+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0245p21c started at 14:50:55 on 26-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0245p21c in P2(1)/c CELL 0.71073 24.2668 6.9038 23.7477 90.000 93.232 90.000 ZERR 8.00 0.0009 0.0002 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 128 168 32 56 8 8 V = 3972.20 F(000) = 1856.0 Mu = 0.30 mm-1 Cell Wt = 3559.26 Rho = 1.488 MERG 2 OMIT -3.00 55.00 OMIT 4 0 -8 OMIT 1 0 -24 OMIT 2 -1 11 BASF 0.50273 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.17 0.31 0.39 ACTA HTAB O91 Cl1 HTAB O92 Cl2 BOND $H WGHT 0.03040 14.98070 L.S. 8 TEMP -153.00 FVAR 0.24823 MOLE 1 C2 1 -0.042448 0.415141 0.232305 11.00000 0.02269 0.01932 = 0.01555 -0.00400 -0.00123 0.00165 AFIX 43 H2 2 -0.019267 0.385332 0.264720 11.00000 -1.20000 AFIX 0 C3 1 -0.097396 0.447267 0.238068 11.00000 0.02213 0.01852 = 0.01939 -0.00249 0.00510 -0.00302 C4 1 -0.130021 0.493773 0.189320 11.00000 0.01569 0.02879 = 0.01172 -0.00246 -0.00006 0.00191 AFIX 43 H4 2 -0.168217 0.520153 0.191905 11.00000 -1.20000 AFIX 0 C5 1 -0.106956 0.501336 0.137824 11.00000 0.01031 0.01723 = 0.02110 -0.00256 0.00232 0.00004 C6 1 -0.050154 0.463940 0.131908 11.00000 0.01499 0.01329 = 0.00883 -0.00097 0.00376 -0.00349 C7 1 0.038005 0.380671 0.173440 11.00000 0.01046 0.02842 = 0.01872 0.00182 -0.00069 0.00047 AFIX 23 H7A 2 0.045966 0.244059 0.183628 11.00000 -1.20000 H7B 2 0.062041 0.465007 0.197965 11.00000 -1.20000 AFIX 0 C8 1 -0.122466 0.432231 0.294130 11.00000 0.02854 0.03861 = 0.02096 -0.00756 0.00314 0.00101 AFIX 137 H8A 2 -0.093075 0.426778 0.324131 11.00000 -1.50000 H8B 2 -0.144922 0.314432 0.295134 11.00000 -1.50000 H8C 2 -0.145799 0.545649 0.299796 11.00000 -1.50000 AFIX 0 C9 1 0.071217 0.667793 0.073291 11.00000 0.01554 0.01576 = 0.02394 -0.00118 0.00188 -0.00176 AFIX 137 H9A 2 0.068790 0.672006 0.031977 11.00000 -1.50000 H9B 2 0.109141 0.696344 0.087183 11.00000 -1.50000 H9C 2 0.046144 0.764321 0.088006 11.00000 -1.50000 AFIX 0 C22 1 0.117687 0.052231 -0.010826 11.00000 0.01331 0.01661 = 0.02672 -0.00220 -0.00207 -0.00052 AFIX 43 H22 2 0.089350 0.011097 -0.037388 11.00000 -1.20000 AFIX 0 C23 1 0.171520 0.004228 -0.019533 11.00000 0.02019 0.01165 = 0.02303 0.00207 0.00201 -0.00159 C24 1 0.211236 0.064409 0.021603 11.00000 0.01840 0.01218 = 0.02638 0.00449 0.00256 -0.00022 AFIX 43 H24 2 0.248946 0.034606 0.017063 11.00000 -1.20000 AFIX 0 C25 1 0.197182 0.165390 0.068362 11.00000 0.01469 0.01394 = 0.02131 0.00355 -0.00727 -0.00513 C26 1 0.141658 0.222433 0.074794 11.00000 0.01644 0.01264 = 0.01787 0.00488 0.00093 -0.00481 C27 1 0.046723 0.226100 0.042353 11.00000 0.00778 0.02665 = 0.01506 0.00514 0.00072 0.00463 AFIX 23 H27A 2 0.023489 0.118428 0.055023 11.00000 -1.20000 H27B 2 0.030111 0.277018 0.006302 11.00000 -1.20000 AFIX 0 C28 1 0.187059 -0.102847 -0.071579 11.00000 0.02023 0.02358 = 0.04469 -0.01000 0.00586 0.00443 AFIX 137 H28A 2 0.153780 -0.128829 -0.095703 11.00000 -1.50000 H28B 2 0.204855 -0.225644 -0.060608 11.00000 -1.50000 H28C 2 0.212654 -0.023731 -0.092289 11.00000 -1.50000 AFIX 0 N1 3 -0.020380 0.425010 0.181183 11.00000 0.01680 0.01359 = 0.01841 -0.00189 0.00108 -0.00015 N5 3 -0.142775 0.552630 0.089126 11.00000 0.01183 0.01906 = 0.01886 -0.00164 0.00150 -0.00265 N21 3 0.103880 0.157170 0.034853 11.00000 0.00939 0.01124 = 0.02521 0.00388 -0.00016 -0.00281 N25 3 0.240034 0.221486 0.110359 11.00000 0.01257 0.02150 = 0.01978 0.00332 -0.00419 0.00078 O5A 4 -0.188135 0.624062 0.097130 11.00000 0.01207 0.04146 = 0.02847 0.00604 0.00104 0.00884 O5B 4 -0.126412 0.521676 0.041916 11.00000 0.01914 0.03648 = 0.01395 0.00516 0.00182 0.00059 O6 4 -0.024380 0.465335 0.086891 11.00000 0.01683 0.02036 = 0.00766 0.00123 -0.00026 0.00327 O25A 4 0.227275 0.250362 0.158693 11.00000 0.02124 0.04460 = 0.01821 -0.00209 0.00046 -0.00060 O25B 4 0.287364 0.234106 0.095236 11.00000 0.01199 0.03321 = 0.03212 0.00442 -0.00185 -0.00392 O26 4 0.124237 0.332848 0.112755 11.00000 0.01262 0.02058 = 0.02079 -0.00392 -0.00076 0.00038 SI1 5 0.051545 0.423799 0.097272 11.00000 0.01098 0.01715 = 0.01683 -0.00041 -0.00002 0.00046 CL1 6 0.045140 0.457455 0.357845 11.00000 0.02352 0.02346 = 0.02668 0.00186 -0.00232 0.00102 MOLE 2 C32 1 0.384729 0.953015 0.475088 11.00000 0.01954 0.01303 = 0.01733 0.00288 -0.00219 -0.00467 AFIX 43 H32 2 0.413294 0.987915 0.451276 11.00000 -1.20000 AFIX 0 C33 1 0.331509 1.013988 0.461454 11.00000 0.01631 0.01511 = 0.02074 -0.00105 0.00253 0.00159 C34 1 0.291917 0.965734 0.500093 11.00000 0.01499 0.01474 = 0.02175 -0.00314 -0.00371 -0.00072 AFIX 43 H34 2 0.255179 1.011550 0.493726 11.00000 -1.20000 AFIX 0 C35 1 0.304837 0.855175 0.546350 11.00000 0.00957 0.01029 = 0.02345 -0.00309 -0.00056 0.00177 C36 1 0.358904 0.783801 0.557111 11.00000 0.01638 0.01064 = 0.02068 -0.00649 0.00102 0.00061 C37 1 0.453619 0.770275 0.535143 11.00000 0.00873 0.01894 = 0.02047 0.00181 0.00000 -0.00184 AFIX 23 H37A 2 0.477747 0.875560 0.550502 11.00000 -1.20000 H37B 2 0.469652 0.718483 0.500802 11.00000 -1.20000 AFIX 0 C38 1 0.317187 1.121588 0.407934 11.00000 0.02506 0.01886 = 0.01992 0.00548 -0.00411 0.00024 AFIX 137 H38A 2 0.350794 1.144763 0.387917 11.00000 -1.50000 H38B 2 0.300162 1.245848 0.416769 11.00000 -1.50000 H38C 2 0.291222 1.044639 0.384059 11.00000 -1.50000 AFIX 0 C39 1 0.427508 0.326990 0.563574 11.00000 0.01850 0.02277 = 0.02069 -0.00340 0.00286 0.00079 AFIX 137 H39A 2 0.427082 0.324996 0.522289 11.00000 -1.50000 H39B 2 0.390592 0.296121 0.575728 11.00000 -1.50000 H39C 2 0.453966 0.230794 0.578964 11.00000 -1.50000 AFIX 0 C42 1 0.541203 0.576455 0.735645 11.00000 0.01911 0.02047 = 0.00843 -0.00409 0.00062 -0.00137 AFIX 43 H42 2 0.517763 0.607459 0.765070 11.00000 -1.20000 AFIX 0 C43 1 0.596736 0.543350 0.748852 11.00000 0.02120 0.02493 = 0.01602 0.00157 0.00232 -0.00413 C44 1 0.627923 0.494473 0.704091 11.00000 0.01618 0.01427 = 0.02347 0.00456 -0.00444 -0.00178 AFIX 43 H44 2 0.665915 0.465149 0.711301 11.00000 -1.20000 AFIX 0 C45 1 0.606169 0.486760 0.649901 11.00000 0.01757 0.01342 = 0.01395 -0.00024 0.00476 0.00088 C46 1 0.549712 0.525714 0.636520 11.00000 0.01996 0.00972 = 0.01214 0.00033 0.00346 0.00099 C47 1 0.460884 0.611376 0.667540 11.00000 0.01226 0.02476 = 0.01631 -0.00190 0.00392 0.00698 AFIX 23 H47A 2 0.452953 0.747695 0.677177 11.00000 -1.20000 H47B 2 0.436674 0.526284 0.688858 11.00000 -1.20000 AFIX 0 C48 1 0.620532 0.557159 0.808048 11.00000 0.02766 0.04626 = 0.01712 0.00264 -0.00570 -0.00642 AFIX 137 H48A 2 0.645565 0.668452 0.811470 11.00000 -1.50000 H48B 2 0.640993 0.438321 0.817810 11.00000 -1.50000 H48C 2 0.590666 0.573772 0.833735 11.00000 -1.50000 AFIX 0 N31 3 0.397190 0.845157 0.521358 11.00000 0.00842 0.01932 = 0.01101 0.00040 0.00287 0.00001 N35 3 0.261340 0.812729 0.584851 11.00000 0.01554 0.01703 = 0.02607 -0.00591 0.00203 0.00154 N41 3 0.519405 0.565888 0.682036 11.00000 0.01372 0.01340 = 0.00851 0.00049 0.00083 -0.00055 N45 3 0.641876 0.432952 0.604902 11.00000 0.01359 0.01455 = 0.02427 -0.00558 0.00347 -0.00773 O35A 4 0.214343 0.871340 0.571009 11.00000 0.01052 0.03209 = 0.03776 0.00430 0.00481 0.00560 O35B 4 0.272644 0.720853 0.627539 11.00000 0.01887 0.05267 = 0.03123 0.01619 0.00782 0.01044 O36 4 0.375667 0.665931 0.596232 11.00000 0.01349 0.02448 = 0.01682 0.00063 0.00097 0.00084 O45A 4 0.627533 0.468945 0.555604 11.00000 0.01986 0.03468 = 0.01136 -0.00354 -0.00030 -0.00217 O45B 4 0.686644 0.357805 0.619339 11.00000 0.01330 0.03705 = 0.03234 0.00038 0.00117 0.01113 O46 4 0.524156 0.526398 0.588265 11.00000 0.01137 0.01822 = 0.01438 -0.00082 0.00003 0.00134 SI2 5 0.448077 0.570872 0.589540 11.00000 0.01152 0.01686 = 0.01179 -0.00153 0.00005 0.00222 CL2 6 0.457720 0.963820 0.354193 11.00000 0.02235 0.02611 = 0.02128 0.00158 0.00310 -0.00239 MOLE 3 C91 1 0.190980 0.485432 0.280747 11.00000 0.05993 0.05839 = 0.03793 0.00496 0.00249 0.00471 AFIX 137 H91A 2 0.195284 0.612934 0.298595 11.00000 -1.50000 H91B 2 0.211166 0.482755 0.246157 11.00000 -1.50000 H91C 2 0.205712 0.385521 0.306763 11.00000 -1.50000 AFIX 0 O91 4 0.137065 0.451186 0.267997 11.00000 0.04598 0.10644 = 0.03784 0.00349 -0.00054 -0.01645 AFIX 147 H91 2 0.118552 0.484915 0.295184 11.00000 -1.50000 AFIX 0 MOLE 4 C92 1 0.312176 0.991744 0.258488 11.00000 0.05845 0.05460 = 0.04532 0.00259 -0.00588 0.00036 AFIX 137 H92A 2 0.297059 0.892682 0.282831 11.00000 -1.50000 H92B 2 0.293043 0.986115 0.221063 11.00000 -1.50000 H92C 2 0.306936 1.120055 0.275007 11.00000 -1.50000 AFIX 0 O92 4 0.366288 0.959376 0.253776 11.00000 0.04803 0.14545 = 0.03283 0.01861 0.00146 0.01373 AFIX 147 H92 2 0.382874 0.968578 0.285678 11.00000 -1.50000 AFIX 0 HKLF 5 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 2009src0245p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C2 - N1 C3 C3 - C2 C4 C8 C4 - C5 C3 C5 - C4 C6 N5 C6 - O6 N1 C5 C7 - N1 Si1 C8 - C3 C9 - Si1 C22 - N21 C23 C23 - C22 C24 C28 C24 - C25 C23 C25 - C24 C26 N25 C26 - O26 N21 C25 C27 - N21 Si1 C28 - C23 N1 - C2 C6 C7 N5 - O5B O5A C5 N21 - C26 C22 C27 N25 - O25A O25B C25 O5A - N5 O5B - N5 O6 - C6 Si1 O25A - N25 O25B - N25 O26 - C26 Si1 Si1 - C9 O6 C7 C27 O26 Cl1 - no bonds found C32 - N31 C33 C33 - C32 C34 C38 C34 - C35 C33 C35 - C34 C36 N35 C36 - O36 N31 C35 C37 - N31 Si2 C38 - C33 C39 - Si2 C42 - N41 C43 C43 - C44 C42 C48 C44 - C45 C43 C45 - C44 C46 N45 C46 - O46 N41 C45 C47 - N41 Si2 C48 - C43 N31 - C32 C36 C37 N35 - O35B O35A C35 N41 - C42 C46 C47 N45 - O45A O45B C45 O35A - N35 O35B - N35 O36 - C36 Si2 O45A - N45 O45B - N45 O46 - C46 Si2 Si2 - C39 O46 C47 O36 C37 Cl2 - no bonds found C91 - O91 O91 - C91 C92 - O92 O92 - C92 ** MERG code changed to 0 for compatibility with HKLF and BASF parameters ** h k l Fo^2 Sigma Why rejected 22 0 -1 19.15 3.85 observed but should be systematically absent 9162 Reflections read, of which 805 rejected 0 =< h =< 31, -8 =< k =< 0, -30 =< l =< 30, Max. 2-theta = 54.97 1 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0696 Maximum memory for data reduction = 4793 / 119 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 = 6266 / 714700 wR2 = 0.1557 before cycle 1 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.007 OSF 2 0.50273 0.00144 0.002 BASF 1 Mean shift/su = 0.001 Maximum = 0.007 for OSF Max. shift = 0.000 A for H48B Max. dU = 0.000 for N45 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 2 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.002 for U23 Cl2 Max. shift = 0.000 A for H38C Max. dU = 0.000 for N45 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 3 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for H92 Max. dU = 0.000 for C92 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 4 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H91 Max. dU = 0.000 for C91 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 5 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H91 Max. dU = 0.000 for O91 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 6 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for x N45 Max. shift = 0.000 A for H91 Max. dU = 0.000 for C48 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 7 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H92 Max. dU = 0.000 for C48 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6266 / 714700 wR2 = 0.1557 before cycle 8 for 8358 data and 534 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24823 0.00045 0.000 OSF 2 0.50273 0.00144 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for U33 Cl2 Max. shift = 0.000 A for H91 Max. dU = 0.000 for O45A Largest correlation matrix elements -0.513 U33 Cl2 / U33 Cl1 -0.508 U33 C42 / U33 C2 -0.504 U33 Si2 / U33 Si1 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.0193 0.3853 0.2647 43 0.950 0.000 C2 N1 C3 H4 -0.1682 0.5202 0.1919 43 0.950 0.000 C4 C5 C3 H7A 0.0460 0.2441 0.1836 23 0.990 0.000 C7 N1 Si1 H7B 0.0620 0.4650 0.1980 23 0.990 0.000 C7 N1 Si1 H8A -0.0931 0.4268 0.3241 137 0.980 0.000 C8 C3 H8A H8B -0.1449 0.3144 0.2951 137 0.980 0.000 C8 C3 H8A H8C -0.1458 0.5456 0.2998 137 0.980 0.000 C8 C3 H8A H9A 0.0688 0.6720 0.0320 137 0.980 0.000 C9 Si1 H9A H9B 0.1091 0.6963 0.0872 137 0.980 0.000 C9 Si1 H9A H9C 0.0461 0.7643 0.0880 137 0.980 0.000 C9 Si1 H9A H22 0.0894 0.0111 -0.0374 43 0.950 0.000 C22 N21 C23 H24 0.2489 0.0346 0.0171 43 0.950 0.000 C24 C25 C23 H27A 0.0235 0.1184 0.0550 23 0.990 0.000 C27 N21 Si1 H27B 0.0301 0.2770 0.0063 23 0.990 0.000 C27 N21 Si1 H28A 0.1538 -0.1288 -0.0957 137 0.980 0.000 C28 C23 H28A H28B 0.2049 -0.2256 -0.0606 137 0.980 0.000 C28 C23 H28A H28C 0.2127 -0.0237 -0.0923 137 0.980 0.000 C28 C23 H28A H32 0.4133 0.9879 0.4513 43 0.950 0.000 C32 N31 C33 H34 0.2552 1.0115 0.4937 43 0.950 0.000 C34 C35 C33 H37A 0.4777 0.8756 0.5505 23 0.990 0.000 C37 N31 Si2 H37B 0.4697 0.7185 0.5008 23 0.990 0.000 C37 N31 Si2 H38A 0.3508 1.1448 0.3879 137 0.980 0.000 C38 C33 H38A H38B 0.3002 1.2458 0.4168 137 0.980 0.000 C38 C33 H38A H38C 0.2912 1.0446 0.3841 137 0.980 0.000 C38 C33 H38A H39A 0.4271 0.3250 0.5223 137 0.980 0.000 C39 Si2 H39A H39B 0.3906 0.2961 0.5757 137 0.980 0.000 C39 Si2 H39A H39C 0.4540 0.2308 0.5790 137 0.980 0.000 C39 Si2 H39A H42 0.5178 0.6075 0.7651 43 0.950 0.000 C42 N41 C43 H44 0.6659 0.4651 0.7113 43 0.950 0.000 C44 C45 C43 H47A 0.4530 0.7477 0.6772 23 0.990 0.000 C47 N41 Si2 H47B 0.4367 0.5263 0.6889 23 0.990 0.000 C47 N41 Si2 H48A 0.6456 0.6685 0.8115 137 0.980 0.000 C48 C43 H48A H48B 0.6410 0.4383 0.8178 137 0.980 0.000 C48 C43 H48A H48C 0.5907 0.5738 0.8337 137 0.980 0.000 C48 C43 H48A H91A 0.1953 0.6129 0.2986 137 0.980 0.000 C91 O91 H91A H91B 0.2112 0.4828 0.2462 137 0.980 0.000 C91 O91 H91A H91C 0.2057 0.3855 0.3068 137 0.980 0.000 C91 O91 H91A H91 0.1186 0.4849 0.2952 147 0.840 0.000 O91 C91 H91 H92A 0.2971 0.8927 0.2828 137 0.980 0.000 C92 O92 H92A H92B 0.2930 0.9861 0.2211 137 0.980 0.000 C92 O92 H92A H92C 0.3069 1.1201 0.2750 137 0.980 0.000 C92 O92 H92A H92 0.3829 0.9686 0.2857 147 0.840 0.000 O92 C92 H92 2009src0245p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.04245 0.41514 0.23231 1.00000 0.02269 0.01932 0.01555 -0.00400 -0.00123 0.00165 0.01927 0.00977 0.00023 0.00083 0.00024 0.00000 0.00305 0.00307 0.00335 0.00239 0.00243 0.00248 0.00132 H2 -0.01927 0.38533 0.26472 1.00000 0.02313 0.00000 0.00000 C3 -0.09740 0.44727 0.23807 1.00000 0.02213 0.01852 0.01939 -0.00249 0.00510 -0.00302 0.01987 0.01006 0.00024 0.00083 0.00025 0.00000 0.00300 0.00296 0.00322 0.00245 0.00245 0.00253 0.00127 C4 -0.13002 0.49377 0.18932 1.00000 0.01569 0.02879 0.01172 -0.00246 -0.00006 0.00191 0.01876 0.00985 0.00023 0.00083 0.00024 0.00000 0.00268 0.00333 0.00289 0.00251 0.00231 0.00248 0.00126 H4 -0.16822 0.52015 0.19190 1.00000 0.02252 0.00000 0.00000 C5 -0.10696 0.50134 0.13782 1.00000 0.01031 0.01723 0.02110 -0.00256 0.00232 0.00004 0.01616 0.00945 0.00021 0.00078 0.00024 0.00000 0.00248 0.00280 0.00316 0.00238 0.00226 0.00225 0.00119 C6 -0.05015 0.46394 0.13191 1.00000 0.01499 0.01329 0.00883 -0.00097 0.00376 -0.00349 0.01226 0.00903 0.00022 0.00074 0.00022 0.00000 0.00253 0.00275 0.00276 0.00216 0.00208 0.00217 0.00112 C7 0.03801 0.38067 0.17344 1.00000 0.01046 0.02842 0.01872 0.00182 -0.00069 0.00047 0.01926 0.00990 0.00020 0.00088 0.00023 0.00000 0.00254 0.00330 0.00319 0.00256 0.00227 0.00235 0.00126 H7A 0.04597 0.24406 0.18363 1.00000 0.02311 0.00000 0.00000 H7B 0.06204 0.46501 0.19796 1.00000 0.02311 0.00000 0.00000 C8 -0.12247 0.43223 0.29413 1.00000 0.02854 0.03861 0.02096 -0.00756 0.00314 0.00101 0.02930 0.01134 0.00025 0.00098 0.00026 0.00000 0.00344 0.00381 0.00328 0.00302 0.00276 0.00298 0.00150 H8A -0.09307 0.42678 0.32413 1.00000 0.04395 0.00000 0.00000 H8B -0.14492 0.31443 0.29513 1.00000 0.04395 0.00000 0.00000 H8C -0.14580 0.54565 0.29980 1.00000 0.04395 0.00000 0.00000 C9 0.07122 0.66779 0.07329 1.00000 0.01554 0.01576 0.02394 -0.00118 0.00188 -0.00176 0.01838 0.00949 0.00022 0.00075 0.00024 0.00000 0.00262 0.00271 0.00329 0.00244 0.00232 0.00215 0.00121 H9A 0.06879 0.67201 0.03198 1.00000 0.02758 0.00000 0.00000 H9B 0.10914 0.69634 0.08718 1.00000 0.02758 0.00000 0.00000 H9C 0.04614 0.76432 0.08801 1.00000 0.02758 0.00000 0.00000 C22 0.11769 0.05223 -0.01083 1.00000 0.01331 0.01661 0.02672 -0.00220 -0.00207 -0.00052 0.01900 0.00988 0.00022 0.00079 0.00025 0.00000 0.00266 0.00292 0.00333 0.00264 0.00227 0.00229 0.00125 H22 0.08935 0.01110 -0.03739 1.00000 0.02280 0.00000 0.00000 C23 0.17152 0.00423 -0.01953 1.00000 0.02019 0.01165 0.02303 0.00207 0.00201 -0.00159 0.01826 0.00975 0.00023 0.00077 0.00024 0.00000 0.00282 0.00270 0.00322 0.00231 0.00234 0.00228 0.00122 C24 0.21124 0.06441 0.02160 1.00000 0.01840 0.01218 0.02638 0.00449 0.00256 -0.00022 0.01894 0.00990 0.00023 0.00077 0.00024 0.00000 0.00266 0.00266 0.00321 0.00241 0.00235 0.00226 0.00120 H24 0.24895 0.03461 0.01706 1.00000 0.02272 0.00000 0.00000 C25 0.19718 0.16539 0.06836 1.00000 0.01469 0.01394 0.02131 0.00355 -0.00727 -0.00513 0.01696 0.00902 0.00021 0.00076 0.00023 0.00000 0.00264 0.00267 0.00306 0.00236 0.00223 0.00210 0.00120 C26 0.14166 0.22243 0.07479 1.00000 0.01644 0.01264 0.01787 0.00488 0.00093 -0.00481 0.01565 0.00914 0.00021 0.00075 0.00023 0.00000 0.00259 0.00262 0.00302 0.00237 0.00223 0.00218 0.00114 C27 0.04672 0.22610 0.04235 1.00000 0.00778 0.02665 0.01506 0.00514 0.00072 0.00463 0.01649 0.00954 0.00020 0.00084 0.00022 0.00000 0.00234 0.00310 0.00285 0.00245 0.00201 0.00231 0.00119 H27A 0.02349 0.11843 0.05502 1.00000 0.01979 0.00000 0.00000 H27B 0.03011 0.27702 0.00630 1.00000 0.01979 0.00000 0.00000 C28 0.18706 -0.10285 -0.07158 1.00000 0.02023 0.02358 0.04469 -0.01000 0.00586 0.00443 0.02935 0.01092 0.00024 0.00088 0.00028 0.00000 0.00293 0.00333 0.00407 0.00297 0.00283 0.00264 0.00148 H28A 0.15378 -0.12883 -0.09570 1.00000 0.04402 0.00000 0.00000 H28B 0.20485 -0.22564 -0.06061 1.00000 0.04402 0.00000 0.00000 H28C 0.21265 -0.02373 -0.09229 1.00000 0.04402 0.00000 0.00000 N1 -0.02038 0.42501 0.18118 1.00000 0.01680 0.01359 0.01841 -0.00189 0.00108 -0.00015 0.01626 0.00775 0.00018 0.00064 0.00019 0.00000 0.00235 0.00235 0.00277 0.00200 0.00192 0.00193 0.00105 N5 -0.14278 0.55263 0.08913 1.00000 0.01183 0.01905 0.01886 -0.00164 0.00150 -0.00265 0.01656 0.00795 0.00018 0.00066 0.00020 0.00000 0.00234 0.00247 0.00269 0.00208 0.00188 0.00191 0.00105 N21 0.10388 0.15717 0.03485 1.00000 0.00939 0.01124 0.02521 0.00388 -0.00016 -0.00281 0.01532 0.00767 0.00017 0.00062 0.00020 0.00000 0.00213 0.00227 0.00267 0.00197 0.00191 0.00178 0.00099 N25 0.24003 0.22149 0.11036 1.00000 0.01257 0.02150 0.01978 0.00332 -0.00419 0.00078 0.01814 0.00801 0.00018 0.00067 0.00020 0.00000 0.00219 0.00247 0.00263 0.00210 0.00190 0.00197 0.00102 O5A -0.18813 0.62406 0.09713 1.00000 0.01207 0.04146 0.02847 0.00604 0.00104 0.00883 0.02734 0.00735 0.00015 0.00063 0.00017 0.00000 0.00190 0.00257 0.00250 0.00200 0.00166 0.00184 0.00100 O5B -0.12641 0.52168 0.04192 1.00000 0.01914 0.03648 0.01395 0.00516 0.00182 0.00059 0.02316 0.00725 0.00016 0.00061 0.00017 0.00000 0.00203 0.00247 0.00221 0.00187 0.00170 0.00187 0.00094 O6 -0.02438 0.46533 0.08689 1.00000 0.01683 0.02036 0.00766 0.00123 -0.00026 0.00327 0.01499 0.00633 0.00014 0.00053 0.00015 0.00000 0.00189 0.00208 0.00194 0.00159 0.00150 0.00161 0.00082 O25A 0.22727 0.25036 0.15869 1.00000 0.02124 0.04460 0.01821 -0.00209 0.00046 -0.00060 0.02804 0.00729 0.00016 0.00068 0.00017 0.00000 0.00204 0.00253 0.00219 0.00204 0.00165 0.00200 0.00096 O25B 0.28736 0.23411 0.09524 1.00000 0.01199 0.03321 0.03212 0.00442 -0.00185 -0.00392 0.02589 0.00670 0.00014 0.00060 0.00017 0.00000 0.00180 0.00229 0.00235 0.00195 0.00162 0.00174 0.00091 O26 0.12424 0.33285 0.11275 1.00000 0.01262 0.02058 0.02079 -0.00392 -0.00076 0.00038 0.01806 0.00629 0.00014 0.00054 0.00016 0.00000 0.00185 0.00200 0.00223 0.00174 0.00154 0.00155 0.00086 Si1 0.05155 0.42380 0.09727 1.00000 0.01098 0.01715 0.01683 -0.00041 -0.00002 0.00046 0.01502 0.00264 0.00006 0.00022 0.00006 0.00000 0.00073 0.00080 0.00092 0.00065 0.00059 0.00060 0.00036 Cl1 0.04514 0.45745 0.35784 1.00000 0.02352 0.02346 0.02668 0.00186 -0.00232 0.00102 0.02470 0.00257 0.00006 0.00021 0.00006 0.00000 0.00076 0.00084 0.00090 0.00064 0.00059 0.00060 0.00037 C32 0.38473 0.95302 0.47509 1.00000 0.01954 0.01303 0.01733 0.00288 -0.00219 -0.00467 0.01676 0.00906 0.00023 0.00076 0.00023 0.00000 0.00277 0.00273 0.00300 0.00237 0.00225 0.00227 0.00118 H32 0.41329 0.98792 0.45128 1.00000 0.02011 0.00000 0.00000 C33 0.33151 1.01399 0.46145 1.00000 0.01631 0.01511 0.02074 -0.00105 0.00253 0.00159 0.01733 0.00949 0.00022 0.00077 0.00023 0.00000 0.00262 0.00273 0.00307 0.00236 0.00230 0.00225 0.00118 C34 0.29192 0.96573 0.50009 1.00000 0.01499 0.01474 0.02174 -0.00314 -0.00371 -0.00072 0.01733 0.00910 0.00022 0.00076 0.00023 0.00000 0.00262 0.00279 0.00321 0.00237 0.00216 0.00221 0.00121 H34 0.25518 1.01155 0.49373 1.00000 0.02080 0.00000 0.00000 C35 0.30484 0.85518 0.54635 1.00000 0.00957 0.01029 0.02345 -0.00309 -0.00056 0.00177 0.01449 0.00900 0.00020 0.00074 0.00024 0.00000 0.00240 0.00249 0.00312 0.00230 0.00219 0.00205 0.00113 C36 0.35890 0.78380 0.55711 1.00000 0.01638 0.01064 0.02068 -0.00649 0.00102 0.00061 0.01590 0.00902 0.00021 0.00075 0.00023 0.00000 0.00261 0.00263 0.00312 0.00233 0.00224 0.00217 0.00116 C37 0.45362 0.77027 0.53514 1.00000 0.00873 0.01894 0.02047 0.00181 0.00000 -0.00184 0.01608 0.00929 0.00019 0.00080 0.00023 0.00000 0.00245 0.00286 0.00306 0.00245 0.00208 0.00218 0.00118 H37A 0.47775 0.87556 0.55050 1.00000 0.01930 0.00000 0.00000 H37B 0.46965 0.71848 0.50080 1.00000 0.01930 0.00000 0.00000 C38 0.31719 1.12159 0.40793 1.00000 0.02506 0.01886 0.01992 0.00548 -0.00411 0.00024 0.02148 0.00995 0.00023 0.00081 0.00023 0.00000 0.00300 0.00292 0.00310 0.00247 0.00238 0.00242 0.00126 H38A 0.35079 1.14476 0.38792 1.00000 0.03222 0.00000 0.00000 H38B 0.30016 1.24585 0.41677 1.00000 0.03222 0.00000 0.00000 H38C 0.29122 1.04464 0.38406 1.00000 0.03222 0.00000 0.00000 C39 0.42751 0.32699 0.56357 1.00000 0.01850 0.02277 0.02069 -0.00340 0.00286 0.00079 0.02059 0.00949 0.00022 0.00078 0.00024 0.00000 0.00284 0.00307 0.00323 0.00251 0.00230 0.00233 0.00127 H39A 0.42708 0.32500 0.52229 1.00000 0.03089 0.00000 0.00000 H39B 0.39059 0.29612 0.57573 1.00000 0.03089 0.00000 0.00000 H39C 0.45397 0.23079 0.57896 1.00000 0.03089 0.00000 0.00000 C42 0.54120 0.57646 0.73564 1.00000 0.01911 0.02047 0.00843 -0.00409 0.00062 -0.00137 0.01601 0.00913 0.00021 0.00081 0.00022 0.00000 0.00287 0.00307 0.00294 0.00231 0.00213 0.00241 0.00124 H42 0.51776 0.60746 0.76507 1.00000 0.01921 0.00000 0.00000 C43 0.59674 0.54335 0.74885 1.00000 0.02120 0.02493 0.01602 0.00157 0.00232 -0.00413 0.02067 0.01002 0.00023 0.00085 0.00024 0.00000 0.00296 0.00323 0.00312 0.00252 0.00247 0.00251 0.00130 C44 0.62792 0.49447 0.70409 1.00000 0.01618 0.01427 0.02347 0.00456 -0.00444 -0.00178 0.01818 0.00983 0.00023 0.00077 0.00026 0.00000 0.00267 0.00281 0.00328 0.00253 0.00242 0.00227 0.00125 H44 0.66592 0.46515 0.71130 1.00000 0.02182 0.00000 0.00000 C45 0.60617 0.48676 0.64990 1.00000 0.01757 0.01342 0.01395 -0.00024 0.00476 0.00088 0.01483 0.00975 0.00022 0.00077 0.00023 0.00000 0.00264 0.00268 0.00282 0.00223 0.00222 0.00229 0.00115 C46 0.54971 0.52571 0.63652 1.00000 0.01996 0.00972 0.01214 0.00033 0.00346 0.00099 0.01384 0.00951 0.00022 0.00074 0.00023 0.00000 0.00283 0.00266 0.00285 0.00220 0.00219 0.00220 0.00116 C47 0.46088 0.61138 0.66754 1.00000 0.01226 0.02476 0.01631 -0.00190 0.00392 0.00698 0.01766 0.00971 0.00021 0.00085 0.00023 0.00000 0.00254 0.00308 0.00305 0.00245 0.00226 0.00234 0.00122 H47A 0.45295 0.74770 0.67718 1.00000 0.02119 0.00000 0.00000 H47B 0.43667 0.52628 0.68886 1.00000 0.02119 0.00000 0.00000 C48 0.62053 0.55716 0.80805 1.00000 0.02766 0.04626 0.01712 0.00264 -0.00570 -0.00642 0.03061 0.01084 0.00026 0.00102 0.00026 0.00000 0.00328 0.00409 0.00317 0.00310 0.00267 0.00314 0.00154 H48A 0.64557 0.66845 0.81147 1.00000 0.04591 0.00000 0.00000 H48B 0.64099 0.43832 0.81781 1.00000 0.04591 0.00000 0.00000 H48C 0.59067 0.57377 0.83373 1.00000 0.04591 0.00000 0.00000 N31 0.39719 0.84516 0.52136 1.00000 0.00842 0.01932 0.01101 0.00040 0.00287 0.00001 0.01283 0.00748 0.00017 0.00064 0.00018 0.00000 0.00201 0.00236 0.00232 0.00193 0.00170 0.00181 0.00093 N35 0.26134 0.81273 0.58485 1.00000 0.01554 0.01703 0.02607 -0.00591 0.00203 0.00154 0.01951 0.00788 0.00018 0.00064 0.00021 0.00000 0.00236 0.00237 0.00280 0.00212 0.00204 0.00193 0.00105 N41 0.51940 0.56589 0.68204 1.00000 0.01372 0.01340 0.00851 0.00049 0.00083 -0.00055 0.01187 0.00736 0.00017 0.00061 0.00017 0.00000 0.00218 0.00225 0.00234 0.00188 0.00173 0.00180 0.00095 N45 0.64188 0.43295 0.60490 1.00000 0.01359 0.01455 0.02426 -0.00558 0.00347 -0.00773 0.01737 0.00783 0.00018 0.00064 0.00021 0.00000 0.00232 0.00233 0.00279 0.00214 0.00195 0.00191 0.00104 O35A 0.21434 0.87134 0.57101 1.00000 0.01052 0.03209 0.03776 0.00430 0.00481 0.00560 0.02666 0.00709 0.00015 0.00058 0.00017 0.00000 0.00178 0.00229 0.00249 0.00197 0.00169 0.00176 0.00094 O35B 0.27264 0.72085 0.62754 1.00000 0.01887 0.05267 0.03123 0.01619 0.00782 0.01044 0.03401 0.00829 0.00016 0.00070 0.00018 0.00000 0.00210 0.00298 0.00264 0.00235 0.00188 0.00213 0.00113 O36 0.37567 0.66593 0.59623 1.00000 0.01349 0.02448 0.01682 0.00063 0.00097 0.00084 0.01826 0.00640 0.00014 0.00054 0.00016 0.00000 0.00185 0.00208 0.00213 0.00177 0.00155 0.00162 0.00085 O45A 0.62753 0.46895 0.55560 1.00000 0.01986 0.03468 0.01136 -0.00354 -0.00030 -0.00217 0.02201 0.00688 0.00016 0.00061 0.00017 0.00000 0.00210 0.00245 0.00212 0.00187 0.00168 0.00184 0.00095 O45B 0.68664 0.35780 0.61934 1.00000 0.01330 0.03705 0.03234 0.00038 0.00117 0.01113 0.02757 0.00722 0.00015 0.00061 0.00018 0.00000 0.00197 0.00245 0.00260 0.00204 0.00174 0.00179 0.00100 O46 0.52416 0.52640 0.58827 1.00000 0.01137 0.01822 0.01438 -0.00082 0.00003 0.00134 0.01468 0.00619 0.00014 0.00052 0.00015 0.00000 0.00179 0.00200 0.00208 0.00165 0.00149 0.00155 0.00082 Si2 0.44808 0.57087 0.58954 1.00000 0.01152 0.01686 0.01179 -0.00153 0.00005 0.00222 0.01341 0.00259 0.00006 0.00022 0.00006 0.00000 0.00074 0.00079 0.00082 0.00063 0.00055 0.00059 0.00035 Cl2 0.45772 0.96382 0.35419 1.00000 0.02235 0.02611 0.02128 0.00158 0.00310 -0.00239 0.02318 0.00253 0.00006 0.00022 0.00006 0.00000 0.00075 0.00085 0.00084 0.00062 0.00056 0.00060 0.00036 C91 0.19098 0.48543 0.28075 1.00000 0.05993 0.05839 0.03793 0.00496 0.00249 0.00471 0.05209 0.01441 0.00033 0.00126 0.00032 0.00000 0.00518 0.00547 0.00468 0.00388 0.00385 0.00444 0.00213 H91A 0.19528 0.61293 0.29859 1.00000 0.07814 0.00000 0.00000 H91B 0.21117 0.48275 0.24616 1.00000 0.07814 0.00000 0.00000 H91C 0.20571 0.38552 0.30676 1.00000 0.07814 0.00000 0.00000 O91 0.13707 0.45119 0.26800 1.00000 0.04598 0.10644 0.03784 0.00349 -0.00054 -0.01645 0.06353 0.01014 0.00023 0.00107 0.00023 0.00000 0.00323 0.00523 0.00350 0.00345 0.00253 0.00357 0.00175 H91 0.11855 0.48492 0.29518 1.00000 0.09529 0.00000 0.00000 C92 0.31218 0.99174 0.25849 1.00000 0.05845 0.05460 0.04532 0.00259 -0.00588 0.00036 0.05312 0.01420 0.00033 0.00123 0.00034 0.00000 0.00536 0.00522 0.00536 0.00405 0.00400 0.00435 0.00218 H92A 0.29706 0.89268 0.28283 1.00000 0.07969 0.00000 0.00000 H92B 0.29304 0.98611 0.22106 1.00000 0.07969 0.00000 0.00000 H92C 0.30694 1.12006 0.27501 1.00000 0.07969 0.00000 0.00000 O92 0.36629 0.95938 0.25378 1.00000 0.04803 0.14545 0.03283 0.01861 0.00146 0.01373 0.07547 0.01240 0.00024 0.00121 0.00023 0.00000 0.00340 0.00649 0.00337 0.00410 0.00259 0.00398 0.00210 H92 0.38287 0.96858 0.28568 1.00000 0.11320 0.00000 0.00000 Final Structure Factor Calculation for 2009src0245p21c in P2(1)/c Total number of l.s. parameters = 534 Maximum vector length = 511 Memory required = 5732 / 25039 wR2 = 0.1557 before cycle 9 for 8358 data and 0 / 534 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 14.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0702 for 5961 Fo > 4sig(Fo) and 0.1152 for all 8358 data wR2 = 0.1557, GooF = S = 1.086, Restrained GooF = 1.086 for all data Occupancy sum of asymmetric unit = 58.00 for non-hydrogen and 42.00 for hydrogen atoms Principal mean square atomic displacements U 0.0252 0.0197 0.0129 C2 0.0265 0.0168 0.0163 C3 0.0295 0.0155 0.0113 C4 0.0224 0.0160 0.0100 C5 0.0185 0.0109 0.0073 C6 0.0288 0.0188 0.0102 C7 0.0414 0.0288 0.0176 C8 0.0242 0.0171 0.0139 C9 0.0280 0.0165 0.0125 C22 0.0234 0.0204 0.0109 C23 0.0278 0.0182 0.0108 C24 0.0297 0.0129 0.0082 C25 0.0224 0.0171 0.0075 C26 0.0294 0.0135 0.0066 C27 0.0487 0.0255 0.0138 C28 0.0191 0.0168 0.0129 N1 0.0211 0.0176 0.0109 N5 0.0265 0.0123 0.0071 N21 0.0249 0.0197 0.0098 N25 0.0456 0.0268 0.0095 O5A 0.0376 0.0192 0.0127 O5B 0.0223 0.0152 0.0074 O6 0.0448 0.0214 0.0179 O25A 0.0383 0.0282 0.0111 O25B 0.0249 0.0170 0.0124 O26 0.0176 0.0166 0.0109 Si1 0.0296 0.0243 0.0202 Cl1 0.0247 0.0152 0.0103 C32 0.0212 0.0173 0.0135 C33 0.0251 0.0155 0.0114 C34 0.0245 0.0110 0.0080 C35 0.0239 0.0164 0.0074 C36 0.0220 0.0178 0.0084 C37 0.0297 0.0219 0.0128 C38 0.0253 0.0202 0.0163 C39 0.0222 0.0187 0.0072 C42 0.0277 0.0195 0.0148 C43 0.0285 0.0137 0.0123 C44 0.0199 0.0136 0.0111 C45 0.0207 0.0112 0.0096 C46 0.0279 0.0177 0.0074 C47 0.0491 0.0287 0.0140 C48 0.0193 0.0122 0.0069 N31 0.0290 0.0168 0.0127 N35 0.0141 0.0130 0.0084 N41 0.0287 0.0173 0.0062 N45 0.0409 0.0303 0.0088 O35A 0.0641 0.0226 0.0153 O35B 0.0246 0.0168 0.0134 O36 0.0354 0.0199 0.0107 O45A 0.0415 0.0324 0.0089 O45B 0.0187 0.0143 0.0111 O46 0.0182 0.0114 0.0107 Si2 0.0274 0.0235 0.0187 Cl2 0.0642 0.0553 0.0368 C91 0.1110 0.0426 0.0370 O91 0.0635 0.0549 0.0409 C92 0.1500 0.0469 0.0295 O92 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.022 0.029 0.038 0.047 0.059 0.073 0.091 0.123 1.000 Number in group 861. 851. 796. 877. 826. 876. 815. 796. 829. 831. GooF 1.261 1.138 1.132 1.034 1.070 1.078 1.062 0.971 0.977 1.096 K 3.346 1.415 1.153 1.001 0.951 0.952 0.996 1.011 1.012 1.006 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.07 1.18 1.35 1.69 inf Number in group 863. 815. 845. 836. 825. 830. 840. 834. 833. 837. GooF 1.239 1.089 1.048 1.060 1.076 1.087 0.993 0.997 1.059 1.178 K 1.058 1.024 1.022 0.997 1.011 1.006 1.015 1.010 1.000 1.007 R1 0.285 0.238 0.182 0.158 0.137 0.097 0.070 0.056 0.052 0.041 Recommended weighting scheme: WGHT 0.0304 14.9807 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) 4 0 -30 1986.05 30.34 8.42 0.014 0.79 4 0 -30 1986.05 30.34 8.42 0.014 0.79 1 0 -20 973.55 81.62 7.83 0.023 1.19 10 -1 11 563.78 83.43 6.66 0.023 1.53 9 -2 -15 1649.95 609.37 6.55 0.062 1.30 3 -1 -16 5441.91 3368.12 6.50 0.146 1.44 0 0 24 1779.62 3608.66 6.47 0.151 0.99 28 -3 8 1450.83 449.03 5.72 0.053 0.77 4 0 24 754.46 57.17 5.67 0.019 0.97 13 -1 13 362.06 48.38 5.41 0.017 1.25 5 -5 13 3916.75 2465.63 5.38 0.125 1.07 8 0 2 3377.97 2182.19 5.11 0.117 2.90 6 -6 -6 610.52 175.38 5.07 0.033 1.07 10 0 -6 2525.48 1522.43 5.01 0.098 2.12 1 -2 -20 323.92 0.65 4.85 0.002 1.12 2 -1 -12 327.98 32.22 4.78 0.014 1.89 9 -2 2 18270.22 14798.09 4.75 0.305 2.07 13 -1 -13 6075.96 4409.83 4.51 0.167 1.32 4 -1 -8 647.19 277.18 4.36 0.042 2.53 13 0 -22 596.88 63.70 4.29 0.020 0.96 18 -2 -21 -76.60 777.48 4.26 0.070 0.86 0 0 16 4517.37 3250.91 4.23 0.143 1.48 5 -2 -7 263.06 29.89 4.17 0.014 2.20 14 -4 23 1006.17 56.82 4.17 0.019 0.77 7 -8 3 1658.88 803.45 4.06 0.071 0.83 2 -2 -11 1221.84 664.14 4.05 0.065 1.82 8 -4 -15 272.48 21.36 3.98 0.012 1.10 4 -3 -11 143.95 6.35 3.91 0.006 1.54 5 0 -16 5395.49 4076.75 3.90 0.160 1.44 3 -1 -24 414.31 11.23 3.86 0.008 0.98 0 -3 12 286.76 67.40 3.80 0.021 1.50 13 -3 12 485.39 105.50 3.78 0.026 1.14 5 0 -30 1986.05 1019.00 3.76 0.080 0.79 5 0 -30 1986.05 1019.00 3.76 0.080 0.79 8 -5 -4 -37.00 139.29 3.75 0.030 1.23 4 -1 -14 2473.39 1703.09 3.74 0.104 1.61 14 -4 11 1190.36 603.39 3.67 0.062 1.05 20 -3 5 -3.08 401.08 3.67 0.050 1.03 22 -6 -9 419.67 1095.28 3.66 0.083 0.77 2 0 12 2526.29 1772.00 3.64 0.106 1.93 6 -1 -11 957.97 554.38 3.61 0.059 1.87 4 0 0 10238.08 12277.14 3.55 0.278 6.06 12 -1 -15 195.55 4.81 3.55 0.006 1.26 20 -2 11 655.63 1286.35 3.50 0.090 0.99 10 -3 -15 1342.75 770.97 3.50 0.070 1.17 9 0 -6 1258.20 777.84 3.47 0.070 2.29 4 0 -2 326.68 126.32 3.43 0.028 5.52 4 -3 11 695.39 330.58 3.39 0.046 1.51 14 -8 -3 441.74 3.13 3.34 0.004 0.77 13 -4 -14 736.45 288.60 3.30 0.043 1.03 Bond lengths and angles C2 - Distance Angles N1 1.3559 (0.0068) C3 1.3662 (0.0077) 121.23 (0.54) H2 0.9500 119.38 119.38 C2 - N1 C3 C3 - Distance Angles C2 1.3662 (0.0077) C4 1.4024 (0.0078) 117.60 (0.53) C8 1.4982 (0.0082) 121.69 (0.56) 120.72 (0.55) C3 - C2 C4 C4 - Distance Angles C5 1.3743 (0.0076) C3 1.4024 (0.0079) 120.26 (0.54) H4 0.9500 119.87 119.87 C4 - C5 C3 C5 - Distance Angles C4 1.3743 (0.0076) C6 1.4171 (0.0071) 121.91 (0.53) N5 1.4509 (0.0070) 117.57 (0.48) 120.52 (0.48) C5 - C4 C6 C6 - Distance Angles O6 1.2687 (0.0058) N1 1.3668 (0.0066) 117.45 (0.49) C5 1.4171 (0.0071) 127.64 (0.51) 114.91 (0.46) C6 - O6 N1 C7 - Distance Angles N1 1.4712 (0.0064) Si1 1.8803 (0.0058) 108.00 (0.35) H7A 0.9900 110.10 110.10 H7B 0.9900 110.10 110.10 108.43 C7 - N1 Si1 H7A C8 - Distance Angles C3 1.4982 (0.0082) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C3 H8A H8B C9 - Distance Angles Si1 1.8494 (0.0053) 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 C22 - Distance Angles N21 1.3619 (0.0070) C23 1.3746 (0.0074) 121.78 (0.51) H22 0.9500 119.11 119.11 C22 - N21 C23 C23 - Distance Angles C22 1.3746 (0.0074) C24 1.3963 (0.0078) 116.57 (0.52) C28 1.5063 (0.0080) 121.72 (0.52) 121.69 (0.52) C23 - C22 C24 C24 - Distance Angles C25 1.3704 (0.0077) C23 1.3963 (0.0078) 121.65 (0.53) H24 0.9500 119.17 119.17 C24 - C25 C23 C25 - Distance Angles C24 1.3704 (0.0077) C26 1.4202 (0.0071) 120.61 (0.50) N25 1.4523 (0.0066) 119.40 (0.49) 119.94 (0.49) C25 - C24 C26 C26 - Distance Angles O26 1.2710 (0.0063) N21 1.3583 (0.0067) 117.12 (0.46) C25 1.4202 (0.0071) 126.73 (0.49) 116.10 (0.49) C26 - O26 N21 C27 - Distance Angles N21 1.4866 (0.0061) Si1 1.8869 (0.0058) 107.00 (0.34) H27A 0.9900 110.32 110.32 H27B 0.9900 110.32 110.32 108.56 C27 - N21 Si1 H27A C28 - Distance Angles C23 1.5063 (0.0080) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C23 H28A H28B N1 - Distance Angles C2 1.3559 (0.0068) C6 1.3668 (0.0066) 124.06 (0.49) C7 1.4712 (0.0064) 122.22 (0.47) 113.59 (0.44) N1 - C2 C6 N5 - Distance Angles O5B 1.2290 (0.0057) O5A 1.2307 (0.0056) 123.26 (0.48) C5 1.4509 (0.0070) 118.35 (0.45) 118.40 (0.45) N5 - O5B O5A N21 - Distance Angles C26 1.3583 (0.0067) C22 1.3619 (0.0070) 123.09 (0.45) C27 1.4866 (0.0061) 114.06 (0.44) 122.60 (0.44) N21 - C26 C22 N25 - Distance Angles O25A 1.2220 (0.0057) O25B 1.2257 (0.0054) 123.70 (0.46) C25 1.4523 (0.0066) 118.62 (0.44) 117.66 (0.47) N25 - O25A O25B O5A - Distance Angles N5 1.2307 (0.0056) O5A - O5B - Distance Angles N5 1.2290 (0.0057) O5B - O6 - Distance Angles C6 1.2687 (0.0058) Si1 1.8672 (0.0038) 114.66 (0.35) O6 - C6 O25A - Distance Angles N25 1.2220 (0.0057) O25A - O25B - Distance Angles N25 1.2257 (0.0054) O25B - O26 - Distance Angles C26 1.2710 (0.0063) Si1 1.8889 (0.0037) 113.93 (0.34) O26 - C26 Si1 - Distance Angles C9 1.8494 (0.0054) O6 1.8672 (0.0038) 95.13 (0.21) C7 1.8803 (0.0058) 120.17 (0.27) 85.80 (0.20) C27 1.8869 (0.0058) 116.94 (0.25) 89.86 (0.19) 122.89 (0.26) O26 1.8889 (0.0037) 96.22 (0.21) 168.66 (0.19) 88.40 (0.20) 85.12 (0.20) Si1 - C9 O6 C7 C27 C32 - Distance Angles N31 1.3475 (0.0065) C33 1.3794 (0.0073) 121.61 (0.51) H32 0.9500 119.20 119.20 C32 - N31 C33 C33 - Distance Angles C32 1.3794 (0.0073) C34 1.4055 (0.0075) 116.09 (0.51) C38 1.4960 (0.0073) 121.37 (0.49) 122.53 (0.49) C33 - C32 C34 C34 - Distance Angles C35 1.3597 (0.0075) C33 1.4055 (0.0075) 121.70 (0.50) H34 0.9500 119.15 119.15 C34 - C35 C33 C35 - Distance Angles C34 1.3597 (0.0075) C36 1.4113 (0.0068) 120.80 (0.51) N35 1.4645 (0.0069) 118.37 (0.46) 120.83 (0.49) C35 - C34 C36 C36 - Distance Angles O36 1.2838 (0.0064) N31 1.3611 (0.0066) 116.69 (0.45) C35 1.4113 (0.0068) 127.28 (0.50) 116.02 (0.49) C36 - O36 N31 C37 - Distance Angles N31 1.4829 (0.0061) Si2 1.8978 (0.0055) 107.65 (0.33) H37A 0.9900 110.18 110.18 H37B 0.9900 110.18 110.18 108.48 C37 - N31 Si2 H37A C38 - Distance Angles C33 1.4960 (0.0073) H38A 0.9800 109.47 H38B 0.9800 109.47 109.47 H38C 0.9800 109.47 109.47 109.47 C38 - C33 H38A H38B C39 - Distance Angles Si2 1.8519 (0.0055) H39A 0.9800 109.47 H39B 0.9800 109.47 109.47 H39C 0.9800 109.47 109.47 109.47 C39 - Si2 H39A H39B C42 - Distance Angles N41 1.3528 (0.0063) C43 1.3853 (0.0075) 121.87 (0.51) H42 0.9500 119.07 119.07 C42 - N41 C43 C43 - Distance Angles C44 1.3810 (0.0081) C42 1.3853 (0.0075) 115.74 (0.53) C48 1.4924 (0.0078) 122.74 (0.55) 121.50 (0.52) C43 - C44 C42 C44 - Distance Angles C45 1.3642 (0.0075) C43 1.3810 (0.0080) 122.41 (0.55) H44 0.9500 118.80 118.80 C44 - C45 C43 C45 - Distance Angles C44 1.3642 (0.0075) C46 1.4146 (0.0075) 121.52 (0.51) N45 1.4612 (0.0068) 119.07 (0.51) 119.39 (0.49) C45 - C44 C46 C46 - Distance Angles O46 1.2719 (0.0061) N41 1.3696 (0.0065) 117.01 (0.49) C45 1.4146 (0.0075) 128.31 (0.50) 114.68 (0.49) C46 - O46 N41 C47 - Distance Angles N41 1.4760 (0.0063) Si2 1.8817 (0.0057) 107.54 (0.34) H47A 0.9900 110.20 110.20 H47B 0.9900 110.20 110.20 108.49 C47 - N41 Si2 H47A C48 - Distance Angles C43 1.4924 (0.0078) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C43 H48A H48B N31 - Distance Angles C32 1.3475 (0.0065) C36 1.3611 (0.0066) 123.43 (0.45) C37 1.4829 (0.0061) 122.32 (0.43) 114.09 (0.42) N31 - C32 C36 N35 - Distance Angles O35B 1.2140 (0.0059) O35A 1.2370 (0.0055) 123.66 (0.48) C35 1.4645 (0.0069) 119.27 (0.43) 117.05 (0.46) N35 - O35B O35A N41 - Distance Angles C42 1.3528 (0.0063) C46 1.3696 (0.0065) 123.69 (0.47) C47 1.4760 (0.0063) 121.87 (0.43) 114.29 (0.43) N41 - C42 C46 N45 - Distance Angles O45A 1.2278 (0.0056) O45B 1.2349 (0.0056) 123.19 (0.47) C45 1.4612 (0.0068) 119.87 (0.46) 116.90 (0.47) N45 - O45A O45B O35A - Distance Angles N35 1.2370 (0.0055) O35A - O35B - Distance Angles N35 1.2140 (0.0059) O35B - O36 - Distance Angles C36 1.2838 (0.0064) Si2 1.8908 (0.0037) 114.66 (0.33) O36 - C36 O45A - Distance Angles N45 1.2278 (0.0056) O45A - O45B - Distance Angles N45 1.2349 (0.0056) O45B - O46 - Distance Angles C46 1.2719 (0.0061) Si2 1.8735 (0.0037) 114.64 (0.34) O46 - C46 Si2 - Distance Angles C39 1.8519 (0.0056) O46 1.8735 (0.0037) 95.33 (0.21) C47 1.8817 (0.0057) 119.30 (0.27) 86.10 (0.20) O36 1.8908 (0.0037) 96.27 (0.21) 168.39 (0.18) 88.19 (0.20) C37 1.8978 (0.0056) 117.45 (0.26) 90.01 (0.19) 123.24 (0.26) 84.68 (0.20) Si2 - C39 O46 C47 O36 C91 - Distance Angles O91 1.3471 (0.0089) H91A 0.9800 109.47 H91B 0.9800 109.47 109.47 H91C 0.9800 109.47 109.47 109.47 C91 - O91 H91A H91B O91 - Distance Angles C91 1.3471 (0.0090) H91 0.8400 109.47 O91 - C91 C92 - Distance Angles O92 1.3429 (0.0090) H92A 0.9800 109.47 H92B 0.9800 109.47 109.47 H92C 0.9800 109.47 109.47 109.47 C92 - O92 H92A H92B O92 - Distance Angles C92 1.3429 (0.0090) H92 0.8400 109.47 O92 - C92 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.39 3.173(6) 154.9 O91-H91...Cl1 0.84 2.37 3.164(6) 158.1 O92-H92...Cl2 FMAP and GRID set by program FMAP 2 2 32 GRID -3.448 -1 -1 3.448 1 1 R1 = 0.1131 for 8303 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.67 at 0.3595 0.1094 0.2696 [ 1.12 A from O92 ] Deepest hole -0.66 at 0.2807 -0.0010 0.2643 [ 0.78 A from C92 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 6740 /104407 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3595 1.1094 0.2696 1.00000 0.05 0.67 1.12 O92 1.18 H92 1.29 H92C 1.42 C92 Q2 1 0.2517 0.3793 0.1687 1.00000 0.05 0.56 1.09 O25A 1.77 N25 2.23 O25B 2.25 H91B Q3 1 0.1493 0.5879 0.2883 1.00000 0.05 0.53 1.05 H91 1.09 O91 1.14 H91A 1.26 C91 Q4 1 0.3092 0.8285 0.4507 1.00000 0.05 0.52 1.41 C33 1.58 C34 2.08 C32 2.11 O45B Q5 1 0.4496 0.5734 0.6401 1.00000 0.05 0.51 0.74 C47 1.20 SI2 1.26 H47B 1.49 H47A Q6 1 -0.1208 0.5486 0.1107 1.00000 0.05 0.47 0.72 N5 0.78 C5 1.64 O5B 1.73 O5A Q7 1 0.3813 0.2551 0.5406 1.00000 0.05 0.47 0.90 H39B 1.31 H39A 1.32 C39 1.95 H39C Q8 1 0.4401 0.9206 0.4178 1.00000 0.05 0.47 1.15 H32 1.62 CL2 1.98 C32 2.49 H37B Q9 1 0.0185 0.5881 0.3404 1.00000 0.05 0.45 1.17 CL1 1.96 H7A 2.38 N1 2.42 H2 Q10 1 0.4684 0.4343 0.7611 1.00000 0.05 0.44 1.69 H42 1.95 H47B 2.14 C42 2.29 H92 Shortest distances between peaks (including symmetry equivalents) 1 10 2.68 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 0.02: Analyse other restraints etc. 0.73: 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 16.91: Structure factors and derivatives 29.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 2.30: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.28: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.20: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0245p21c finished at 14:51:46 Total CPU time: 50.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++