+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0980 started at 13:54:27 on 03-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0980 in P-1 CELL 0.71073 8.1291 10.8097 11.8595 109.321 103.396 100.002 ZERR 2.00 0.0003 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O SI CL UNIT 28 32 4 4 2 4 V = 920.42 F(000) = 356.0 Mu = 0.42 mm-1 Cell Wt = 686.56 Rho = 1.239 MERG 2 OMIT -3.00 55.00 OMIT 0 -1 2 OMIT -1 -1 2 OMIT -1 0 2 OMIT 0 -2 4 EXTI 0.01510 SHEL 7 0.77 DFIX 1.65 0.02 C6 CL6 C26 CL26 DFIX 1.45 0.02 C6 C8 C26 C28 SIMU C2 C3 C4 C5 C6 C8 DELU C2 C3 C4 C5 C6 C8 FMAP 2 PLAN 10 SIZE 0.06 0.13 0.22 ACTA BOND $H WGHT 0.08800 0.01040 L.S. 8 TEMP -153.00 FVAR 7.86300 0.45151 0.38144 PART 1 C28 1 0.212425 0.268718 -0.199351 21.00000 0.02036 0.03127 = 0.02141 0.01051 0.00696 0.00841 AFIX 137 H28A 2 0.235017 0.294172 -0.267472 21.00000 -1.50000 H28B 2 0.134941 0.319153 -0.163972 21.00000 -1.50000 H28C 2 0.155904 0.170676 -0.232434 21.00000 -1.50000 AFIX 0 CL26 6 0.178958 0.276788 -0.204535 -21.00000 0.04376 0.07390 = 0.03786 0.03256 0.00190 0.00704 PART 2 C8 1 0.282825 0.439808 0.559517 -31.00000 0.07072 0.04597 = 0.03689 -0.00821 0.02408 0.00609 AFIX 137 H8A 2 0.259701 0.481742 0.639105 -31.00000 -1.50000 H8B 2 0.319461 0.510233 0.528528 -31.00000 -1.50000 H8C 2 0.376453 0.395119 0.572926 -31.00000 -1.50000 AFIX 0 CL6 6 0.292859 0.463156 0.583964 31.00000 0.03911 0.03096 = 0.01751 0.00211 0.00696 0.00162 PART 0 C2 1 0.013944 0.168518 0.257362 11.00000 0.02981 0.02923 = 0.02778 0.01235 0.00946 0.00924 C3 1 -0.154856 0.139914 0.269045 11.00000 0.02800 0.04132 = 0.03509 0.01596 0.01141 0.00705 AFIX 43 H3 2 -0.249812 0.072344 0.201388 11.00000 -1.20000 AFIX 0 C4 1 -0.180100 0.211396 0.380034 11.00000 0.03315 0.05124 = 0.04026 0.02429 0.01669 0.01711 AFIX 43 H4 2 -0.293820 0.192677 0.389093 11.00000 -1.20000 AFIX 0 C5 1 -0.042283 0.310807 0.479599 11.00000 0.04234 0.04304 = 0.03130 0.01459 0.01886 0.01774 AFIX 43 H5 2 -0.061411 0.359434 0.556138 11.00000 -1.20000 AFIX 0 C6 1 0.121343 0.337814 0.466056 11.00000 0.03977 0.02870 = 0.02307 0.01109 0.01063 0.01026 C7 1 0.317658 0.285935 0.332654 11.00000 0.02807 0.03605 = 0.02515 0.01165 0.00977 0.00568 AFIX 23 H7A 2 0.405526 0.266567 0.392975 11.00000 -1.20000 H7B 2 0.360770 0.381710 0.342942 11.00000 -1.20000 AFIX 0 C22 1 0.530028 0.290171 0.091760 11.00000 0.03294 0.02748 = 0.02564 0.00746 0.01188 0.00865 C23 1 0.690451 0.347184 0.079854 11.00000 0.03264 0.03085 = 0.03886 0.01096 0.01602 0.00551 AFIX 43 H23 2 0.797881 0.363674 0.142363 11.00000 -1.20000 AFIX 0 C24 1 0.690883 0.378705 -0.022108 11.00000 0.04095 0.03759 = 0.04710 0.01706 0.02440 0.00853 AFIX 43 H24 2 0.799577 0.416882 -0.030529 11.00000 -1.20000 AFIX 0 C25 1 0.534441 0.355886 -0.114384 11.00000 0.05546 0.05127 = 0.04243 0.02315 0.02470 0.01310 AFIX 43 H25 2 0.536416 0.377763 -0.185411 11.00000 -1.20000 AFIX 0 C26 1 0.377841 0.301606 -0.101622 11.00000 0.04824 0.03862 = 0.03042 0.01460 0.01545 0.01194 C27 1 0.215960 0.215055 0.026832 11.00000 0.02806 0.02965 = 0.02334 0.00567 0.00880 0.00730 AFIX 23 H27A 2 0.138146 0.134172 -0.047400 11.00000 -1.20000 H27B 2 0.150865 0.284779 0.045765 11.00000 -1.20000 AFIX 0 C31 1 0.327089 -0.003054 0.135038 11.00000 0.03663 0.03897 = 0.04657 0.01749 0.01706 0.01362 AFIX 137 H31A 2 0.401950 -0.003284 0.212669 11.00000 -1.50000 H31B 2 0.386283 -0.022467 0.070524 11.00000 -1.50000 H31C 2 0.215182 -0.072998 0.105623 11.00000 -1.50000 AFIX 0 N1 3 0.148189 0.264510 0.356578 11.00000 0.02876 0.02882 = 0.02394 0.01119 0.00902 0.00708 N21 3 0.376350 0.269682 0.000823 11.00000 0.03424 0.02596 = 0.02531 0.00772 0.01222 0.00787 O2 4 0.051999 0.107720 0.156272 11.00000 0.02547 0.03693 = 0.02595 0.00686 0.00932 0.00196 O22 4 0.512694 0.254281 0.182748 11.00000 0.02750 0.04053 = 0.02565 0.01365 0.00935 0.00571 SI1 5 0.285106 0.166747 0.165928 11.00000 0.02527 0.03102 = 0.02448 0.00953 0.00866 0.00572 CL2 6 1.155238 0.517211 0.243695 11.00000 0.05226 0.03465 = 0.03747 0.01348 0.02511 0.01056 HKLF 4 Covalent radii and connectivity table for 2008src0980 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C28_a - C26 Cl26_a - C26 C8_b - C6 Cl6_b - C6 C2 - O2 N1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - N1 C5 C8_b Cl6_b C7 - N1 Si1 C22 - O22 N21 C23 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C25 N21 C28_a Cl26_a C27 - N21 Si1 C31 - Si1 N1 - C2 C6 C7 N21 - C26 C22 C27 O2 - C2 Si1 O22 - C22 Si1 Si1 - O2 C31 O22 C27 C7 Cl2 - no bonds found 18624 Reflections read, of which 38 rejected -10 =< h =< 10, -14 =< k =< 13, -15 =< l =< 15, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 -5 2 10270.42 67.98 7 493.89 -1 -2 2 17176.54 121.81 6 778.08 0 0 2 34257.86 108.59 4 697.73 -2 -6 3 7993.78 122.66 7 815.34 1 -6 3 6967.38 125.12 6 759.15 -2 2 3 7356.49 76.08 7 410.26 0 -8 4 2387.47 121.01 6 678.20 -1 -3 6 37870.82 109.36 5 1422.82 0 -8 7 7194.57 194.02 5 1029.34 9 Inconsistent equivalents 4196 Unique reflections, of which 0 suppressed R(int) = 0.0652 R(sigma) = 0.0654 Friedel opposites merged Maximum memory for data reduction = 2278 / 42649 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 28.00 28.14 H 32.00 32.42 N 4.00 4.00 O 4.00 4.00 SI 2.00 2.00 CL 4.00 3.86 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1560 before cycle 1 for 4196 data and 214 / 214 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.042 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.035 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.86928 0.02431 0.258 OSF 2 0.44853 0.00601 -0.495 FVAR 2 3 0.38350 0.00631 0.326 FVAR 3 4 0.01567 0.00436 0.130 EXTI Mean shift/su = 0.100 Maximum = -0.495 for FVAR 2 Max. shift = 0.013 A for H8C_b Max. dU = 0.000 for Cl26_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1559 before cycle 2 for 4196 data and 214 / 214 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.041 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87047 0.02432 0.049 OSF 2 0.44738 0.00602 -0.192 FVAR 2 3 0.38354 0.00631 0.006 FVAR 3 4 0.01589 0.00439 0.050 EXTI Mean shift/su = 0.043 Maximum = 0.312 for tors H31A Max. shift = 0.006 A for H31C Max. dU = 0.000 for C8_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 3 for 4196 data and 214 / 214 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.041 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87058 0.02432 0.005 OSF 2 0.44728 0.00602 -0.017 FVAR 2 3 0.38324 0.00628 -0.047 FVAR 3 4 0.01591 0.00440 0.006 EXTI Mean shift/su = 0.014 Maximum = -0.200 for U22 C8_b Max. shift = 0.004 A for H31C Max. dU =-0.001 for C8_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 4 for 4196 data and 214 / 214 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.041 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87060 0.02432 0.001 OSF 2 0.44722 0.00602 -0.009 FVAR 2 3 0.38282 0.00625 -0.067 FVAR 3 4 0.01593 0.00440 0.003 EXTI Mean shift/su = 0.009 Maximum = -0.130 for U22 C8_b Max. shift = 0.003 A for H8A_b Max. dU = 0.000 for C8_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 5 for 4196 data and 214 / 214 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.041 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87064 0.02432 0.002 OSF 2 0.44720 0.00602 -0.003 FVAR 2 3 0.38260 0.00623 -0.036 FVAR 3 4 0.01593 0.00440 0.002 EXTI Mean shift/su = 0.006 Maximum = -0.087 for U22 C8_b Max. shift = 0.002 A for H31C Max. dU = 0.000 for C8_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 6 for 4196 data and 214 / 214 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 1.7102 1.6500 0.0602 0.0200 DFIX C6 Cl6_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.042 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87067 0.02432 0.001 OSF 2 0.44718 0.00602 -0.003 FVAR 2 3 0.38246 0.00621 -0.022 FVAR 3 4 0.01594 0.00440 0.001 EXTI Mean shift/su = 0.003 Maximum = -0.056 for U22 C8_b Max. shift = 0.001 A for H31C Max. dU = 0.000 for C8_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 7 for 4196 data and 214 / 214 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 1.7103 1.6500 0.0603 0.0200 DFIX C6 Cl6_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.042 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87067 0.02432 0.000 OSF 2 0.44718 0.00602 0.000 FVAR 2 3 0.38237 0.00620 -0.015 FVAR 3 4 0.01594 0.00440 0.000 EXTI Mean shift/su = 0.002 Maximum = -0.037 for U22 C8_b Max. shift = 0.001 A for H31C Max. dU = 0.000 for C8_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 2870 / 267180 wR2 = 0.1558 before cycle 8 for 4196 data and 214 / 214 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 1.7104 1.6500 0.0604 0.0200 DFIX C6 Cl6_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.042 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 7.87068 0.02432 0.000 OSF 2 0.44717 0.00602 -0.001 FVAR 2 3 0.38232 0.00620 -0.009 FVAR 3 4 0.01594 0.00440 0.001 EXTI Mean shift/su = 0.001 Maximum = -0.023 for U22 C8_b Max. shift = 0.000 A for H31C Max. dU = 0.000 for C8_b Largest correlation matrix elements -0.935 z Cl26_a / z C28_a -0.811 U23 Cl6_b / z Cl6_b 0.741 U22 Cl6_b / y C8_b -0.927 z Cl6_b / U33 C8_b 0.780 U23 Cl6_b / U33 C8_b 0.732 U33 Cl6_b / z C8_b -0.927 y Cl26_a / y C28_a 0.768 U23 Cl6_b / U33 Cl6_b -0.728 U22 Cl6_b / y Cl6_b -0.902 y Cl6_b / U22 C8_b -0.763 U33 Cl6_b / z Cl6_b -0.720 U22 Cl26_a / U22 C28_a 0.878 x Cl26_a / U11 C28_a -0.761 U33 Cl26_a / U33 C28_a -0.714 U11 C28_a / x C28_a -0.846 U11 Cl26_a / x C28_a -0.756 U23 Cl6_b / y Cl6_b -0.709 z Cl6_b / z C8_b -0.834 x Cl6_b / x C8_b 0.754 U11 Cl26_a / x Cl26_a 0.709 U23 Cl6_b / U22 C8_b -0.824 x Cl26_a / x C28_a -0.748 U13 Cl26_a / z C28_a -0.708 U23 Cl26_a / U23 C28_a Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H28A 0.2361 0.2953 -0.2679 137 0.980 0.000 C28_a C26 H28A_a H28B 0.1351 0.3205 -0.1649 137 0.980 0.000 C28_a C26 H28A_a H28C 0.1550 0.1717 -0.2337 137 0.980 0.000 C28_a C26 H28A_a H8A 0.2597 0.4802 0.6399 137 0.980 0.000 C8_b C6 H8A_b H8B 0.3219 0.5089 0.5302 137 0.980 0.000 C8_b C6 H8A_b H8C 0.3756 0.3924 0.5738 137 0.980 0.000 C8_b C6 H8A_b H3 -0.2499 0.0725 0.2012 43 0.950 0.000 C3 C4 C2 H4 -0.2938 0.1926 0.3892 43 0.950 0.000 C4 C3 C5 H5 -0.0613 0.3594 0.5563 43 0.950 0.000 C5 C6 C4 H7A 0.4056 0.2667 0.3929 23 0.990 0.000 C7 N1 Si1 H7B 0.3606 0.3817 0.3427 23 0.990 0.000 C7 N1 Si1 H23 0.7978 0.3637 0.1422 43 0.950 0.000 C23 C24 C22 H24 0.7997 0.4169 -0.0303 43 0.950 0.000 C24 C23 C25 H25 0.5364 0.3778 -0.1856 43 0.950 0.000 C25 C26 C24 H27A 0.1381 0.1342 -0.0476 23 0.990 0.000 C27 N21 Si1 H27B 0.1508 0.2848 0.0456 23 0.990 0.000 C27 N21 Si1 H31A 0.3995 -0.0040 0.2131 137 0.980 0.000 C31 Si1 H31A H31B 0.3889 -0.0214 0.0720 137 0.980 0.000 C31 Si1 H31A H31C 0.2150 -0.0732 0.1035 137 0.980 0.000 C31 Si1 H31A 2008src0980 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C28_a 0.21237 0.26965 -0.20017 0.44717 0.02018 0.02987 0.02151 0.00865 0.00705 0.00649 0.02415 0.03917 0.00213 0.00192 0.00185 0.00602 0.00553 0.00453 0.00580 0.00393 0.00414 0.00401 0.00281 H28A_a 0.23606 0.29532 -0.26792 0.44717 0.03622 0.00602 0.00000 H28B_a 0.13514 0.32050 -0.16492 0.44717 0.03622 0.00602 0.00000 H28C_a 0.15499 0.17171 -0.23370 0.44717 0.03622 0.00602 0.00000 Cl26_a 0.17899 0.27654 -0.20440 0.55283 0.04441 0.07513 0.03839 0.03292 0.00246 0.00686 0.05289 0.01202 0.00064 0.00056 0.00049 0.00602 0.00189 0.00207 0.00143 0.00141 0.00115 0.00126 0.00135 C8_b 0.28324 0.43825 0.56041 0.61768 0.07237 0.04036 0.03676 -0.00847 0.02527 0.00459 0.05611 0.02683 0.00181 0.00149 0.00137 0.00620 0.00603 0.00715 0.00817 0.00417 0.00433 0.00355 0.00557 H8A_b 0.25974 0.48017 0.63985 0.61768 0.08417 0.00620 0.00000 H8B_b 0.32186 0.50887 0.53015 0.61768 0.08417 0.00620 0.00000 H8C_b 0.37559 0.39240 0.57379 0.61768 0.08417 0.00620 0.00000 Cl6_b 0.29286 0.46363 0.58391 0.38232 0.03931 0.03021 0.01830 0.00163 0.00707 0.00179 0.03277 0.01375 0.00053 0.00064 0.00060 0.00620 0.00134 0.00182 0.00174 0.00185 0.00096 0.00103 0.00088 C2 0.01391 0.16853 0.25724 1.00000 0.02981 0.02928 0.02767 0.01230 0.00939 0.00923 0.02833 0.00605 0.00031 0.00025 0.00023 0.00000 0.00123 0.00124 0.00128 0.00107 0.00104 0.00104 0.00053 C3 -0.15489 0.13997 0.26890 1.00000 0.02803 0.04142 0.03520 0.01592 0.01148 0.00704 0.03462 0.00682 0.00033 0.00028 0.00026 0.00000 0.00125 0.00146 0.00144 0.00122 0.00112 0.00113 0.00059 H3 -0.24990 0.07255 0.20118 1.00000 0.04155 0.00000 0.00000 C4 -0.18008 0.21140 0.38014 1.00000 0.03303 0.05121 0.04064 0.02428 0.01669 0.01707 0.03815 0.00715 0.00035 0.00030 0.00026 0.00000 0.00135 0.00164 0.00157 0.00136 0.00120 0.00126 0.00063 H4 -0.29377 0.19260 0.38924 1.00000 0.04577 0.00000 0.00000 C5 -0.04223 0.31079 0.47976 1.00000 0.04245 0.04310 0.03120 0.01466 0.01881 0.01773 0.03667 0.00697 0.00036 0.00028 0.00026 0.00000 0.00146 0.00153 0.00141 0.00123 0.00121 0.00128 0.00061 H5 -0.06134 0.35937 0.55632 1.00000 0.04400 0.00000 0.00000 C6 0.12137 0.33779 0.46618 1.00000 0.03988 0.02865 0.02311 0.01105 0.01074 0.01030 0.02996 0.00616 0.00034 0.00025 0.00022 0.00000 0.00134 0.00124 0.00125 0.00106 0.00106 0.00109 0.00054 C7 0.31760 0.28596 0.33251 1.00000 0.02816 0.03603 0.02514 0.01171 0.00981 0.00572 0.02995 0.00601 0.00031 0.00026 0.00023 0.00000 0.00122 0.00135 0.00126 0.00109 0.00102 0.00108 0.00054 H7A 0.40555 0.26670 0.39287 1.00000 0.03594 0.00000 0.00000 H7B 0.36060 0.38171 0.34270 1.00000 0.03594 0.00000 0.00000 C22 0.53002 0.29022 0.09163 1.00000 0.03295 0.02755 0.02572 0.00746 0.01191 0.00868 0.02894 0.00598 0.00032 0.00024 0.00023 0.00000 0.00127 0.00122 0.00127 0.00105 0.00106 0.00105 0.00053 C23 0.69037 0.34720 0.07971 1.00000 0.03280 0.03107 0.03857 0.01116 0.01601 0.00563 0.03429 0.00657 0.00034 0.00026 0.00026 0.00000 0.00132 0.00133 0.00151 0.00119 0.00117 0.00110 0.00059 H23 0.79778 0.36367 0.14223 1.00000 0.04115 0.00000 0.00000 C24 0.69095 0.37867 -0.02196 1.00000 0.04077 0.03756 0.04741 0.01688 0.02434 0.00843 0.04015 0.00708 0.00037 0.00027 0.00028 0.00000 0.00150 0.00148 0.00172 0.00134 0.00136 0.00125 0.00066 H24 0.79972 0.41685 -0.03028 1.00000 0.04818 0.00000 0.00000 C25 0.53435 0.35589 -0.11456 1.00000 0.05544 0.05113 0.04250 0.02299 0.02473 0.01297 0.04684 0.00785 0.00041 0.00032 0.00029 0.00000 0.00185 0.00178 0.00173 0.00150 0.00148 0.00151 0.00073 H25 0.53636 0.37777 -0.18559 1.00000 0.05621 0.00000 0.00000 C26 0.37782 0.30160 -0.10166 1.00000 0.04821 0.03846 0.03079 0.01436 0.01548 0.01180 0.03831 0.00692 0.00038 0.00028 0.00025 0.00000 0.00160 0.00148 0.00144 0.00123 0.00126 0.00128 0.00063 C27 0.21589 0.21508 0.02669 1.00000 0.02815 0.02971 0.02325 0.00568 0.00876 0.00731 0.02821 0.00594 0.00031 0.00025 0.00022 0.00000 0.00120 0.00125 0.00120 0.00103 0.00099 0.00103 0.00053 H27A 0.13812 0.13419 -0.04756 1.00000 0.03386 0.00000 0.00000 H27B 0.15079 0.28480 0.04559 1.00000 0.03386 0.00000 0.00000 C31 0.32707 -0.00303 0.13497 1.00000 0.03664 0.03914 0.04590 0.01751 0.01681 0.01357 0.03911 0.00702 0.00036 0.00027 0.00028 0.00000 0.00141 0.00150 0.00167 0.00133 0.00129 0.00124 0.00064 H31A 0.39946 -0.00404 0.21306 1.00000 0.05867 0.00000 0.00000 H31B 0.38893 -0.02141 0.07201 1.00000 0.05867 0.00000 0.00000 H31C 0.21498 -0.07324 0.10350 1.00000 0.05867 0.00000 0.00000 N1 0.14818 0.26451 0.35650 1.00000 0.02879 0.02881 0.02408 0.01117 0.00908 0.00708 0.02693 0.00484 0.00025 0.00020 0.00018 0.00000 0.00104 0.00106 0.00106 0.00089 0.00086 0.00088 0.00045 N21 0.37635 0.26968 0.00083 1.00000 0.03434 0.02615 0.02502 0.00790 0.01220 0.00794 0.02855 0.00493 0.00026 0.00020 0.00019 0.00000 0.00111 0.00103 0.00108 0.00089 0.00089 0.00089 0.00046 O2 0.05203 0.10772 0.15633 1.00000 0.02560 0.03701 0.02575 0.00702 0.00934 0.00199 0.03149 0.00402 0.00021 0.00017 0.00015 0.00000 0.00085 0.00097 0.00092 0.00078 0.00072 0.00074 0.00041 O22 0.51272 0.25426 0.18283 1.00000 0.02753 0.04059 0.02575 0.01367 0.00937 0.00573 0.03135 0.00416 0.00021 0.00018 0.00016 0.00000 0.00086 0.00100 0.00093 0.00080 0.00072 0.00077 0.00041 Si1 0.28511 0.16674 0.16595 1.00000 0.02529 0.03107 0.02449 0.00956 0.00867 0.00573 0.02737 0.00161 0.00008 0.00007 0.00006 0.00000 0.00035 0.00039 0.00038 0.00030 0.00028 0.00028 0.00021 Cl2 1.15523 0.51721 0.24367 1.00000 0.05233 0.03469 0.03755 0.01348 0.02514 0.01056 0.03979 0.00171 0.00009 0.00007 0.00006 0.00000 0.00043 0.00037 0.00040 0.00030 0.00032 0.00030 0.00023 Final Structure Factor Calculation for 2008src0980 in P-1 Total number of l.s. parameters = 214 Maximum vector length = 511 Memory required = 2656 / 25039 wR2 = 0.1558 before cycle 9 for 4196 data and 0 / 214 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 1.7105 1.6500 0.0605 0.0200 DFIX C6 Cl6_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 9. 30. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.010 0.051 0.000 0.000 rms deviation 0.000 0.042 0.000 0.000 0.000 0.000 0.000 0.008 0.011 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.034 for 43 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0880 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0560 for 3002 Fo > 4sig(Fo) and 0.0808 for all 4196 data wR2 = 0.1558, GooF = S = 1.036, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 16.19 for hydrogen atoms Principal mean square atomic displacements U 0.0312 0.0216 0.0197 C28_a 0.0846 0.0479 0.0261 Cl26_a 0.0920 0.0578 0.0186 C8_b 0.0473 0.0344 0.0166 Cl6_b 0.0305 0.0283 0.0261 C2 0.0429 0.0346 0.0264 C3 0.0528 0.0337 0.0279 C4 0.0475 0.0384 0.0240 C5 0.0401 0.0281 0.0218 C6 0.0386 0.0282 0.0230 C7 0.0341 0.0306 0.0222 C22 0.0444 0.0318 0.0267 C23 0.0552 0.0387 0.0266 C24 0.0591 0.0518 0.0296 C25 0.0485 0.0384 0.0281 C26 0.0351 0.0281 0.0214 C27 0.0465 0.0386 0.0322 C31 0.0299 0.0282 0.0227 N1 0.0354 0.0281 0.0221 N21 0.0460 0.0252 0.0232 O2 0.0430 0.0278 0.0233 O22 0.0333 0.0255 0.0233 Si1 0.0583 0.0347 0.0264 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.032 0.044 0.056 0.071 0.088 0.117 0.169 1.000 Number in group 451. 420. 412. 414. 406. 435. 403. 414. 421. 420. GooF 0.758 0.945 1.011 1.140 1.201 1.172 1.080 0.998 0.965 1.042 K 6.909 1.811 1.147 1.016 1.016 0.995 0.988 1.018 1.029 1.023 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 433. 406. 430. 424. 419. 412. 412. 425. 412. 423. GooF 0.892 0.974 0.948 0.961 0.947 1.010 0.904 0.970 1.104 1.511 K 1.077 1.081 1.046 1.028 1.032 1.022 1.044 1.034 1.021 1.014 R1 0.217 0.205 0.149 0.114 0.084 0.075 0.056 0.044 0.041 0.049 Recommended weighting scheme: WGHT 0.0881 0.0000 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 1 2 127.51 71.67 6.49 0.070 4.06 0 -2 1 710.76 1376.79 6.47 0.309 5.31 -3 0 5 36.23 16.38 6.21 0.034 1.96 -1 -3 4 155.23 289.46 6.03 0.142 2.55 -1 -1 1 146.83 39.92 5.79 0.053 5.90 8 -7 6 6.21 50.90 5.51 0.059 0.80 -1 -2 2 279.45 491.33 5.36 0.184 3.96 0 -2 3 1018.59 494.63 5.12 0.185 3.61 1 -1 1 610.24 1116.53 4.96 0.278 5.83 3 0 1 3.45 17.55 4.84 0.035 2.31 0 -2 2 756.39 282.15 4.62 0.140 4.60 -1 -2 3 1501.33 2343.33 4.58 0.403 3.42 3 0 4 35.68 64.60 4.35 0.067 1.60 -1 -4 7 227.62 150.64 4.32 0.102 1.61 1 -8 4 23.31 3.53 4.04 0.016 1.34 -2 0 5 4.62 12.63 4.01 0.030 2.17 -5 -7 6 21.02 5.92 4.00 0.020 1.01 -6 2 11 122.63 222.53 3.98 0.124 0.88 5 -9 3 16.09 4.53 3.97 0.018 1.03 2 2 1 39.90 62.18 3.87 0.066 2.36 -7 3 7 21.42 42.20 3.84 0.054 1.00 -1 6 2 11.56 2.36 3.81 0.013 1.48 -3 -3 13 22.07 43.98 3.64 0.055 0.91 2 -10 4 14.41 4.67 3.62 0.018 1.07 1 1 7 20.65 4.46 3.49 0.018 1.32 2 8 2 11.40 35.72 3.48 0.050 0.98 -1 0 3 391.83 545.78 3.48 0.194 3.68 -1 -4 3 136.73 190.23 3.43 0.115 2.36 -2 -3 13 10.81 29.33 3.36 0.045 0.91 -1 4 0 64.14 88.97 3.25 0.078 2.55 0 -3 1 21.14 9.42 3.21 0.026 3.54 -2 1 8 27.96 14.75 3.20 0.032 1.33 -5 -9 7 2.60 17.81 3.09 0.035 0.88 1 -4 2 61.96 45.50 3.05 0.056 2.62 -3 -10 13 70.48 134.97 3.03 0.097 0.78 5 2 7 12.47 33.99 3.03 0.049 0.86 7 -2 6 56.79 89.43 3.03 0.079 0.86 3 -2 12 3.62 124.44 3.02 0.093 0.81 5 -3 9 24.35 44.58 3.02 0.056 0.88 -2 -1 2 69.08 101.66 3.01 0.084 3.45 -4 8 2 17.39 7.52 2.99 0.023 1.12 -8 3 2 13.86 25.26 2.99 0.042 1.01 7 0 4 6.05 26.64 2.98 0.043 0.91 0 -1 4 581.06 775.20 2.96 0.232 2.86 -6 5 1 56.07 82.66 2.92 0.076 1.23 -6 4 1 41.93 22.89 2.91 0.040 1.29 -4 -6 6 15.27 5.58 2.91 0.020 1.20 -2 -12 7 38.75 82.17 2.91 0.075 0.83 -5 1 0 11.05 18.78 2.91 0.036 1.57 -3 3 5 48.14 66.33 2.89 0.068 1.58 Bond lengths and angles C28_a - Distance Angles C26 1.4617 (0.0146) H28A_a 0.9800 109.47 H28B_a 0.9800 109.47 109.47 H28C_a 0.9800 109.47 109.47 109.47 C28_a - C26 H28A_a H28B_a Cl26_a - Distance Angles C26 1.6993 (0.0056) Cl26_a - C8_b - Distance Angles C6 1.4761 (0.0110) H8A_b 0.9800 109.48 H8B_b 0.9800 109.46 109.47 H8C_b 0.9800 109.48 109.47 109.47 C8_b - C6 H8A_b H8B_b Cl6_b - Distance Angles C6 1.7105 (0.0058) Cl6_b - C2 - Distance Angles O2 1.2970 (0.0029) N1 1.3626 (0.0032) 116.87 (0.20) C3 1.4022 (0.0033) 123.74 (0.23) 119.38 (0.22) C2 - O2 N1 C3 - Distance Angles C4 1.3728 (0.0038) C2 1.4022 (0.0033) 118.67 (0.25) H3 0.9500 120.67 120.67 C3 - C4 C2 C4 - Distance Angles C3 1.3728 (0.0038) C5 1.3907 (0.0040) 121.21 (0.24) H4 0.9500 119.39 119.39 C4 - C3 C5 C5 - Distance Angles C6 1.3694 (0.0037) C4 1.3907 (0.0040) 119.22 (0.23) H5 0.9500 120.39 120.39 C5 - C6 C4 C6 - Distance Angles N1 1.3698 (0.0031) C5 1.3694 (0.0037) 119.80 (0.24) C8_b 1.4761 (0.0112) 112.90 (0.73) 127.27 (0.74) Cl6_b 1.7105 (0.0059) 119.35 (0.29) 120.84 (0.28) 6.84 (0.88) C6 - N1 C5 C8_b C7 - Distance Angles N1 1.4648 (0.0029) Si1 1.8942 (0.0025) 108.09 (0.16) H7A 0.9900 110.08 110.08 H7B 0.9900 110.08 110.08 108.42 C7 - N1 Si1 H7A C22 - Distance Angles O22 1.2924 (0.0029) N21 1.3754 (0.0032) 115.80 (0.21) C23 1.4009 (0.0034) 125.15 (0.23) 119.05 (0.23) C22 - O22 N21 C23 - Distance Angles C24 1.3576 (0.0039) C22 1.4009 (0.0034) 119.43 (0.25) H23 0.9500 120.29 120.29 C23 - C24 C22 C24 - Distance Angles C23 1.3576 (0.0039) C25 1.3970 (0.0042) 121.14 (0.26) H24 0.9500 119.43 119.43 C24 - C23 C25 C25 - Distance Angles C26 1.3701 (0.0040) C24 1.3970 (0.0042) 119.16 (0.27) H25 0.9500 120.42 120.42 C25 - C26 C24 C26 - Distance Angles C25 1.3701 (0.0040) N21 1.3709 (0.0033) 119.98 (0.26) C28_a 1.4617 (0.0146) 120.47 (0.96) 119.44 (0.96) Cl26_a 1.6993 (0.0056) 123.34 (0.30) 116.63 (0.28) 6.14 (0.98) C26 - C25 N21 C28_a C27 - Distance Angles N21 1.4770 (0.0030) Si1 1.8867 (0.0025) 107.86 (0.15) H27A 0.9900 110.13 110.13 H27B 0.9900 110.13 110.13 108.45 C27 - N21 Si1 H27A C31 - Distance Angles Si1 1.8570 (0.0026) 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 1.3626 (0.0032) C6 1.3698 (0.0031) 121.66 (0.20) C7 1.4648 (0.0029) 114.27 (0.19) 124.00 (0.21) N1 - C2 C6 N21 - Distance Angles C26 1.3709 (0.0033) C22 1.3754 (0.0032) 121.23 (0.21) C27 1.4770 (0.0030) 124.72 (0.21) 114.04 (0.20) N21 - C26 C22 O2 - Distance Angles C2 1.2970 (0.0029) Si1 1.8553 (0.0017) 114.76 (0.15) O2 - C2 O22 - Distance Angles C22 1.2924 (0.0029) Si1 1.8584 (0.0017) 115.48 (0.15) O22 - C22 Si1 - Distance Angles O2 1.8553 (0.0017) C31 1.8570 (0.0026) 94.97 (0.10) O22 1.8584 (0.0017) 170.57 (0.08) 94.43 (0.10) C27 1.8867 (0.0025) 90.62 (0.09) 117.38 (0.12) 85.69 (0.09) C7 1.8942 (0.0025) 86.00 (0.09) 120.22 (0.12) 88.65 (0.09) 122.39 (0.11) Si1 - O2 C31 O22 C27 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0802 for 4196 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.1763 0.0234 0.4603 [ 3.14 A from H28C ] Deepest hole -0.32 at 0.0770 0.5110 0.2040 [ 0.67 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2750 / 23319 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1763 -0.0234 -0.4603 1.00000 0.05 0.51 3.14 H28C 3.25 N1 3.38 H7A 3.43 C2 Q2 1 0.2990 0.0430 0.4875 1.00000 0.05 0.34 3.06 H7A 3.33 H4 3.44 H31A 3.47 H8C Q3 1 0.3079 0.0725 0.4662 1.00000 0.05 0.33 2.60 H7A 3.10 N1 3.14 H31A 3.16 H8C Q4 1 -0.2045 0.0415 -0.3954 1.00000 0.05 0.32 2.90 H28C 3.05 H31A 3.39 H31C 3.39 CL26 Q5 1 0.2503 0.0928 -0.4574 1.00000 0.05 0.32 2.61 H28A 2.84 H28C 3.09 H8C 3.14 C28 Q6 1 0.4619 -0.0126 0.1518 1.00000 0.05 0.31 0.96 H31B 0.97 H31A 1.10 C31 1.88 H31C Q7 1 -0.3838 0.0014 0.5204 1.00000 0.05 0.30 3.06 H4 3.18 H31A 3.37 H7A 3.62 C4 Q8 1 0.4999 0.4360 0.3807 1.00000 0.05 0.29 1.09 H7B 1.46 H8B 1.71 CL6 1.79 H8C Q9 1 -0.3438 0.2040 0.2975 1.00000 0.05 0.27 1.12 H4 1.43 C4 1.85 C3 1.87 O22 Q10 1 0.3975 0.1188 0.5627 1.00000 0.05 0.27 2.96 H8C 2.96 H7A 2.99 H28A 3.14 H25 Shortest distances between peaks (including symmetry equivalents) 2 3 0.47 2 7 0.91 2 5 0.91 1 2 0.94 1 4 0.96 1 5 0.98 2 10 1.03 1 3 1.08 3 5 1.09 3 10 1.09 3 7 1.12 5 10 1.13 2 4 1.15 3 4 1.25 7 10 1.31 4 7 1.46 1 7 1.73 5 7 1.74 4 5 1.77 1 10 1.81 7 7 1.83 4 10 2.18 6 9 2.40 7 10 2.41 2 7 2.66 8 8 2.71 3 7 2.74 8 9 2.99 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.97: 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 1.28: Structure factors and derivatives 2.55: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0980 finished at 13:54:33 Total CPU time: 5.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++