467 0.00395 0.00022 0.00022 0.00012 0.00000 0.00101 0.00110 0.00111 0.00087 0.00088 0.00083 0.00045 N4 -0.60199 -0.27768 0.31259 1.00000 0.02204 0.02490 0.02704 0.00145 0.00201 0.00724 0.02441 0.00411 0.00022 0.00022 0.00012 0.00000 0.00101 0.00110 0.00114 0.00088 0.00091 0.00085 0.00045 Cl1 0.14769 0.01469 0.09993 1.00000 0.05126 0.04055 0.03947 -0.01409 0.00416 0.01049 0.04462 0.00150 0.00009 0.00008 0.00004 0.00000 0.00044 0.00042 0.00042 0.00033 0.00036 0.00034 0.00020 Cl2 0.40315 0.07721 0.25131 1.00000 0.04091 0.04356 0.05070 0.00833 0.00254 0.02749 0.04184 0.00161 0.00008 0.00008 0.00005 0.00000 0.00039 0.00042 0.00045 0.00034 0.00035 0.00033 0.00018 Cl3 0.39713 0.38054 0.15316 1.00000 0.02792 0.03280 0.05712 0.01471 0.01183 0.00557 0.03904 0.00152 0.00007 0.00007 0.00005 0.00000 0.00032 0.00037 0.00047 0.00033 0.00033 0.00028 0.00018 Cl4 -0.30297 -0.38795 0.36123 1.00000 0.03786 0.03721 0.04305 0.00554 -0.00331 0.01608 0.03809 0.00149 0.00008 0.00008 0.00004 0.00000 0.00037 0.00039 0.00041 0.00032 0.00033 0.00030 0.00017 Cl5 -0.12398 -0.11446 0.24907 1.00000 0.02333 0.05032 0.04923 0.00085 0.00305 -0.00368 0.04330 0.00143 0.00007 0.00009 0.00005 0.00000 0.00032 0.00045 0.00045 0.00036 0.00032 0.00030 0.00019 Cl6 -0.34435 -0.01164 0.39134 1.00000 0.04430 0.03321 0.03756 -0.01264 -0.00843 0.00696 0.03954 0.00134 0.00008 0.00008 0.00004 0.00000 0.00039 0.00037 0.00039 0.00030 0.00033 0.00030 0.00018 Sn1 0.22934 0.18599 0.19883 1.00000 0.02254 0.02243 0.02519 0.00226 0.00433 0.00808 0.02289 0.00033 0.00002 0.00002 0.00001 0.00000 0.00011 0.00011 0.00012 0.00007 0.00008 0.00007 0.00008 Sn2 -0.35836 -0.19970 0.30148 1.00000 0.02095 0.02538 0.02432 -0.00169 -0.00238 0.00334 0.02414 0.00031 0.00002 0.00002 0.00001 0.00000 0.00011 0.00011 0.00012 0.00008 0.00008 0.00007 0.00008 Si1 0.16100 0.20922 0.39166 1.00000 0.02820 0.02944 0.02268 0.00168 -0.00051 0.00477 0.02720 0.00141 0.00008 0.00008 0.00004 0.00000 0.00036 0.00039 0.00036 0.00030 0.00030 0.00030 0.00016 Si2 -0.43809 -0.21478 0.10756 1.00000 0.03217 0.02176 0.02350 0.00088 0.00219 0.00624 0.02590 0.00142 0.00008 0.00007 0.00004 0.00000 0.00037 0.00035 0.00036 0.00028 0.00030 0.00029 0.00016 Final Structure Factor Calculation for DIRDIF output for 01SRC073 Total number of l.s. parameters = 298 Maximum vector length = 511 Memory required = 3457 / 25039 wR2 = 0.0812 before cycle 5 for 6924 data and 0 / 298 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0440 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0307 for 5961 Fo > 4sig(Fo) and 0.0386 for all 6924 data wR2 = 0.0812, GooF = S = 0.980, Restrained GooF = 0.980 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0279 0.0226 0.0154 C1 0.0395 0.0254 0.0207 C2 0.0565 0.0261 0.0190 C3 0.0592 0.0241 0.0205 C4 0.0397 0.0257 0.0216 C5 0.0621 0.0415 0.0242 C6 0.0511 0.0417 0.0276 C7 0.0595 0.0468 0.0270 C8 0.0647 0.0449 0.0301 C9 0.0285 0.0237 0.0162 C10 0.0384 0.0319 0.0232 C11 0.0539 0.0292 0.0191 C12 0.0501 0.0315 0.0200 C13 0.0412 0.0288 0.0218 C14 0.0525 0.0461 0.0259 C15 0.0508 0.0429 0.0274 C16 0.0697 0.0360 0.0240 C17 0.0534 0.0440 0.0254 C18 0.0272 0.0235 0.0192 N1 0.0277 0.0233 0.0217 N2 0.0300 0.0261 0.0179 N3 0.0274 0.0252 0.0207 N4 0.0609 0.0499 0.0231 Cl1 0.0578 0.0487 0.0191 Cl2 0.0623 0.0331 0.0217 Cl3 0.0457 0.0424 0.0261 Cl4 0.0610 0.0483 0.0206 Cl5 0.0537 0.0446 0.0203 Cl6 0.0279 0.0226 0.0182 Sn1 0.0286 0.0254 0.0183 Sn2 0.0321 0.0271 0.0225 Si1 0.0327 0.0236 0.0214 Si2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.041 0.061 0.085 0.112 0.141 0.173 0.224 0.307 1.000 Number in group 717. 682. 693. 676. 708. 675. 691. 706. 681. 695. GooF 1.084 1.015 1.063 1.058 1.004 0.969 0.849 0.867 0.917 0.946 K 1.399 0.993 0.960 0.962 0.972 0.979 1.007 1.016 1.028 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 694. 696. 703. 681. 686. 707. 680. 695. 685. 697. GooF 0.930 0.825 0.915 0.918 0.934 0.967 0.933 0.927 0.965 1.381 K 0.990 1.010 1.006 1.015 1.032 1.040 1.042 1.026 1.006 0.979 R1 0.088 0.066 0.064 0.047 0.041 0.033 0.031 0.025 0.024 0.028 Recommended weighting scheme: WGHT 0.0288 0.1952 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 -1 8 584.73 411.95 5.35 0.090 2.19 -3 2 5 181.13 137.73 5.13 0.052 2.21 -1 0 7 22.38 3.13 5.03 0.008 2.45 0 2 4 227.13 162.64 5.02 0.057 3.12 2 -5 3 41.88 6.00 4.95 0.011 1.85 2 2 0 734.01 585.85 4.78 0.108 2.90 -2 -1 1 20.15 11.05 4.46 0.015 3.66 1 -2 4 1350.31 1694.66 4.30 0.184 3.30 -3 2 0 308.07 388.13 4.29 0.088 2.86 0 1 8 311.38 233.83 4.21 0.068 2.12 1 0 5 520.84 661.26 4.19 0.115 3.26 -2 1 5 689.99 863.01 4.13 0.131 2.77 1 1 6 61.89 100.39 4.09 0.045 2.57 -1 4 4 35.98 17.78 4.04 0.019 2.07 -2 1 6 14.35 3.62 4.03 0.008 2.46 0 5 1 40.30 15.59 3.89 0.018 1.85 0 -1 3 22.80 0.93 3.86 0.004 5.15 3 3 0 36.85 6.10 3.86 0.011 1.93 0 3 0 1575.37 1306.19 3.77 0.161 3.13 -1 1 5 593.67 747.86 3.71 0.122 3.16 3 4 8 272.29 336.86 3.59 0.082 1.29 -1 -2 7 1569.10 1879.08 3.56 0.193 2.17 3 1 3 495.61 600.03 3.53 0.109 2.39 -1 0 1 1273.15 2467.87 3.46 0.221 8.08 4 -3 6 32.12 61.46 3.45 0.035 1.72 3 -3 3 7142.15 9066.19 3.39 0.425 2.32 -2 10 11 202.91 374.92 3.38 0.086 0.81 -4 5 6 27.40 8.27 3.38 0.013 1.42 -1 6 1 44.99 9.14 3.37 0.013 1.59 -2 -4 6 428.14 355.05 3.36 0.084 1.64 -5 3 7 716.99 855.72 3.35 0.130 1.43 1 -3 7 68.66 94.13 3.32 0.043 2.05 -2 5 2 349.03 291.60 3.32 0.076 1.84 -2 0 8 702.27 836.73 3.28 0.129 2.01 -1 6 5 35.29 12.70 3.26 0.016 1.43 -1 5 1 1849.87 1575.29 3.26 0.177 1.91 -2 2 2 196.41 164.12 3.25 0.057 3.40 -9 6 1 49.15 77.74 3.23 0.039 0.95 3 -5 3 88.04 54.37 3.22 0.033 1.75 3 -1 1 4846.99 5710.40 3.21 0.337 3.03 -3 -1 4 11.86 1.98 3.19 0.006 2.33 -4 3 3 95.42 70.29 3.14 0.037 1.95 -8 -4 10 507.15 680.87 3.10 0.116 0.84 10 0 11 133.99 305.27 3.09 0.078 0.77 5 -9 4 111.17 45.77 3.08 0.030 1.00 -5 7 8 33.76 3.33 3.07 0.008 1.06 2 0 5 592.54 718.24 3.07 0.119 2.74 4 1 7 9956.90 11809.07 3.06 0.485 1.57 -3 0 2 705.55 1084.17 3.06 0.147 2.85 1 -8 5 95.75 57.08 3.05 0.034 1.16 Bond lengths and angles C1 - Distance Angles N2 1.3577 (0.0032) N1 1.3706 (0.0032) 110.43 (0.20) C2 1.4081 (0.0035) 118.81 (0.24) 130.70 (0.24) Sn1 2.6105 (0.0024) 58.44 (0.12) 52.13 (0.12) 173.70 (0.18) C1 - N2 N1 C2 C2 - Distance Angles C3 1.3743 (0.0042) C1 1.4081 (0.0035) 117.63 (0.26) C2 - C3 C3 - Distance Angles C2 1.3743 (0.0042) C4 1.3879 (0.0044) 121.98 (0.25) C3 - C2 C4 - Distance Angles C5 1.3777 (0.0039) C3 1.3879 (0.0044) 119.28 (0.27) C4 - C5 C5 - Distance Angles N2 1.3500 (0.0035) C4 1.3777 (0.0039) 118.47 (0.26) C6 1.5000 (0.0039) 116.86 (0.23) 124.64 (0.27) C5 - N2 C4 C6 - Distance Angles C5 1.5000 (0.0039) C6 - C7 - Distance Angles Si1 1.8565 (0.0029) C7 - C8 - Distance Angles Si1 1.8481 (0.0031) C8 - C9 - Distance Angles Si1 1.8626 (0.0031) C9 - C10 - Distance Angles N4 1.3537 (0.0033) N3 1.3756 (0.0031) 109.83 (0.22) C11 1.3998 (0.0036) 118.98 (0.23) 131.19 (0.24) Sn2 2.6124 (0.0026) 57.70 (0.13) 52.14 (0.12) 176.35 (0.19) C10 - N4 N3 C11 C11 - Distance Angles C12 1.3632 (0.0039) C10 1.3998 (0.0036) 118.14 (0.27) C11 - C12 C12 - Distance Angles C11 1.3632 (0.0039) C13 1.3919 (0.0043) 121.90 (0.26) C12 - C11 C13 - Distance Angles C14 1.3750 (0.0041) C12 1.3919 (0.0043) 118.87 (0.25) C13 - C14 C14 - Distance Angles N4 1.3527 (0.0033) C13 1.3750 (0.0040) 118.78 (0.26) C15 1.5021 (0.0041) 116.55 (0.25) 124.65 (0.26) C14 - N4 C13 C15 - Distance Angles C14 1.5021 (0.0041) C15 - C16 - Distance Angles Si2 1.8613 (0.0029) C16 - C17 - Distance Angles Si2 1.8526 (0.0029) C17 - C18 - Distance Angles Si2 1.8563 (0.0032) C18 - N1 - Distance Angles C1 1.3706 (0.0032) Si1 1.7639 (0.0023) 132.69 (0.17) Sn1 2.0737 (0.0020) 96.42 (0.15) 130.56 (0.11) N1 - C1 Si1 N2 - Distance Angles C5 1.3500 (0.0035) C1 1.3577 (0.0032) 123.79 (0.21) Sn1 2.2245 (0.0021) 145.79 (0.18) 90.22 (0.15) N2 - C5 C1 N3 - Distance Angles C10 1.3756 (0.0031) Si2 1.7697 (0.0022) 132.88 (0.18) Sn2 2.0751 (0.0022) 96.30 (0.16) 130.69 (0.11) N3 - C10 Si2 N4 - Distance Angles C14 1.3527 (0.0033) C10 1.3537 (0.0033) 123.32 (0.23) Sn2 2.2087 (0.0020) 145.54 (0.19) 91.09 (0.15) N4 - C14 C10 Cl1 - Distance Angles Sn1 2.3235 (0.0011) Cl1 - Cl2 - Distance Angles Sn1 2.3441 (0.0009) Cl2 - Cl3 - Distance Angles Sn1 2.3256 (0.0011) Cl3 - Cl4 - Distance Angles Sn2 2.3279 (0.0009) Cl4 - Cl5 - Distance Angles Sn2 2.3464 (0.0010) Cl5 - Cl6 - Distance Angles Sn2 2.3244 (0.0010) Cl6 - Sn1 - Distance Angles N1 2.0737 (0.0020) N2 2.2245 (0.0021) 62.73 (0.08) Cl1 2.3235 (0.0011) 127.00 (0.06) 91.64 (0.06) Cl3 2.3256 (0.0011) 118.44 (0.07) 95.51 (0.06) 108.99 (0.04) Cl2 2.3441 (0.0009) 98.93 (0.06) 161.00 (0.06) 96.43 (0.04) 98.05 (0.03) C1 2.6105 (0.0024) 31.45 (0.08) 31.34 (0.08) 110.47 (0.06) 110.88 (0.06) 130.00 (0.06) Sn1 - N1 N2 Cl1 Cl3 Cl2 Sn2 - Distance Angles N3 2.0751 (0.0022) N4 2.2087 (0.0020) 62.76 (0.08) Cl6 2.3244 (0.0010) 126.03 (0.06) 92.58 (0.06) Cl4 2.3279 (0.0009) 119.98 (0.06) 94.28 (0.06) 108.33 (0.03) Cl5 2.3464 (0.0010) 98.82 (0.06) 161.45 (0.06) 97.40 (0.04) 97.33 (0.04) C10 2.6124 (0.0026) 31.56 (0.08) 31.20 (0.08) 111.25 (0.06) 110.03 (0.06) 130.32 (0.06) Sn2 - N3 N4 Cl6 Cl4 Cl5 Si1 - Distance Angles N1 1.7639 (0.0023) C8 1.8481 (0.0031) 109.66 (0.13) C7 1.8565 (0.0029) 110.85 (0.13) 109.75 (0.15) C9 1.8626 (0.0031) 107.12 (0.14) 110.61 (0.16) 108.82 (0.14) Si1 - N1 C8 C7 Si2 - Distance Angles N3 1.7697 (0.0022) C17 1.8526 (0.0029) 109.02 (0.12) C18 1.8563 (0.0032) 111.36 (0.12) 109.63 (0.16) C16 1.8613 (0.0029) 108.36 (0.13) 110.46 (0.15) 108.00 (0.14) Si2 - N3 C17 C18 FMAP and GRID set by program FMAP 2 3 42 GRID -1.282 -2 -2 1.282 2 2 R1 = 0.0381 for 6924 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.74 at 0.8189 0.5738 0.0957 [ 1.44 A from H16A ] Deepest hole -1.08 at 0.6933 0.8734 0.2881 [ 0.80 A from SN2 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3240 / 28101 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1811 -0.4262 0.0957 1.00000 0.05 0.74 1.44 H16A 1.57 H16C 1.70 C16 1.99 H16B Q2 1 -0.1041 -0.1768 0.3009 1.00000 0.05 0.67 1.17 CL5 2.31 SN2 2.44 H8A 2.68 CL4 Q3 1 -0.4797 -0.2924 0.3335 1.00000 0.05 0.59 1.23 N4 1.40 SN2 2.14 CL4 2.18 C10 Q4 1 0.1262 0.1033 0.2410 1.00000 0.05 0.58 1.35 SN1 1.46 N1 2.14 C1 2.32 N2 Q5 1 0.4892 0.2183 0.1967 1.00000 0.05 0.56 1.76 CL2 2.15 CL3 2.20 H3 2.35 SN1 Q6 1 0.0516 0.4144 0.4053 1.00000 0.05 0.55 0.64 H7A 1.50 C7 2.08 H7C 2.16 H13 Q7 1 0.1155 0.1910 0.1982 1.00000 0.05 0.49 1.07 SN1 1.28 N2 1.73 N1 1.75 C1 Q8 1 -0.1787 -0.0077 0.2486 1.00000 0.05 0.48 1.26 CL5 2.23 H17C 2.42 SN2 2.74 C1 Q9 1 0.1630 0.2824 0.2282 1.00000 0.05 0.47 1.32 SN1 1.41 N1 1.42 N2 1.56 C1 Q10 1 0.0837 0.2481 0.2866 1.00000 0.05 0.46 0.49 N1 0.92 C1 1.90 N2 2.08 SI1 Shortest distances between peaks (including symmetry equivalents) 7 9 1.00 4 7 1.20 9 10 1.29 7 10 1.68 4 10 1.71 4 9 1.72 2 8 2.18 6 10 2.64 4 8 2.77 Time profile in seconds ----------------------- 0.17: 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. 3.31: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.70: Structure factors and derivatives 4.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.50: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:28:41 Total CPU time: 12.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++