+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0289 started at 11:14:35 on 16-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0289 in P2(1)/n CELL 0.71073 10.2948 12.6066 14.3449 90.000 109.010 90.000 ZERR 4.00 0.0003 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 52 52 16 24 4 8 V = 1760.18 F(000) = 860.0 Mu = 0.48 mm-1 Cell Wt = 1681.06 Rho = 1.586 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.06 0.10 0.12 ACTA BOND $H WGHT 0.03040 2.11980 L.S. 8 TEMP -153.00 FVAR 0.52911 MOLE 1 C2 1 0.488014 0.350863 -0.236542 11.00000 0.01274 0.01644 = 0.02136 -0.00074 0.00640 -0.00012 AFIX 43 H2 2 0.583108 0.358647 -0.201055 11.00000 -1.20000 AFIX 0 C3 1 0.438972 0.364415 -0.336152 11.00000 0.01881 0.01382 = 0.01750 -0.00038 0.00974 -0.00136 C4 1 0.298593 0.356285 -0.390383 11.00000 0.02008 0.01517 = 0.01383 -0.00193 0.00528 -0.00080 AFIX 43 H4 2 0.266809 0.365721 -0.459877 11.00000 -1.20000 AFIX 0 C5 1 0.208949 0.334473 -0.340694 11.00000 0.01461 0.01723 = 0.01539 -0.00106 0.00307 -0.00033 AFIX 43 H5 2 0.113006 0.331426 -0.374983 11.00000 -1.20000 AFIX 0 C6 1 0.259512 0.316584 -0.238607 11.00000 0.01389 0.01259 = 0.01673 -0.00155 0.00605 0.00148 C7 1 0.438088 0.310472 -0.081057 11.00000 0.01607 0.02490 = 0.01063 0.00303 0.00335 0.00193 AFIX 23 H7A 2 0.467868 0.378580 -0.046308 11.00000 -1.20000 H7B 2 0.514860 0.259205 -0.058702 11.00000 -1.20000 AFIX 0 C22 1 0.128785 0.403378 0.139051 11.00000 0.01319 0.01821 = 0.01714 -0.00031 0.00555 0.00200 AFIX 43 H22 2 0.050016 0.444099 0.104868 11.00000 -1.20000 AFIX 0 C23 1 0.172827 0.396606 0.239589 11.00000 0.01519 0.02029 = 0.01438 -0.00166 0.00542 0.00037 C24 1 0.289443 0.337794 0.291426 11.00000 0.01866 0.02497 = 0.01180 0.00104 0.00328 0.00006 AFIX 43 H24 2 0.316960 0.332198 0.361207 11.00000 -1.20000 AFIX 0 C25 1 0.362960 0.288602 0.239906 11.00000 0.01802 0.02835 = 0.01509 0.00292 0.00215 0.00599 AFIX 43 H25 2 0.444092 0.250312 0.273805 11.00000 -1.20000 AFIX 0 C26 1 0.317603 0.295047 0.136076 11.00000 0.01245 0.01798 = 0.01495 -0.00008 0.00431 0.00058 C27 1 0.158802 0.349033 -0.019514 11.00000 0.01462 0.01921 = 0.00977 -0.00003 0.00259 0.00220 AFIX 23 H27A 2 0.163663 0.421419 -0.044936 11.00000 -1.20000 H27B 2 0.063269 0.322973 -0.047901 11.00000 -1.20000 AFIX 0 C31 1 0.251343 0.112925 -0.071246 11.00000 0.03177 0.01641 = 0.02199 -0.00077 0.01320 -0.00072 AFIX 137 H31A 2 0.152959 0.099278 -0.102433 11.00000 -1.50000 H31B 2 0.283554 0.077875 -0.006788 11.00000 -1.50000 H31C 2 0.301897 0.085039 -0.113186 11.00000 -1.50000 AFIX 0 N1 3 0.397150 0.325925 -0.189448 11.00000 0.01274 0.01705 = 0.01278 -0.00077 0.00359 0.00019 N3 3 0.537017 0.386606 -0.387843 11.00000 0.02069 0.02235 = 0.01969 -0.00107 0.01009 -0.00232 N21 3 0.200272 0.350562 0.089333 11.00000 0.01350 0.01781 = 0.01180 0.00023 0.00407 0.00125 N23 3 0.092464 0.451590 0.292349 11.00000 0.02040 0.02518 = 0.01504 -0.00337 0.00660 -0.00030 O3A 4 0.657117 0.404716 -0.338661 11.00000 0.02019 0.04165 = 0.02697 0.00214 0.01107 -0.00554 O3B 4 0.494325 0.384845 -0.478084 11.00000 0.03474 0.05545 = 0.01629 -0.00286 0.01262 -0.01509 O6 4 0.184393 0.290071 -0.186596 11.00000 0.01260 0.02117 = 0.01424 -0.00020 0.00555 -0.00215 O23A 4 0.106443 0.420862 0.376761 11.00000 0.03273 0.03842 = 0.01626 0.00064 0.01186 0.00464 O23B 4 0.017182 0.523743 0.250431 11.00000 0.03037 0.03531 = 0.02354 0.00141 0.00976 0.01593 O26 4 0.377303 0.250564 0.080472 11.00000 0.01678 0.02542 = 0.01408 0.00158 0.00578 0.00649 SI1 5 0.280851 0.257612 -0.054864 11.00000 0.01392 0.01625 = 0.01294 0.00075 0.00523 0.00140 CL2 6 0.200377 0.629731 0.031601 11.00000 0.01803 0.02621 = 0.02344 -0.00405 0.00597 -0.00311 MOLE 2 CL1 6 0.688487 0.428931 0.146675 11.00000 0.05401 0.02201 = 0.02878 -0.00258 0.01896 -0.00177 HKLF 4 Covalent radii and connectivity table for 2009src0289 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C2 - N1 C3 C3 - C2 C4 N3 C4 - C5 C3 C5 - C4 C6 C6 - O6 N1 C5 C7 - N1 Si1 C22 - N21 C23 C23 - C22 C24 N23 C24 - C25 C23 C25 - C24 C26 C26 - O26 N21 C25 C27 - N21 Si1 C31 - Si1 N1 - C2 C6 C7 N3 - O3B O3A C3 N21 - C22 C26 C27 N23 - O23B O23A C23 O3A - N3 O3B - N3 O6 - C6 Si1 O23A - N23 O23B - N23 O26 - C26 Si1 Si1 - C31 O6 O26 C27 C7 Cl2 - no bonds found Cl1 - no bonds found 30941 Reflections read, of which 882 rejected -13 =< h =< 13, -16 =< k =< 16, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -1 3 6 0.17 0.15 8 1.93 1 Inconsistent equivalents 4039 Unique reflections, of which 0 suppressed R(int) = 0.0687 R(sigma) = 0.0505 Friedel opposites merged Maximum memory for data reduction = 2085 / 40382 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 = 2711 / 294669 wR2 = 0.0987 before cycle 1 for 4039 data and 236 / 236 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 -0.007 OSF Mean shift/su = 0.002 Maximum = 0.013 for U23 Cl2 Max. shift = 0.000 A for H31B Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 2 for 4039 data and 236 / 236 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 -0.006 OSF Mean shift/su = 0.001 Maximum = -0.006 for OSF Max. shift = 0.000 A for H31C Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 3 for 4039 data and 236 / 236 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for tors H31A Max. shift = 0.000 A for H31C Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 4 for 4039 data and 236 / 236 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H31A Max. shift = 0.000 A for H31C Max. dU = 0.000 for Cl1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 5 for 4039 data and 236 / 236 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H31A Max. shift = 0.000 A for H31C Max. dU = 0.000 for C6 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 6 for 4039 data and 236 / 236 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H31C Max. dU = 0.000 for C31 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 7 for 4039 data and 236 / 236 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H31A Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2711 / 294669 wR2 = 0.0987 before cycle 8 for 4039 data and 236 / 236 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52910 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H31A Max. dU = 0.000 for C5 Largest correlation matrix elements 0.521 U13 Cl1 / U11 Cl1 0.512 U13 N3 / U11 N3 0.514 U13 O3A / U11 O3A 0.511 U13 C31 / U11 C31 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5831 0.3586 -0.2011 43 0.950 0.000 C2 N1 C3 H4 0.2668 0.3657 -0.4599 43 0.950 0.000 C4 C5 C3 H5 0.1130 0.3314 -0.3750 43 0.950 0.000 C5 C4 C6 H7A 0.4679 0.3786 -0.0463 23 0.990 0.000 C7 N1 Si1 H7B 0.5149 0.2592 -0.0587 23 0.990 0.000 C7 N1 Si1 H22 0.0500 0.4441 0.1049 43 0.950 0.000 C22 N21 C23 H24 0.3170 0.3322 0.3612 43 0.950 0.000 C24 C25 C23 H25 0.4441 0.2503 0.2738 43 0.950 0.000 C25 C24 C26 H27A 0.1637 0.4214 -0.0449 23 0.990 0.000 C27 N21 Si1 H27B 0.0633 0.3230 -0.0479 23 0.990 0.000 C27 N21 Si1 H31A 0.1530 0.0993 -0.1024 137 0.980 0.000 C31 Si1 H31A H31B 0.2835 0.0779 -0.0068 137 0.980 0.000 C31 Si1 H31A H31C 0.3019 0.0850 -0.1132 137 0.980 0.000 C31 Si1 H31A 2009src0289 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.48801 0.35086 -0.23654 1.00000 0.01273 0.01644 0.02135 -0.00074 0.00640 -0.00012 0.01663 0.00446 0.00023 0.00017 0.00016 0.00000 0.00111 0.00108 0.00114 0.00088 0.00091 0.00085 0.00046 H2 0.58311 0.35865 -0.20106 1.00000 0.01996 0.00000 0.00000 C3 0.43897 0.36441 -0.33615 1.00000 0.01881 0.01382 0.01749 -0.00037 0.00974 -0.00136 0.01578 0.00442 0.00023 0.00017 0.00016 0.00000 0.00116 0.00103 0.00107 0.00085 0.00091 0.00087 0.00045 C4 0.29859 0.35628 -0.39038 1.00000 0.02008 0.01516 0.01383 -0.00193 0.00528 -0.00080 0.01641 0.00436 0.00023 0.00017 0.00016 0.00000 0.00119 0.00106 0.00102 0.00084 0.00089 0.00088 0.00045 H4 0.26681 0.36572 -0.45988 1.00000 0.01970 0.00000 0.00000 C5 0.20895 0.33447 -0.34069 1.00000 0.01461 0.01723 0.01539 -0.00106 0.00307 -0.00033 0.01618 0.00438 0.00023 0.00017 0.00016 0.00000 0.00113 0.00109 0.00105 0.00086 0.00087 0.00087 0.00045 H5 0.11301 0.33143 -0.37498 1.00000 0.01942 0.00000 0.00000 C6 0.25951 0.31658 -0.23861 1.00000 0.01389 0.01259 0.01673 -0.00155 0.00605 0.00148 0.01414 0.00427 0.00022 0.00017 0.00016 0.00000 0.00109 0.00101 0.00104 0.00083 0.00086 0.00083 0.00043 C7 0.43809 0.31047 -0.08106 1.00000 0.01607 0.02490 0.01062 0.00303 0.00334 0.00193 0.01744 0.00451 0.00023 0.00019 0.00015 0.00000 0.00114 0.00119 0.00100 0.00089 0.00085 0.00093 0.00046 H7A 0.46787 0.37858 -0.04631 1.00000 0.02093 0.00000 0.00000 H7B 0.51486 0.25920 -0.05870 1.00000 0.02093 0.00000 0.00000 C22 0.12879 0.40338 0.13905 1.00000 0.01319 0.01821 0.01714 -0.00031 0.00554 0.00200 0.01603 0.00439 0.00023 0.00017 0.00016 0.00000 0.00112 0.00110 0.00107 0.00087 0.00088 0.00086 0.00045 H22 0.05002 0.44410 0.10487 1.00000 0.01924 0.00000 0.00000 C23 0.17283 0.39661 0.23959 1.00000 0.01519 0.02029 0.01438 -0.00166 0.00542 0.00037 0.01647 0.00442 0.00023 0.00018 0.00016 0.00000 0.00114 0.00112 0.00103 0.00087 0.00087 0.00088 0.00045 C24 0.28944 0.33779 0.29143 1.00000 0.01866 0.02497 0.01180 0.00104 0.00328 0.00006 0.01888 0.00454 0.00024 0.00019 0.00016 0.00000 0.00119 0.00120 0.00102 0.00089 0.00087 0.00095 0.00047 H24 0.31696 0.33220 0.36121 1.00000 0.02266 0.00000 0.00000 C25 0.36296 0.28860 0.23991 1.00000 0.01802 0.02835 0.01509 0.00292 0.00215 0.00599 0.02127 0.00477 0.00025 0.00019 0.00016 0.00000 0.00120 0.00130 0.00108 0.00094 0.00092 0.00098 0.00050 H25 0.44409 0.25031 0.27380 1.00000 0.02553 0.00000 0.00000 C26 0.31760 0.29505 0.13608 1.00000 0.01245 0.01798 0.01495 -0.00007 0.00431 0.00058 0.01516 0.00431 0.00022 0.00017 0.00015 0.00000 0.00109 0.00108 0.00104 0.00085 0.00086 0.00085 0.00044 C27 0.15880 0.34903 -0.01951 1.00000 0.01462 0.01921 0.00977 -0.00003 0.00259 0.00220 0.01487 0.00429 0.00022 0.00018 0.00015 0.00000 0.00110 0.00109 0.00098 0.00083 0.00082 0.00087 0.00044 H27A 0.16366 0.42142 -0.04494 1.00000 0.01784 0.00000 0.00000 H27B 0.06327 0.32297 -0.04790 1.00000 0.01784 0.00000 0.00000 C31 0.25134 0.11292 -0.07125 1.00000 0.03177 0.01641 0.02199 -0.00077 0.01320 -0.00072 0.02231 0.00492 0.00027 0.00018 0.00017 0.00000 0.00143 0.00113 0.00119 0.00094 0.00106 0.00099 0.00051 H31A 0.15296 0.09928 -0.10244 1.00000 0.03346 0.00000 0.00000 H31B 0.28354 0.07788 -0.00679 1.00000 0.03346 0.00000 0.00000 H31C 0.30191 0.08504 -0.11318 1.00000 0.03346 0.00000 0.00000 N1 0.39715 0.32593 -0.18945 1.00000 0.01273 0.01705 0.01278 -0.00077 0.00359 0.00019 0.01433 0.00355 0.00018 0.00014 0.00013 0.00000 0.00093 0.00092 0.00086 0.00072 0.00072 0.00072 0.00037 N3 0.53702 0.38661 -0.38784 1.00000 0.02069 0.02235 0.01969 -0.00107 0.01009 -0.00232 0.02005 0.00395 0.00021 0.00016 0.00014 0.00000 0.00111 0.00102 0.00099 0.00081 0.00085 0.00082 0.00042 N21 0.20027 0.35056 0.08933 1.00000 0.01350 0.01781 0.01179 0.00023 0.00407 0.00125 0.01438 0.00359 0.00018 0.00014 0.00013 0.00000 0.00093 0.00093 0.00085 0.00071 0.00071 0.00073 0.00038 N23 0.09246 0.45159 0.29235 1.00000 0.02039 0.02518 0.01504 -0.00336 0.00660 -0.00030 0.02000 0.00380 0.00020 0.00016 0.00013 0.00000 0.00106 0.00107 0.00093 0.00081 0.00079 0.00084 0.00042 O3A 0.65712 0.40472 -0.33866 1.00000 0.02019 0.04165 0.02697 0.00215 0.01107 -0.00554 0.02878 0.00357 0.00018 0.00015 0.00013 0.00000 0.00098 0.00109 0.00094 0.00080 0.00078 0.00079 0.00041 O3B 0.49433 0.38485 -0.47808 1.00000 0.03473 0.05545 0.01629 -0.00286 0.01262 -0.01509 0.03445 0.00361 0.00019 0.00017 0.00012 0.00000 0.00110 0.00129 0.00087 0.00084 0.00079 0.00093 0.00047 O6 0.18439 0.29007 -0.18660 1.00000 0.01260 0.02117 0.01424 -0.00020 0.00555 -0.00215 0.01572 0.00296 0.00015 0.00012 0.00011 0.00000 0.00077 0.00081 0.00073 0.00061 0.00060 0.00062 0.00033 O23A 0.10644 0.42086 0.37676 1.00000 0.03273 0.03842 0.01626 0.00064 0.01186 0.00465 0.02819 0.00361 0.00018 0.00015 0.00012 0.00000 0.00104 0.00106 0.00083 0.00074 0.00075 0.00081 0.00041 O23B 0.01718 0.52374 0.25043 1.00000 0.03037 0.03531 0.02354 0.00141 0.00976 0.01593 0.02950 0.00372 0.00018 0.00015 0.00012 0.00000 0.00103 0.00105 0.00090 0.00077 0.00077 0.00083 0.00042 O26 0.37730 0.25056 0.08047 1.00000 0.01678 0.02541 0.01408 0.00158 0.00578 0.00649 0.01857 0.00313 0.00016 0.00013 0.00011 0.00000 0.00080 0.00086 0.00074 0.00065 0.00063 0.00067 0.00034 Si1 0.28085 0.25761 -0.05486 1.00000 0.01392 0.01625 0.01294 0.00075 0.00523 0.00140 0.01416 0.00120 0.00006 0.00005 0.00004 0.00000 0.00030 0.00030 0.00028 0.00023 0.00023 0.00024 0.00014 Cl2 0.20038 0.62973 0.03160 1.00000 0.01803 0.02621 0.02344 -0.00405 0.00597 -0.00311 0.02275 0.00112 0.00006 0.00005 0.00004 0.00000 0.00030 0.00031 0.00029 0.00023 0.00023 0.00023 0.00014 Cl1 0.68849 0.42893 0.14668 1.00000 0.05400 0.02200 0.02878 -0.00258 0.01896 -0.00177 0.03360 0.00138 0.00008 0.00005 0.00005 0.00000 0.00045 0.00032 0.00033 0.00025 0.00031 0.00029 0.00017 Final Structure Factor Calculation for 2009src0289 in P2(1)/n Total number of l.s. parameters = 236 Maximum vector length = 511 Memory required = 2475 / 25039 wR2 = 0.0987 before cycle 9 for 4039 data and 0 / 236 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0304 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0445 for 3273 Fo > 4sig(Fo) and 0.0622 for all 4039 data wR2 = 0.0987, GooF = S = 1.021, Restrained GooF = 1.021 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0215 0.0163 0.0121 C2 0.0213 0.0140 0.0121 C3 0.0204 0.0164 0.0124 C4 0.0183 0.0169 0.0134 C5 0.0172 0.0148 0.0103 C6 0.0256 0.0167 0.0100 C7 0.0190 0.0171 0.0120 C22 0.0208 0.0154 0.0132 C23 0.0251 0.0199 0.0117 C24 0.0311 0.0205 0.0122 C25 0.0181 0.0151 0.0124 C26 0.0204 0.0145 0.0097 C27 0.0325 0.0182 0.0163 C31 0.0173 0.0134 0.0123 N1 0.0248 0.0205 0.0148 N3 0.0182 0.0132 0.0118 N21 0.0262 0.0204 0.0134 N23 0.0435 0.0275 0.0153 O3A 0.0634 0.0271 0.0128 O3B 0.0217 0.0145 0.0110 O6 0.0410 0.0303 0.0133 O23A 0.0493 0.0234 0.0158 O23B 0.0289 0.0140 0.0128 O26 0.0170 0.0135 0.0120 Si1 0.0291 0.0223 0.0168 Cl2 0.0542 0.0258 0.0208 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.029 0.043 0.057 0.073 0.093 0.119 0.149 0.208 1.000 Number in group 425. 391. 414. 392. 399. 408. 408. 401. 394. 407. GooF 1.026 0.990 1.101 1.038 1.020 1.001 0.989 1.022 0.999 1.013 K 8.371 1.435 1.071 1.056 1.016 1.001 0.996 1.011 1.006 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 412. 403. 398. 409. 402. 403. 400. 401. 406. 405. GooF 0.973 0.952 0.946 0.943 0.920 0.918 0.901 0.876 1.092 1.521 K 1.007 1.032 1.032 1.014 1.064 1.002 1.014 1.007 1.008 0.994 R1 0.136 0.111 0.103 0.085 0.089 0.049 0.043 0.035 0.035 0.033 Recommended weighting scheme: WGHT 0.0304 2.1176 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) -5 0 5 164.84 57.74 5.81 0.040 1.90 5 1 1 974.21 716.70 4.90 0.142 1.82 -3 1 7 566.79 399.55 4.60 0.106 1.95 4 1 0 108.65 35.41 4.53 0.032 2.39 -2 4 6 779.47 562.35 4.38 0.126 1.89 -4 4 6 1080.46 834.13 4.35 0.154 1.70 1 2 0 4871.14 5762.60 4.12 0.404 5.29 0 0 2 657.99 892.74 4.07 0.159 6.78 5 0 1 12273.02 10350.23 3.97 0.541 1.84 0 7 2 562.34 419.21 3.89 0.109 1.74 -1 2 8 4453.70 3822.71 3.77 0.329 1.70 -4 3 4 773.14 603.76 3.73 0.131 2.07 -9 5 14 185.10 5.53 3.71 0.013 0.83 9 6 2 45.39 120.67 3.55 0.058 0.92 1 0 7 8679.52 7470.59 3.52 0.460 1.79 -5 7 4 163.92 97.20 3.48 0.052 1.34 -2 2 5 162.89 245.14 3.46 0.083 2.55 2 6 3 73.88 31.15 3.42 0.030 1.70 4 2 5 143.10 78.55 3.31 0.047 1.53 -2 6 1 322.57 231.04 3.26 0.081 1.95 1 4 12 143.96 217.26 3.15 0.078 1.02 -1 2 5 38.55 81.44 3.13 0.048 2.61 0 2 5 4041.62 4612.06 3.13 0.361 2.49 -4 2 3 3359.19 3822.96 3.12 0.329 2.33 -6 2 7 289.83 387.53 3.10 0.105 1.47 -2 0 2 25.81 0.13 3.07 0.002 4.76 -2 7 14 127.70 52.86 3.02 0.039 0.88 -3 6 11 479.10 345.25 3.00 0.099 1.11 -4 6 2 45.53 15.13 2.99 0.021 1.63 -2 14 8 231.76 135.70 2.97 0.062 0.80 -3 5 2 640.80 783.04 2.92 0.149 2.02 -3 6 5 260.00 189.42 2.92 0.073 1.61 -11 7 1 246.27 98.77 2.91 0.053 0.81 0 1 11 587.08 721.05 2.89 0.143 1.23 3 3 1 81.84 42.96 2.88 0.035 2.41 -12 4 10 291.75 150.59 2.86 0.065 0.80 4 3 0 1482.38 1273.94 2.85 0.190 2.11 -5 1 7 1046.71 886.98 2.83 0.159 1.66 4 3 1 2513.18 2206.07 2.83 0.250 2.00 0 1 7 71.35 117.49 2.82 0.058 1.92 -4 1 5 193.37 137.01 2.81 0.062 2.17 8 5 5 329.66 453.87 2.81 0.113 0.93 1 3 1 666.79 549.97 2.79 0.125 3.59 1 1 13 223.69 308.76 2.78 0.094 1.00 -8 4 8 50.70 94.79 2.74 0.052 1.11 4 4 0 628.38 513.31 2.73 0.121 1.93 -1 11 1 28.66 1.12 2.73 0.006 1.14 -1 1 4 15591.08 17225.06 2.71 0.699 3.45 -3 0 7 128.22 80.89 2.69 0.048 1.97 1 2 8 999.29 1169.72 2.68 0.182 1.54 Bond lengths and angles C2 - Distance Angles N1 1.3572 (0.0027) C3 1.3623 (0.0030) 118.11 (0.20) H2 0.9500 120.95 120.95 C2 - N1 C3 C3 - Distance Angles C2 1.3623 (0.0030) C4 1.4042 (0.0032) 122.33 (0.20) N3 1.4610 (0.0027) 118.37 (0.20) 119.30 (0.19) C3 - C2 C4 C4 - Distance Angles C5 1.3652 (0.0030) C3 1.4042 (0.0032) 118.31 (0.20) H4 0.9500 120.85 120.85 C4 - C5 C3 C5 - Distance Angles C4 1.3652 (0.0030) C6 1.4035 (0.0030) 119.54 (0.20) H5 0.9500 120.23 120.23 C5 - C4 C6 C6 - Distance Angles O6 1.2815 (0.0025) N1 1.3667 (0.0028) 116.29 (0.19) C5 1.4035 (0.0030) 124.08 (0.20) 119.63 (0.19) C6 - O6 N1 C7 - Distance Angles N1 1.4853 (0.0026) Si1 1.8978 (0.0022) 106.49 (0.14) H7A 0.9900 110.43 110.43 H7B 0.9900 110.43 110.43 108.63 C7 - N1 Si1 H7A C22 - Distance Angles N21 1.3548 (0.0027) C23 1.3663 (0.0030) 118.33 (0.20) H22 0.9500 120.83 120.83 C22 - N21 C23 C23 - Distance Angles C22 1.3663 (0.0030) C24 1.4009 (0.0032) 121.72 (0.20) N23 1.4648 (0.0028) 117.82 (0.20) 120.45 (0.19) C23 - C22 C24 C24 - Distance Angles C25 1.3667 (0.0032) C23 1.4009 (0.0032) 118.87 (0.20) H24 0.9500 120.56 120.56 C24 - C25 C23 C25 - Distance Angles C24 1.3667 (0.0032) C26 1.4107 (0.0030) 119.58 (0.21) H25 0.9500 120.21 120.21 C25 - C24 C26 C26 - Distance Angles O26 1.2837 (0.0025) N21 1.3678 (0.0028) 116.36 (0.18) C25 1.4107 (0.0030) 124.76 (0.20) 118.87 (0.19) C26 - O26 N21 C27 - Distance Angles N21 1.4786 (0.0026) Si1 1.8919 (0.0022) 107.61 (0.14) H27A 0.9900 110.19 110.19 H27B 0.9900 110.19 110.19 108.48 C27 - N21 Si1 H27A C31 - Distance Angles Si1 1.8515 (0.0023) 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 1.3572 (0.0027) C6 1.3667 (0.0028) 122.00 (0.18) C7 1.4853 (0.0026) 123.02 (0.18) 114.95 (0.17) N1 - C2 C6 N3 - Distance Angles O3B 1.2242 (0.0025) O3A 1.2289 (0.0026) 123.91 (0.19) C3 1.4610 (0.0027) 117.63 (0.19) 118.45 (0.18) N3 - O3B O3A N21 - Distance Angles C22 1.3548 (0.0027) C26 1.3678 (0.0028) 122.53 (0.18) C27 1.4786 (0.0026) 122.87 (0.18) 114.59 (0.17) N21 - C22 C26 N23 - Distance Angles O23B 1.2190 (0.0026) O23A 1.2343 (0.0024) 124.77 (0.19) C23 1.4648 (0.0028) 118.27 (0.18) 116.96 (0.19) N23 - O23B O23A O3A - Distance Angles N3 1.2289 (0.0026) O3A - O3B - Distance Angles N3 1.2242 (0.0025) O3B - O6 - Distance Angles C6 1.2815 (0.0025) Si1 1.8713 (0.0016) 115.00 (0.14) O6 - C6 O23A - Distance Angles N23 1.2343 (0.0024) O23A - O23B - Distance Angles N23 1.2190 (0.0026) O23B - O26 - Distance Angles C26 1.2837 (0.0025) Si1 1.8727 (0.0016) 115.08 (0.14) O26 - C26 Si1 - Distance Angles C31 1.8515 (0.0023) O6 1.8713 (0.0016) 94.36 (0.09) O26 1.8727 (0.0016) 95.42 (0.09) 170.06 (0.08) C27 1.8919 (0.0022) 122.57 (0.11) 87.54 (0.08) 85.71 (0.08) C7 1.8978 (0.0022) 115.85 (0.11) 85.96 (0.08) 91.35 (0.08) 121.53 (0.10) Si1 - C31 O6 O26 C27 FMAP and GRID set by program FMAP 2 3 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0613 for 4039 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.52 at 0.7226 0.4015 0.0728 [ 1.27 A from CL1 ] Deepest hole -0.35 at 0.6200 0.4209 0.1088 [ 0.74 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2565 / 22384 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7226 0.4015 0.0728 1.00000 0.05 0.52 1.27 CL1 1.95 CL2 2.61 H27A 2.64 H7A Q2 1 0.3646 0.2809 -0.0781 1.00000 0.05 0.31 0.86 C7 1.06 SI1 1.51 H7B 1.59 H7A Q3 1 0.2678 0.1791 -0.0779 1.00000 0.05 0.30 0.86 C31 1.04 SI1 1.38 H31C 1.50 H31A Q4 1 0.7775 0.4249 0.1757 1.00000 0.05 0.30 0.88 CL1 2.66 O23B 2.90 H27A 2.96 H31C Q5 1 0.1358 0.4175 0.2564 1.00000 0.05 0.30 0.58 C23 0.89 N23 1.67 C22 1.80 O23B Q6 1 0.2140 0.3207 -0.0369 1.00000 0.05 0.29 0.78 C27 1.14 SI1 1.36 H27A 1.51 H27B Q7 1 0.4758 0.3765 -0.3555 1.00000 0.05 0.28 0.56 C3 0.91 N3 1.70 C2 1.75 C4 Q8 1 0.3515 0.0679 -0.0476 1.00000 0.05 0.28 0.94 H31C 1.06 H31B 1.13 C31 1.98 H31A Q9 1 0.2072 0.0715 -0.0135 1.00000 0.05 0.27 0.76 H31B 1.19 C31 1.26 H31A 1.98 H31C Q10 1 0.2412 0.5420 -0.0478 1.00000 0.05 0.26 1.72 H27A 1.73 CL2 1.83 CL1 2.65 C27 Shortest distances between peaks (including symmetry equivalents) 1 10 0.93 1 4 1.43 2 3 1.63 3 8 1.63 8 9 1.71 4 10 1.83 3 9 1.86 2 6 1.90 3 6 2.01 2 8 2.73 6 10 2.81 Time profile in seconds ----------------------- 0.00: 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. 1.42: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.72: Structure factors and derivatives 3.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.33: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0289 finished at 11:14:42 Total CPU time: 6.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++