+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0345pbca started at 16:17:02 on 11-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0345pbca in Pbca CELL 0.71073 6.8700 23.3867 24.3510 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0014 0.0015 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O SI CL UNIT 120 152 32 56 8 8 V = 3912.39 F(000) = 1792.0 Mu = 0.30 mm-1 Cell Wt = 3447.06 Rho = 1.463 MERG 2 OMIT -3.00 50.00 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.05 0.12 0.17 ACTA BOND $H WGHT 0.04000 71.96150 L.S. 4 TEMP -153.00 FVAR 0.27623 MOLE 1 C2 1 0.585268 0.235598 0.456586 11.00000 0.02538 0.02199 = 0.06904 0.01434 0.00017 -0.00321 AFIX 43 H2 2 0.612807 0.267609 0.479313 11.00000 -1.20000 AFIX 0 C3 1 0.555922 0.243031 0.402424 11.00000 0.02980 0.03616 = 0.08112 0.02628 0.00302 0.00451 C4 1 0.512371 0.195789 0.370777 11.00000 0.03214 0.02321 = 0.06699 0.01352 -0.00131 -0.00043 AFIX 43 H4 2 0.490450 0.200305 0.332502 11.00000 -1.20000 AFIX 0 C5 1 0.500308 0.142416 0.393830 11.00000 0.02236 0.03943 = 0.04791 0.01291 0.00365 -0.00526 C6 1 0.536352 0.134000 0.449687 11.00000 0.01387 0.04315 = 0.04869 0.00703 0.00056 -0.00126 C7 1 0.614877 0.172067 0.536814 11.00000 0.03449 0.03038 = 0.05815 0.01206 -0.00130 -0.00810 AFIX 23 H7A 2 0.526744 0.195506 0.559790 11.00000 -1.20000 H7B 2 0.750837 0.182701 0.545603 11.00000 -1.20000 AFIX 0 C8 1 0.573430 0.301352 0.376684 11.00000 0.05517 0.04055 = 0.07722 0.02315 0.01456 0.01046 AFIX 137 H8A 2 0.578306 0.330477 0.405585 11.00000 -1.50000 H8B 2 0.460591 0.308364 0.353001 11.00000 -1.50000 H8C 2 0.692785 0.303168 0.354712 11.00000 -1.50000 AFIX 0 C22 1 0.948481 -0.019155 0.618100 11.00000 0.01817 0.05190 = 0.06140 0.02838 -0.00652 -0.00510 AFIX 43 H22 2 0.988391 -0.044503 0.589770 11.00000 -1.20000 AFIX 0 C23 1 0.998048 -0.031497 0.670745 11.00000 0.03222 0.08430 = 0.03621 0.02251 -0.00816 -0.01407 C24 1 0.946293 0.009295 0.710080 11.00000 0.02865 0.08297 = 0.02726 0.02501 -0.01374 -0.02068 AFIX 43 H24 2 0.985788 0.004419 0.747173 11.00000 -1.20000 AFIX 0 C25 1 0.840357 0.055651 0.695655 11.00000 0.02803 0.07043 = 0.03663 -0.00027 -0.00055 -0.02516 C26 1 0.776072 0.066781 0.641007 11.00000 0.02350 0.05714 = 0.02897 0.01226 0.00194 -0.01600 C27 1 0.773823 0.038901 0.547387 11.00000 0.02786 0.03135 = 0.04131 0.00978 0.00292 -0.00258 AFIX 23 H27A 2 0.723250 0.003070 0.531106 11.00000 -1.20000 H27B 2 0.882104 0.052975 0.524215 11.00000 -1.20000 AFIX 0 C28 1 1.100768 -0.084122 0.686193 11.00000 0.03247 0.09609 = 0.08213 0.05801 -0.00814 0.00556 AFIX 137 H28A 2 1.018542 -0.106783 0.710847 11.00000 -1.50000 H28B 2 1.222511 -0.074310 0.704932 11.00000 -1.50000 H28C 2 1.129837 -0.106411 0.653115 11.00000 -1.50000 AFIX 0 C31 1 0.328233 0.068378 0.570429 11.00000 0.03091 0.04018 = 0.04414 0.01464 0.00482 -0.00097 AFIX 137 H31A 2 0.230075 0.088461 0.548503 11.00000 -1.50000 H31B 2 0.305479 0.075881 0.609499 11.00000 -1.50000 H31C 2 0.319159 0.027188 0.563486 11.00000 -1.50000 AFIX 0 N1 3 0.575573 0.182307 0.478874 11.00000 0.02232 0.02834 = 0.05193 0.00782 -0.00316 0.00246 N5 3 0.451988 0.094216 0.357348 11.00000 0.03233 0.04785 = 0.05582 0.02786 -0.00335 -0.01751 N21 3 0.843468 0.028290 0.604289 11.00000 0.02127 0.05041 = 0.03589 0.01888 -0.00286 -0.00616 N25 3 0.793693 0.097402 0.738625 11.00000 0.03832 0.09739 = 0.06650 0.00857 -0.01015 -0.03805 O5A 4 0.378497 0.105502 0.312448 11.00000 0.05493 0.07282 = 0.06045 0.03829 -0.01279 -0.01662 O5B 4 0.488389 0.046522 0.374041 11.00000 0.04598 0.03682 = 0.05161 0.00932 0.00453 -0.00426 O6 4 0.533705 0.087113 0.475382 11.00000 0.02824 0.02368 = 0.04723 0.01544 -0.00322 -0.00981 O25A 4 0.728495 0.143131 0.726751 11.00000 0.06584 0.13945 = 0.07104 -0.02536 -0.00678 0.04227 O25B 4 0.814424 0.083358 0.785447 11.00000 0.18225 0.07688 = 0.05118 -0.00713 0.00493 -0.08256 O26 4 0.665246 0.106687 0.623851 11.00000 0.03145 0.06577 = 0.04363 0.00644 -0.00210 0.00198 SI1 5 0.574645 0.094166 0.551088 11.00000 0.02577 0.04011 = 0.04750 0.01033 -0.00001 -0.00422 CL2 6 0.043825 0.145931 0.456158 11.00000 0.03150 0.05222 = 0.07197 0.01472 0.00111 0.00401 MOLE 2 O1W 4 0.533353 0.266447 0.652752 11.00000 0.08359 0.04483 = 0.34974 0.06463 -0.03703 -0.01338 HKLF 4 Covalent radii and connectivity table for 2009src0345pbca in Pbca C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C2 - C3 N1 C3 - C2 C4 C8 C4 - C5 C3 C5 - C4 C6 N5 C6 - O6 N1 C5 C7 - N1 Si1 C8 - C3 C22 - C23 N21 C23 - C22 C24 C28 C24 - C25 C23 C25 - C24 C26 N25 C26 - O26 N21 C25 C27 - N21 Si1 C28 - C23 C31 - Si1 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 - C31 O6 C7 C27 O26 Cl2 - no bonds found O1W - no bonds found h k l Fo^2 Sigma Why rejected 1 2 0 7.27 1.55 observed but should be systematically absent 1 5 0 46.39 10.95 observed but should be systematically absent 1 5 0 44.82 10.82 observed but should be systematically absent 1 11 0 100.38 24.23 observed but should be systematically absent 1 11 0 51.67 11.34 observed but should be systematically absent 1 17 0 26.70 6.59 observed but should be systematically absent 1 21 0 80.02 17.32 observed but should be systematically absent 1 23 0 63.56 15.15 observed but should be systematically absent 1 23 0 63.75 11.76 observed but should be systematically absent 1 23 0 50.91 10.36 observed but should be systematically absent 1 24 0 43.54 10.54 observed but should be systematically absent 1 27 0 50.57 12.44 observed but should be systematically absent 3 3 0 6.19 1.54 observed but should be systematically absent 3 9 0 7.27 1.75 observed but should be systematically absent 3 16 0 23.41 5.68 observed but should be systematically absent 5 4 0 10.05 1.94 observed but should be systematically absent 5 4 0 14.50 1.59 observed but should be systematically absent 5 15 0 54.01 13.08 observed but should be systematically absent 5 15 0 60.03 13.50 observed but should be systematically absent 3 0 1 26.11 6.10 observed but should be systematically absent 0 27 2 37.33 9.11 observed but should be systematically absent 0 25 3 22.30 5.34 observed but should be systematically absent 0 13 3 23.55 5.43 observed but should be systematically absent 0 13 3 26.44 4.73 observed but should be systematically absent 0 13 3 23.17 2.37 observed but should be systematically absent 0 5 4 11.20 2.56 observed but should be systematically absent 0 13 5 8.78 1.79 observed but should be systematically absent 0 9 5 15.90 3.13 observed but should be systematically absent 0 7 5 33.41 5.02 observed but should be systematically absent 0 7 5 23.23 5.36 observed but should be systematically absent 0 7 5 18.83 3.48 observed but should be systematically absent 0 9 5 15.94 3.84 observed but should be systematically absent 0 23 7 29.89 6.44 observed but should be systematically absent 0 1 7 14.38 3.04 observed but should be systematically absent 0 7 8 15.52 3.80 observed but should be systematically absent 0 7 8 23.30 4.20 observed but should be systematically absent 0 17 9 23.64 5.35 observed but should be systematically absent 0 1 10 37.67 4.69 observed but should be systematically absent 0 1 10 40.82 5.33 observed but should be systematically absent 0 1 10 20.05 3.32 observed but should be systematically absent 0 1 10 27.04 4.65 observed but should be systematically absent 0 1 10 22.74 4.46 observed but should be systematically absent 0 3 12 52.36 11.77 observed but should be systematically absent 0 5 12 12.96 3.05 observed but should be systematically absent 0 1 13 49.21 10.93 observed but should be systematically absent 0 1 13 29.91 7.36 observed but should be systematically absent 0 1 13 40.44 8.09 observed but should be systematically absent 0 11 13 22.54 3.82 observed but should be systematically absent 0 9 14 37.63 8.69 observed but should be systematically absent 0 1 14 51.92 6.98 observed but should be systematically absent ** etc. ** 25679 Reflections read, of which 5636 rejected -8 =< h =< 8, -27 =< k =< 27, -28 =< l =< 28, Max. 2-theta = 50.00 88 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 5 5 80.04 2.40 6 14.79 0 4 8 441.20 20.55 3 112.23 0 4 12 455.01 29.64 2 167.08 0 8 13 314.57 27.77 2 211.91 5 3 14 25.36 3.83 2 19.30 1 4 16 89.92 4.58 3 23.29 5 6 21 25.42 4.75 2 24.70 1 9 24 16.13 3.34 2 19.61 8 Inconsistent equivalents 3395 Unique reflections, of which 0 suppressed R(int) = 0.0832 R(sigma) = 0.0715 Friedel opposites merged Maximum memory for data reduction = 2363 / 34271 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 120.00 120.00 H 152.00 136.00 N 32.00 32.00 O 56.00 56.00 SI 8.00 8.00 CL 8.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3057 / 320079 wR2 = 0.3534 before cycle 1 for 3395 data and 256 / 256 parameters GooF = S = 1.271; Restrained GooF = 1.271 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 71.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27623 0.00156 0.003 OSF Mean shift/su = 0.000 Maximum = 0.003 for OSF Max. shift = 0.000 A for H31B Max. dU = 0.000 for O1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 3057 / 320079 wR2 = 0.3534 before cycle 2 for 3395 data and 256 / 256 parameters GooF = S = 1.271; Restrained GooF = 1.271 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 71.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27624 0.00156 0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for y N5 Max. shift = 0.000 A for H31B Max. dU = 0.000 for O25B Least-squares cycle 3 Maximum vector length = 511 Memory required = 3057 / 320079 wR2 = 0.3534 before cycle 3 for 3395 data and 256 / 256 parameters GooF = S = 1.271; Restrained GooF = 1.271 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 71.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27624 0.00156 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y N5 Max. shift = 0.000 A for H31B Max. dU = 0.000 for N25 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3057 / 320079 wR2 = 0.3534 before cycle 4 for 3395 data and 256 / 256 parameters GooF = S = 1.271; Restrained GooF = 1.271 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 71.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27624 0.00156 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U22 C4 Max. shift = 0.000 A for N5 Max. dU = 0.000 for N25 Largest correlation matrix elements -0.555 U12 O25B / U11 O25B -0.512 U12 O25B / U22 O25B Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.6128 0.2676 0.4793 43 0.950 0.000 C2 C3 N1 H4 0.4905 0.2003 0.3325 43 0.950 0.000 C4 C5 C3 H7A 0.5267 0.1955 0.5598 23 0.990 0.000 C7 N1 Si1 H7B 0.7508 0.1827 0.5456 23 0.990 0.000 C7 N1 Si1 H8A 0.5783 0.3305 0.4056 137 0.980 0.000 C8 C3 H8A H8B 0.4606 0.3084 0.3530 137 0.980 0.000 C8 C3 H8A H8C 0.6928 0.3032 0.3547 137 0.980 0.000 C8 C3 H8A H22 0.9884 -0.0445 0.5898 43 0.950 0.000 C22 C23 N21 H24 0.9858 0.0044 0.7472 43 0.950 0.000 C24 C25 C23 H27A 0.7233 0.0031 0.5311 23 0.990 0.000 C27 N21 Si1 H27B 0.8821 0.0530 0.5242 23 0.990 0.000 C27 N21 Si1 H28A 1.0185 -0.1068 0.7108 137 0.980 0.000 C28 C23 H28A H28B 1.2225 -0.0743 0.7049 137 0.980 0.000 C28 C23 H28A H28C 1.1298 -0.1064 0.6531 137 0.980 0.000 C28 C23 H28A H31A 0.2301 0.0885 0.5485 137 0.980 0.000 C31 Si1 H31A H31B 0.3055 0.0759 0.6095 137 0.980 0.000 C31 Si1 H31A H31C 0.3192 0.0272 0.5635 137 0.980 0.000 C31 Si1 H31A 2009src0345pbca in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.58527 0.23560 0.45659 1.00000 0.02538 0.02199 0.06906 0.01435 0.00017 -0.00321 0.03881 0.02014 0.00146 0.00042 0.00053 0.00000 0.00515 0.00512 0.00903 0.00539 0.00581 0.00416 0.00291 H2 0.61281 0.26761 0.47931 1.00000 0.04657 0.00000 0.00000 C3 0.55592 0.24303 0.40242 1.00000 0.02980 0.03617 0.08111 0.02628 0.00302 0.00451 0.04903 0.02426 0.00163 0.00050 0.00061 0.00000 0.00599 0.00645 0.01020 0.00663 0.00647 0.00517 0.00345 C4 0.51237 0.19579 0.37078 1.00000 0.03215 0.02320 0.06700 0.01352 -0.00131 -0.00043 0.04078 0.02073 0.00156 0.00043 0.00056 0.00000 0.00577 0.00539 0.00857 0.00555 0.00587 0.00455 0.00294 H4 0.49045 0.20030 0.33250 1.00000 0.04894 0.00000 0.00000 C5 0.50031 0.14242 0.39383 1.00000 0.02235 0.03943 0.04792 0.01291 0.00365 -0.00526 0.03657 0.02020 0.00148 0.00048 0.00050 0.00000 0.00510 0.00606 0.00741 0.00543 0.00513 0.00463 0.00268 C6 0.53635 0.13400 0.44969 1.00000 0.01387 0.04316 0.04868 0.00703 0.00056 -0.00126 0.03524 0.01915 0.00135 0.00047 0.00049 0.00000 0.00451 0.00644 0.00749 0.00554 0.00489 0.00433 0.00266 C7 0.61488 0.17207 0.53681 1.00000 0.03449 0.03038 0.05816 0.01206 -0.00131 -0.00810 0.04101 0.01962 0.00166 0.00044 0.00050 0.00000 0.00592 0.00562 0.00832 0.00552 0.00586 0.00474 0.00291 H7A 0.52675 0.19551 0.55979 1.00000 0.04921 0.00000 0.00000 H7B 0.75084 0.18270 0.54560 1.00000 0.04921 0.00000 0.00000 C8 0.57343 0.30135 0.37668 1.00000 0.05518 0.04055 0.07722 0.02316 0.01456 0.01047 0.05765 0.02639 0.00202 0.00051 0.00060 0.00000 0.00806 0.00697 0.01011 0.00691 0.00763 0.00623 0.00377 H8A 0.57829 0.33048 0.40559 1.00000 0.08647 0.00000 0.00000 H8B 0.46060 0.30836 0.35300 1.00000 0.08647 0.00000 0.00000 H8C 0.69280 0.30317 0.35472 1.00000 0.08647 0.00000 0.00000 C22 0.94848 -0.01915 0.61810 1.00000 0.01817 0.05190 0.06140 0.02838 -0.00651 -0.00510 0.04382 0.02155 0.00144 0.00051 0.00054 0.00000 0.00507 0.00705 0.00847 0.00632 0.00548 0.00491 0.00315 H22 0.98839 -0.04450 0.58977 1.00000 0.05259 0.00000 0.00000 C23 0.99805 -0.03150 0.67074 1.00000 0.03222 0.08431 0.03620 0.02252 -0.00816 -0.01407 0.05091 0.02291 0.00171 0.00063 0.00053 0.00000 0.00629 0.00984 0.00740 0.00709 0.00568 0.00645 0.00351 C24 0.94629 0.00929 0.71008 1.00000 0.02865 0.08297 0.02726 0.02502 -0.01374 -0.02069 0.04630 0.02075 0.00159 0.00060 0.00048 0.00000 0.00585 0.00952 0.00661 0.00656 0.00535 0.00635 0.00338 H24 0.98579 0.00442 0.74717 1.00000 0.05555 0.00000 0.00000 C25 0.84036 0.05565 0.69565 1.00000 0.02803 0.07043 0.03664 -0.00027 -0.00055 -0.02516 0.04504 0.01966 0.00161 0.00059 0.00050 0.00000 0.00561 0.00872 0.00725 0.00648 0.00542 0.00600 0.00319 C26 0.77607 0.06678 0.64101 1.00000 0.02350 0.05716 0.02896 0.01227 0.00194 -0.01600 0.03654 0.01914 0.00151 0.00053 0.00045 0.00000 0.00516 0.00731 0.00642 0.00550 0.00501 0.00525 0.00274 C27 0.77382 0.03890 0.54739 1.00000 0.02786 0.03135 0.04131 0.00978 0.00292 -0.00258 0.03351 0.01873 0.00147 0.00043 0.00045 0.00000 0.00518 0.00538 0.00672 0.00497 0.00508 0.00442 0.00249 H27A 0.72325 0.00307 0.53111 1.00000 0.04021 0.00000 0.00000 H27B 0.88210 0.05298 0.52421 1.00000 0.04021 0.00000 0.00000 C28 1.10077 -0.08412 0.68619 1.00000 0.03247 0.09609 0.08213 0.05801 -0.00815 0.00556 0.07023 0.02874 0.00183 0.00067 0.00064 0.00000 0.00643 0.01138 0.01087 0.00949 0.00720 0.00719 0.00485 H28A 1.01854 -0.10678 0.71085 1.00000 0.10535 0.00000 0.00000 H28B 1.22252 -0.07431 0.70493 1.00000 0.10535 0.00000 0.00000 H28C 1.12983 -0.10641 0.65311 1.00000 0.10535 0.00000 0.00000 C31 0.32823 0.06838 0.57043 1.00000 0.03091 0.04018 0.04413 0.01464 0.00482 -0.00096 0.03841 0.02031 0.00152 0.00048 0.00048 0.00000 0.00555 0.00610 0.00730 0.00546 0.00530 0.00487 0.00275 H31A 0.23008 0.08846 0.54850 1.00000 0.05761 0.00000 0.00000 H31B 0.30547 0.07589 0.60950 1.00000 0.05761 0.00000 0.00000 H31C 0.31917 0.02719 0.56349 1.00000 0.05761 0.00000 0.00000 N1 0.57557 0.18231 0.47887 1.00000 0.02232 0.02834 0.05193 0.00782 -0.00316 0.00246 0.03420 0.01554 0.00119 0.00035 0.00040 0.00000 0.00423 0.00455 0.00620 0.00417 0.00431 0.00366 0.00217 N5 0.45199 0.09421 0.35735 1.00000 0.03233 0.04785 0.05582 0.02785 -0.00336 -0.01752 0.04533 0.01786 0.00134 0.00043 0.00044 0.00000 0.00506 0.00607 0.00697 0.00527 0.00500 0.00461 0.00266 N21 0.84347 0.02829 0.60429 1.00000 0.02127 0.05040 0.03589 0.01888 -0.00285 -0.00616 0.03585 0.01607 0.00120 0.00041 0.00038 0.00000 0.00429 0.00565 0.00558 0.00461 0.00411 0.00407 0.00226 N25 0.79369 0.09740 0.73863 1.00000 0.03833 0.09740 0.06647 0.00856 -0.01015 -0.03806 0.06740 0.02011 0.00172 0.00066 0.00057 0.00000 0.00666 0.01063 0.00967 0.00824 0.00641 0.00706 0.00375 O5A 0.37850 0.10550 0.31245 1.00000 0.05493 0.07282 0.06045 0.03828 -0.01279 -0.01662 0.06273 0.01679 0.00135 0.00041 0.00040 0.00000 0.00555 0.00640 0.00621 0.00525 0.00504 0.00487 0.00277 O5B 0.48839 0.04652 0.37404 1.00000 0.04598 0.03682 0.05162 0.00933 0.00453 -0.00426 0.04481 0.01426 0.00116 0.00033 0.00035 0.00000 0.00465 0.00434 0.00526 0.00399 0.00415 0.00372 0.00205 O6 0.53370 0.08711 0.47538 1.00000 0.02824 0.02368 0.04724 0.01545 -0.00322 -0.00981 0.03305 0.01201 0.00098 0.00028 0.00031 0.00000 0.00365 0.00349 0.00474 0.00330 0.00343 0.00295 0.00177 O25A 0.72849 0.14313 0.72675 1.00000 0.06586 0.13942 0.07105 -0.02536 -0.00679 0.04228 0.09211 0.02199 0.00167 0.00065 0.00049 0.00000 0.00733 0.01144 0.00779 0.00796 0.00621 0.00785 0.00415 O25B 0.81442 0.08336 0.78545 1.00000 0.18225 0.07689 0.05119 -0.00714 0.00493 -0.08257 0.10344 0.01843 0.00228 0.00050 0.00045 0.00000 0.01430 0.00761 0.00695 0.00593 0.00810 0.00877 0.00508 O26 0.66525 0.10669 0.62385 1.00000 0.03145 0.06578 0.04364 0.00645 -0.00210 0.00198 0.04695 0.01434 0.00111 0.00037 0.00034 0.00000 0.00414 0.00556 0.00507 0.00439 0.00387 0.00408 0.00214 Si1 0.57464 0.09417 0.55109 1.00000 0.02578 0.04011 0.04750 0.01033 -0.00001 -0.00422 0.03780 0.00562 0.00043 0.00013 0.00014 0.00000 0.00147 0.00170 0.00205 0.00152 0.00146 0.00130 0.00082 Cl2 0.04382 0.14593 0.45616 1.00000 0.03150 0.05222 0.07197 0.01472 0.00111 0.00401 0.05190 0.00594 0.00041 0.00013 0.00015 0.00000 0.00144 0.00175 0.00236 0.00168 0.00151 0.00131 0.00091 O1W 0.53335 0.26645 0.65275 1.00000 0.08360 0.04484 0.34974 0.06464 -0.03703 -0.01338 0.15939 0.02814 0.00192 0.00046 0.00090 0.00000 0.00881 0.00665 0.02515 0.01074 0.01262 0.00622 0.00818 Final Structure Factor Calculation for 2009src0345pbca in Pbca Total number of l.s. parameters = 256 Maximum vector length = 511 Memory required = 2801 / 25039 wR2 = 0.3534 before cycle 5 for 3395 data and 0 / 256 parameters GooF = S = 1.271; Restrained GooF = 1.271 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 71.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1744 for 2812 Fo > 4sig(Fo) and 0.1940 for all 3395 data wR2 = 0.3534, GooF = S = 1.271, Restrained GooF = 1.271 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0731 0.0265 0.0168 C2 0.0936 0.0307 0.0229 C3 0.0709 0.0321 0.0194 C4 0.0573 0.0337 0.0187 C5 0.0535 0.0384 0.0138 C6 0.0633 0.0380 0.0218 C7 0.0961 0.0480 0.0289 C8 0.0864 0.0279 0.0172 C22 0.0972 0.0302 0.0254 C23 0.1007 0.0244 0.0137 C24 0.0821 0.0367 0.0163 C25 0.0666 0.0290 0.0139 C26 0.0474 0.0305 0.0227 C27 0.1476 0.0414 0.0217 C28 0.0573 0.0332 0.0248 C31 0.0545 0.0278 0.0203 N1 0.0839 0.0370 0.0151 N5 0.0644 0.0233 0.0198 N21 0.1189 0.0643 0.0191 N25 0.1130 0.0474 0.0278 O5A 0.0567 0.0476 0.0302 O5B 0.0568 0.0300 0.0123 O6 0.1658 0.0649 0.0456 O25A 0.2279 0.0516 0.0309 O25B may be split into 0.8412 0.0790 0.7858 and 0.7877 0.0877 0.7851 0.0676 0.0425 0.0308 O26 0.0550 0.0342 0.0242 Si1 0.0800 0.0450 0.0307 Cl2 0.3682 0.0789 0.0310 O1W may be split into 0.5280 0.2687 0.6635 and 0.5387 0.2642 0.6420 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.031 0.040 0.051 0.067 0.088 0.129 1.000 Number in group 368. 337. 356. 322. 319. 337. 355. 321. 338. 342. GooF 1.813 1.573 1.441 1.228 1.293 0.940 0.917 0.884 0.891 1.284 K 42.364 6.846 3.230 1.999 1.627 1.213 1.083 0.987 0.978 0.998 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.07 1.14 1.26 1.44 1.81 inf Number in group 353. 337. 331. 336. 352. 333. 339. 333. 341. 340. GooF 1.260 1.176 1.152 1.266 1.363 1.281 1.357 1.217 1.102 1.480 K 1.433 1.386 1.265 1.224 1.174 1.084 1.026 1.019 1.013 1.022 R1 0.401 0.362 0.323 0.282 0.250 0.209 0.185 0.151 0.113 0.085 Recommended weighting scheme: WGHT 0.0400 71.9528 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) 0 18 1 1701.77 2.13 5.00 0.004 1.30 2 18 1 1474.72 137.98 4.87 0.033 1.21 0 4 2 6483.47 3038.99 4.75 0.156 5.27 1 19 7 1711.12 156.60 4.61 0.035 1.14 0 6 1 701.40 10.77 4.18 0.009 3.85 0 8 4 1464.92 195.88 4.15 0.040 2.64 3 19 5 858.10 45.69 4.09 0.019 1.06 1 1 2 3926.08 7477.95 4.03 0.245 5.80 3 20 7 669.24 2.33 3.92 0.004 1.00 4 12 17 732.39 19.01 3.84 0.012 0.96 3 12 13 653.66 3.54 3.77 0.005 1.16 1 23 2 793.97 52.09 3.71 0.020 1.00 0 8 15 3396.88 6667.36 3.67 0.231 1.42 1 12 16 630.89 0.03 3.60 0.000 1.18 0 4 0 40999.12 54825.31 3.57 0.663 5.85 0 22 5 1025.59 90.94 3.54 0.027 1.04 0 14 3 1011.92 73.36 3.53 0.024 1.64 0 20 2 1090.69 196.19 3.44 0.040 1.16 2 7 27 1122.92 137.59 3.42 0.033 0.84 2 8 4 503.34 16.26 3.42 0.011 2.09 3 1 14 491.10 7.28 3.38 0.008 1.38 1 12 13 724.26 69.28 3.34 0.024 1.33 1 15 12 559.48 33.99 3.31 0.017 1.22 1 9 19 1268.47 278.36 3.24 0.047 1.13 3 5 18 595.23 42.39 3.17 0.018 1.13 2 16 4 394.69 2.65 3.14 0.005 1.31 2 2 4 1492.76 530.63 3.13 0.065 2.90 2 3 20 502.09 17.40 3.11 0.012 1.14 2 16 9 566.14 0.37 3.10 0.002 1.20 0 24 6 765.10 30.21 3.09 0.016 0.95 1 20 5 402.50 0.09 3.09 0.001 1.12 0 8 2 1441.63 506.32 3.09 0.064 2.84 1 8 21 730.09 82.78 3.04 0.026 1.06 0 0 4 5466.28 8428.67 2.97 0.260 6.09 2 9 24 470.95 4.46 2.97 0.006 0.91 1 16 15 394.61 7.56 2.96 0.008 1.07 2 18 13 473.42 33.75 2.96 0.016 1.02 5 20 5 496.40 14.21 2.96 0.011 0.88 1 19 5 2131.97 938.60 2.95 0.087 1.18 1 0 16 2331.09 4336.92 2.94 0.187 1.49 2 2 28 601.76 14.45 2.94 0.011 0.84 5 12 8 384.60 6.22 2.93 0.007 1.05 0 8 18 1093.76 2604.00 2.91 0.145 1.23 2 0 12 14569.37 9890.11 2.88 0.282 1.75 2 10 13 363.34 10.93 2.86 0.009 1.35 0 2 8 3621.20 2040.82 2.86 0.128 2.95 2 13 17 413.38 2.51 2.85 0.004 1.07 4 19 11 365.40 0.27 2.84 0.001 0.91 1 3 2 883.93 2094.19 2.78 0.130 4.75 2 10 22 405.06 15.37 2.78 0.011 0.96 Bond lengths and angles C2 - Distance Angles C3 1.3455 (0.0176) N1 1.3610 (0.0126) 120.12 (1.11) H2 0.9500 119.94 119.94 C2 - C3 N1 C3 - Distance Angles C2 1.3455 (0.0176) C4 1.3799 (0.0176) 118.46 (1.07) C8 1.5059 (0.0153) 120.87 (1.27) 120.67 (1.26) C3 - C2 C4 C4 - Distance Angles C5 1.3711 (0.0143) C3 1.3799 (0.0176) 120.89 (1.22) H4 0.9500 119.56 119.56 C4 - C5 C3 C5 - Distance Angles C4 1.3711 (0.0143) C6 1.3965 (0.0162) 121.09 (1.16) N5 1.4731 (0.0157) 117.60 (1.07) 121.30 (0.97) C5 - C4 C6 C6 - Distance Angles O6 1.2626 (0.0123) N1 1.3616 (0.0140) 117.69 (1.04) C5 1.3965 (0.0162) 127.05 (1.08) 115.25 (0.99) C6 - O6 N1 C7 - Distance Angles N1 1.4563 (0.0143) Si1 1.8752 (0.0104) 108.18 (0.75) H7A 0.9900 110.06 110.06 H7B 0.9900 110.06 110.06 108.41 C7 - N1 Si1 H7A C8 - Distance Angles C3 1.5059 (0.0153) 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 C22 - Distance Angles C23 1.3575 (0.0166) N21 1.3655 (0.0138) 122.54 (1.35) H22 0.9500 118.73 118.73 C22 - C23 N21 C23 - Distance Angles C22 1.3575 (0.0166) C24 1.3978 (0.0187) 115.99 (1.25) C28 1.4677 (0.0183) 122.75 (1.43) 121.26 (1.19) C23 - C22 C24 C24 - Distance Angles C25 1.3522 (0.0176) C23 1.3978 (0.0186) 120.40 (1.11) H24 0.9500 119.80 119.80 C24 - C25 C23 C25 - Distance Angles C24 1.3522 (0.0176) C26 1.4260 (0.0159) 123.74 (1.25) N25 1.4667 (0.0183) 117.78 (1.21) 118.46 (1.25) C25 - C24 C26 C26 - Distance Angles O26 1.2748 (0.0137) N21 1.3506 (0.0147) 118.41 (1.00) C25 1.4260 (0.0159) 128.64 (1.20) 112.95 (1.09) C26 - O26 N21 C27 - Distance Angles N21 1.4868 (0.0134) Si1 1.8844 (0.0105) 107.67 (0.72) H27A 0.9900 110.17 110.17 H27B 0.9900 110.17 110.17 108.47 C27 - N21 Si1 H27A C28 - Distance Angles C23 1.4677 (0.0184) 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 C31 - Distance Angles Si1 1.8577 (0.0106) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - Si1 H31A H31B N1 - Distance Angles C2 1.3610 (0.0126) C6 1.3616 (0.0140) 124.15 (1.02) C7 1.4563 (0.0143) 121.86 (0.97) 113.95 (0.87) N1 - C2 C6 N5 - Distance Angles O5B 1.2132 (0.0116) O5A 1.2329 (0.0127) 125.34 (1.15) C5 1.4731 (0.0157) 117.07 (0.98) 117.60 (0.98) N5 - O5B O5A N21 - Distance Angles C26 1.3506 (0.0147) C22 1.3655 (0.0138) 124.03 (1.03) C27 1.4868 (0.0134) 113.29 (0.88) 122.36 (1.03) N21 - C26 C22 N25 - Distance Angles O25A 1.1950 (0.0168) O25B 1.1950 (0.0154) 121.44 (1.66) C25 1.4667 (0.0183) 120.34 (1.35) 118.14 (1.51) N25 - O25A O25B O5A - Distance Angles N5 1.2329 (0.0127) O5A - O5B - Distance Angles N5 1.2132 (0.0116) O5B - O6 - Distance Angles C6 1.2626 (0.0123) Si1 1.8721 (0.0081) 114.16 (0.73) O6 - C6 O25A - Distance Angles N25 1.1950 (0.0168) O25A - O25B - Distance Angles N25 1.1950 (0.0154) O25B - O26 - Distance Angles C26 1.2748 (0.0137) Si1 1.9007 (0.0088) 112.85 (0.79) O26 - C26 Si1 - Distance Angles C31 1.8577 (0.0107) O6 1.8721 (0.0081) 94.83 (0.45) C7 1.8752 (0.0105) 119.78 (0.52) 85.71 (0.44) C27 1.8844 (0.0105) 116.82 (0.49) 90.09 (0.43) 123.40 (0.50) O26 1.9007 (0.0088) 96.44 (0.47) 168.74 (0.36) 88.56 (0.47) 84.98 (0.44) Si1 - C31 O6 C7 C27 FMAP and GRID set by program FMAP 2 2 26 GRID -1.087 24 -2 1.087 1 2 R1 = 0.1929 for 3395 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.27 at 0.2656 0.2344 0.2479 [ 2.69 A from H4 ] Deepest hole -0.52 at 0.4664 0.1476 0.7015 [ 1.86 A from O25B ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 2882 / 27646 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2656 0.2344 0.2479 1.00000 0.05 1.27 2.69 H4 2.84 H4 2.90 O1W 2.94 O25A Q2 1 0.5692 0.2589 0.6340 1.00000 0.05 0.80 0.55 O1W 2.36 H7A 2.98 H8C 3.06 H7B Q3 1 0.5166 0.2643 0.7002 1.00000 0.05 0.78 1.16 O1W 3.04 H28A 3.04 H8C 3.25 O25A Q4 1 0.5288 0.2958 0.6343 1.00000 0.05 0.62 0.82 O1W 2.57 H28C 2.59 CL2 2.96 H28A Q5 1 0.4410 0.2669 0.6332 1.00000 0.05 0.59 0.79 O1W 2.38 H8C 2.52 H7A 2.79 C3 Q6 1 0.5489 0.0846 0.5106 1.00000 0.05 0.45 0.87 O6 1.03 SI1 1.88 C6 2.08 C27 Q7 1 0.0585 0.1917 0.4313 1.00000 0.05 0.44 1.23 CL2 2.28 O1W 2.41 H2 2.66 H7A Q8 1 0.4921 0.2521 0.5445 1.00000 0.05 0.44 1.40 H7A 1.83 H2 2.06 C7 2.27 C2 Q9 1 0.4631 0.2223 0.7085 1.00000 0.05 0.43 1.77 O1W 2.48 H8C 2.64 O25A 2.92 O25A Q10 1 0.6021 0.2093 0.6218 1.00000 0.05 0.42 1.61 O1W 1.63 H7A 2.21 H7B 2.25 C7 Q11 1 0.4217 0.2952 0.3573 1.00000 0.05 0.41 0.42 H8B 1.15 C8 1.79 H8A 1.87 H8C Q12 1 0.9909 -0.0314 0.7967 1.00000 0.05 0.40 1.47 H24 1.92 O5B 1.99 O5A 2.10 H28B Q13 1 0.7364 0.2189 0.7284 1.00000 0.05 0.39 1.77 O25A 2.56 O1W 2.59 H8B 2.88 N25 Q14 1 0.3871 0.0118 0.3584 1.00000 0.05 0.39 1.14 O5B 1.98 N5 2.05 N21 2.15 C26 Q15 1 0.2540 0.2913 0.3501 1.00000 0.05 0.39 1.48 H8B 2.03 O1W 2.30 C8 2.43 O25A Q16 1 1.1693 -0.0875 0.5918 1.00000 0.05 0.38 1.58 H28C 1.60 H22 2.30 C22 2.32 CL2 Q17 1 0.7219 0.1723 0.7129 1.00000 0.05 0.38 0.76 O25A 1.93 N25 2.34 H8B 2.69 O26 Q18 1 1.0824 -0.0382 0.6040 1.00000 0.05 0.38 0.75 H22 1.08 C22 1.73 C23 2.02 H28C Q19 1 0.7231 0.1058 0.7824 1.00000 0.05 0.37 0.82 O25B 1.19 N25 1.61 O25A 2.55 C25 Q20 1 0.4114 0.0124 0.5497 1.00000 0.05 0.37 0.80 H31C 1.52 C31 2.17 H31A 2.20 H27A Shortest distances between peaks (including symmetry equivalents) 2 5 0.90 2 4 0.90 4 5 0.91 3 9 1.07 13 17 1.16 11 15 1.17 2 10 1.22 10 15 1.25 1 13 1.25 16 18 1.33 7 8 1.51 4 7 1.64 2 3 1.66 3 5 1.71 5 10 1.77 3 4 1.77 15 17 1.77 2 15 1.77 12 14 1.78 13 15 1.93 9 13 1.94 1 9 1.95 2 7 1.97 3 13 1.97 5 7 2.01 1 3 2.08 4 10 2.11 5 9 2.11 1 3 2.13 9 17 2.13 2 9 2.13 6 20 2.16 9 13 2.19 5 8 2.21 2 8 2.25 10 11 2.26 8 10 2.26 17 19 2.30 11 17 2.32 9 10 2.34 3 10 2.38 1 17 2.40 3 15 2.42 4 8 2.43 11 13 2.47 9 15 2.48 10 17 2.52 4 9 2.53 1 9 2.54 5 15 2.58 4 15 2.59 3 17 2.59 7 10 2.67 14 20 2.69 6 20 2.72 2 13 2.73 2 11 2.74 10 13 2.76 20 20 2.77 9 17 2.79 3 13 2.80 1 15 2.82 18 20 2.87 7 16 2.95 13 19 2.96 2 17 2.98 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.42: Structure factors and derivatives 1.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0345pbca finished at 16:17:06 Total CPU time: 4.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++