+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0244p21c started at 10:58:27 on 16-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0244p21c in P2(1)/c CELL 0.71073 8.8936 22.0632 7.8946 90.000 106.318 90.000 ZERR 4.00 0.0002 0.0006 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 52 68 8 12 4 4 V = 1486.69 F(000) = 656.0 Mu = 0.35 mm-1 Cell Wt = 1251.30 Rho = 1.398 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O1W Cl1 EQIV_$1 -x+2, -y, -z+2 HTAB O1W Cl1_$1 FMAP 2 DFIX 0.85 0.02 O1W H1W O1W H2W DANG 1.37 0.02 H1W H2W PLAN 10 SIZE 0.07 0.13 0.28 ACTA BOND $H WGHT 0.00000 2.87500 L.S. 4 TEMP -153.00 FVAR 0.50248 C2 1 0.299893 0.008235 0.607644 11.00000 0.02060 0.01829 = 0.02280 -0.00068 0.00529 -0.00213 AFIX 43 H2 2 0.279654 -0.019554 0.690511 11.00000 -1.20000 AFIX 0 C3 1 0.238673 -0.001900 0.430955 11.00000 0.02273 0.02577 = 0.02558 -0.00507 0.00394 -0.00282 AFIX 43 H3 2 0.175417 -0.036519 0.389899 11.00000 -1.20000 AFIX 0 C4 1 0.270738 0.039680 0.310941 11.00000 0.02543 0.02988 = 0.01661 -0.00451 0.00261 0.00326 AFIX 43 H4 2 0.228798 0.033049 0.187758 11.00000 -1.20000 AFIX 0 C5 1 0.361823 0.089701 0.369498 11.00000 0.01944 0.02744 = 0.01659 0.00247 0.00554 0.00211 AFIX 43 H5 2 0.384840 0.117277 0.287783 11.00000 -1.20000 AFIX 0 C6 1 0.420646 0.099665 0.551679 11.00000 0.01251 0.01934 = 0.01762 0.00073 0.00356 0.00180 C7 1 0.458819 0.072791 0.853543 11.00000 0.01750 0.02065 = 0.01361 -0.00055 0.00382 -0.00136 AFIX 23 H7A 2 0.548414 0.045637 0.906040 11.00000 -1.20000 H7B 2 0.379724 0.067620 0.919076 11.00000 -1.20000 AFIX 0 C22 1 0.968831 0.188947 1.166441 11.00000 0.01933 0.01686 = 0.02459 -0.00142 0.00657 -0.00222 AFIX 43 H22 2 1.032700 0.199295 1.092452 11.00000 -1.20000 AFIX 0 C23 1 1.033363 0.185496 1.344733 11.00000 0.01859 0.02000 = 0.02743 -0.00221 0.00042 -0.00022 AFIX 43 H23 2 1.141566 0.193695 1.395375 11.00000 -1.20000 AFIX 0 C24 1 0.937813 0.169671 1.452434 11.00000 0.02971 0.02086 = 0.01871 0.00018 0.00203 -0.00003 AFIX 43 H24 2 0.981747 0.166817 1.576609 11.00000 -1.20000 AFIX 0 C25 1 0.781119 0.158304 1.378999 11.00000 0.02963 0.01707 = 0.01810 0.00134 0.00584 -0.00236 AFIX 43 H25 2 0.715984 0.148264 1.451831 11.00000 -1.20000 AFIX 0 C26 1 0.718237 0.161710 1.194588 11.00000 0.01969 0.01163 = 0.02076 0.00056 0.00602 0.00025 C27 1 0.738926 0.176127 0.902005 11.00000 0.02028 0.01911 = 0.01489 0.00024 0.00542 -0.00177 AFIX 23 H27A 2 0.792180 0.146175 0.845356 11.00000 -1.20000 H27B 2 0.746023 0.216438 0.849704 11.00000 -1.20000 AFIX 0 C31 1 0.380203 0.216226 0.842068 11.00000 0.02101 0.02363 = 0.02394 0.00032 0.00560 0.00461 AFIX 137 H31A 2 0.280568 0.199329 0.850213 11.00000 -1.50000 H31B 2 0.364480 0.235986 0.727229 11.00000 -1.50000 H31C 2 0.418545 0.246024 0.936395 11.00000 -1.50000 AFIX 0 N1 3 0.389979 0.058166 0.665212 11.00000 0.01558 0.01724 = 0.01638 -0.00015 0.00426 0.00129 N21 3 0.813910 0.177683 1.094111 11.00000 0.01699 0.01440 = 0.01806 -0.00029 0.00450 -0.00164 O6 4 0.503654 0.146416 0.623102 11.00000 0.02247 0.01994 = 0.01583 0.00099 0.00592 -0.00374 O26 4 0.573487 0.150712 1.111377 11.00000 0.01892 0.02621 = 0.01491 -0.00086 0.00537 -0.00343 SI1 5 0.526512 0.154178 0.865560 11.00000 0.01563 0.01623 = 0.01524 -0.00037 0.00461 -0.00054 CL1 6 1.072344 0.096633 0.867000 11.00000 0.02084 0.02134 = 0.02250 0.00327 0.00708 0.00137 MOLE 2 O1W 4 0.848108 0.043020 1.086521 11.00000 0.03062 0.02072 = 0.03347 0.00349 0.01682 0.00068 H1W 2 0.906201 0.057213 1.034503 11.00000 0.04221 H2W 2 0.875833 0.004534 1.110339 11.00000 0.05668 HKLF 4 Covalent radii and connectivity table for 2009src0244p21c 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 C4 - C5 C3 C5 - C4 C6 C6 - O6 N1 C5 C7 - N1 Si1 C22 - N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - O26 N21 C25 C27 - N21 Si1 C31 - Si1 N1 - C6 C2 C7 N21 - C22 C26 C27 O6 - C6 Si1 O26 - C26 Si1 Si1 - C31 O26 O6 C7 C27 Cl1 - no bonds found O1W - no bonds found Operators for generating equivalent atoms: $1 -x+2, -y, -z+2 15312 Reflections read, of which 306 rejected -11 =< h =< 11, -28 =< k =< 28, -10 =< l =< 10, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 3407 Unique reflections, of which 0 suppressed R(int) = 0.0514 R(sigma) = 0.0438 Friedel opposites merged Maximum memory for data reduction = 2045 / 34073 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 = 2577 / 237744 wR2 = 0.1041 before cycle 1 for 3407 data and 190 / 190 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.041 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.052; Restrained GooF = 1.053 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.88 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50251 0.00083 0.036 OSF Mean shift/su = 0.027 Maximum = 1.259 for y H2W Max. shift = 0.025 A for H1W Max. dU = 0.001 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2577 / 237744 wR2 = 0.1041 before cycle 2 for 3407 data and 190 / 190 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.016 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.88 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50251 0.00083 -0.002 OSF Mean shift/su = 0.011 Maximum = 0.415 for y H2W Max. shift = 0.009 A for H1W Max. dU =-0.001 for H2W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2577 / 237744 wR2 = 0.1041 before cycle 3 for 3407 data and 190 / 190 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.88 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50251 0.00083 0.001 OSF Mean shift/su = 0.002 Maximum = 0.032 for U11 H1W Max. shift = 0.001 A for H2W Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2577 / 237744 wR2 = 0.1041 before cycle 4 for 3407 data and 190 / 190 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.88 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.50251 0.00083 0.000 OSF Mean shift/su = 0.000 Maximum = -0.007 for z H2W Max. shift = 0.000 A for H2W Max. dU = 0.000 for H2W Largest correlation matrix elements 0.617 z H1W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2797 -0.0196 0.6905 43 0.950 0.000 C2 N1 C3 H3 0.1754 -0.0365 0.3899 43 0.950 0.000 C3 C2 C4 H4 0.2288 0.0330 0.1878 43 0.950 0.000 C4 C5 C3 H5 0.3848 0.1173 0.2878 43 0.950 0.000 C5 C4 C6 H7A 0.5484 0.0456 0.9060 23 0.990 0.000 C7 N1 Si1 H7B 0.3797 0.0676 0.9191 23 0.990 0.000 C7 N1 Si1 H22 1.0327 0.1993 1.0924 43 0.950 0.000 C22 N21 C23 H23 1.1416 0.1937 1.3954 43 0.950 0.000 C23 C22 C24 H24 0.9817 0.1668 1.5766 43 0.950 0.000 C24 C25 C23 H25 0.7160 0.1483 1.4518 43 0.950 0.000 C25 C24 C26 H27A 0.7922 0.1462 0.8454 23 0.990 0.000 C27 N21 Si1 H27B 0.7460 0.2164 0.8497 23 0.990 0.000 C27 N21 Si1 H31A 0.2805 0.1993 0.8501 137 0.980 0.000 C31 Si1 H31A H31B 0.3645 0.2360 0.7273 137 0.980 0.000 C31 Si1 H31A H31C 0.4185 0.2460 0.9365 137 0.980 0.000 C31 Si1 H31A 2009src0244p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.29989 0.00824 0.60764 1.00000 0.02058 0.01830 0.02280 -0.00068 0.00529 -0.00213 0.02073 0.00443 0.00027 0.00011 0.00031 0.00000 0.00111 0.00113 0.00115 0.00090 0.00091 0.00088 0.00047 H2 0.27965 -0.01955 0.69052 1.00000 0.02487 0.00000 0.00000 C3 0.23867 -0.00190 0.43095 1.00000 0.02273 0.02578 0.02557 -0.00506 0.00395 -0.00283 0.02527 0.00472 0.00028 0.00012 0.00032 0.00000 0.00120 0.00128 0.00123 0.00100 0.00098 0.00097 0.00052 H3 0.17542 -0.03652 0.38989 1.00000 0.03033 0.00000 0.00000 C4 0.27074 0.03968 0.31094 1.00000 0.02542 0.02989 0.01661 -0.00452 0.00262 0.00328 0.02464 0.00469 0.00028 0.00012 0.00031 0.00000 0.00124 0.00133 0.00111 0.00096 0.00095 0.00101 0.00052 H4 0.22879 0.03305 0.18775 1.00000 0.02957 0.00000 0.00000 C5 0.36183 0.08970 0.36950 1.00000 0.01945 0.02744 0.01659 0.00247 0.00554 0.00212 0.02106 0.00457 0.00027 0.00011 0.00030 0.00000 0.00110 0.00124 0.00108 0.00092 0.00088 0.00093 0.00047 H5 0.38484 0.11728 0.28778 1.00000 0.02528 0.00000 0.00000 C6 0.42065 0.09967 0.55168 1.00000 0.01250 0.01934 0.01763 0.00073 0.00356 0.00179 0.01663 0.00424 0.00024 0.00010 0.00029 0.00000 0.00097 0.00110 0.00105 0.00085 0.00082 0.00081 0.00043 C7 0.45882 0.07279 0.85354 1.00000 0.01750 0.02063 0.01362 -0.00055 0.00381 -0.00135 0.01737 0.00413 0.00026 0.00010 0.00028 0.00000 0.00105 0.00113 0.00101 0.00085 0.00083 0.00086 0.00044 H7A 0.54842 0.04564 0.90604 1.00000 0.02084 0.00000 0.00000 H7B 0.37972 0.06762 0.91908 1.00000 0.02084 0.00000 0.00000 C22 0.96883 0.18895 1.16644 1.00000 0.01933 0.01687 0.02458 -0.00142 0.00657 -0.00222 0.02018 0.00439 0.00027 0.00010 0.00031 0.00000 0.00110 0.00109 0.00118 0.00090 0.00092 0.00086 0.00047 H22 1.03270 0.19929 1.09245 1.00000 0.02422 0.00000 0.00000 C23 1.03336 0.18550 1.34474 1.00000 0.01860 0.02000 0.02742 -0.00220 0.00042 -0.00022 0.02323 0.00456 0.00028 0.00011 0.00032 0.00000 0.00112 0.00116 0.00125 0.00096 0.00095 0.00090 0.00050 H23 1.14157 0.19369 1.39538 1.00000 0.02788 0.00000 0.00000 C24 0.93781 0.16967 1.45243 1.00000 0.02971 0.02087 0.01871 0.00018 0.00202 -0.00004 0.02407 0.00471 0.00029 0.00011 0.00032 0.00000 0.00130 0.00120 0.00112 0.00091 0.00097 0.00097 0.00051 H24 0.98175 0.16682 1.57662 1.00000 0.02889 0.00000 0.00000 C25 0.78112 0.15830 1.37900 1.00000 0.02963 0.01708 0.01810 0.00134 0.00584 -0.00236 0.02178 0.00452 0.00029 0.00010 0.00030 0.00000 0.00126 0.00112 0.00111 0.00088 0.00096 0.00093 0.00048 H25 0.71598 0.14826 1.45184 1.00000 0.02614 0.00000 0.00000 C26 0.71824 0.16171 1.19459 1.00000 0.01969 0.01163 0.02075 0.00056 0.00602 0.00025 0.01729 0.00430 0.00026 0.00010 0.00029 0.00000 0.00109 0.00100 0.00110 0.00082 0.00089 0.00081 0.00044 C27 0.73892 0.17613 0.90201 1.00000 0.02028 0.01910 0.01490 0.00025 0.00542 -0.00177 0.01800 0.00421 0.00026 0.00010 0.00028 0.00000 0.00111 0.00111 0.00104 0.00085 0.00087 0.00086 0.00045 H27A 0.79218 0.14618 0.84535 1.00000 0.02160 0.00000 0.00000 H27B 0.74602 0.21644 0.84970 1.00000 0.02160 0.00000 0.00000 C31 0.38020 0.21623 0.84207 1.00000 0.02101 0.02364 0.02394 0.00032 0.00560 0.00461 0.02301 0.00479 0.00027 0.00011 0.00032 0.00000 0.00115 0.00122 0.00117 0.00096 0.00094 0.00094 0.00049 H31A 0.28054 0.19933 0.85012 1.00000 0.03451 0.00000 0.00000 H31B 0.36454 0.23601 0.72726 1.00000 0.03451 0.00000 0.00000 H31C 0.41851 0.24601 0.93645 1.00000 0.03451 0.00000 0.00000 N1 0.38998 0.05817 0.66521 1.00000 0.01559 0.01724 0.01639 -0.00015 0.00425 0.00129 0.01645 0.00355 0.00021 0.00008 0.00024 0.00000 0.00087 0.00092 0.00089 0.00072 0.00072 0.00071 0.00038 N21 0.81391 0.17768 1.09411 1.00000 0.01699 0.01441 0.01807 -0.00029 0.00451 -0.00165 0.01657 0.00353 0.00021 0.00008 0.00024 0.00000 0.00091 0.00090 0.00092 0.00071 0.00074 0.00070 0.00038 O6 0.50366 0.14642 0.62310 1.00000 0.02246 0.01994 0.01583 0.00099 0.00592 -0.00374 0.01930 0.00300 0.00018 0.00007 0.00020 0.00000 0.00082 0.00082 0.00076 0.00062 0.00064 0.00064 0.00034 O26 0.57349 0.15071 1.11138 1.00000 0.01892 0.02623 0.01490 -0.00086 0.00537 -0.00344 0.01989 0.00301 0.00018 0.00008 0.00020 0.00000 0.00079 0.00088 0.00075 0.00064 0.00062 0.00066 0.00034 Si1 0.52651 0.15418 0.86556 1.00000 0.01563 0.01624 0.01523 -0.00037 0.00461 -0.00054 0.01565 0.00116 0.00007 0.00003 0.00008 0.00000 0.00029 0.00030 0.00029 0.00023 0.00023 0.00023 0.00014 Cl1 1.07234 0.09663 0.86700 1.00000 0.02084 0.02134 0.02250 0.00327 0.00708 0.00137 0.02136 0.00111 0.00006 0.00003 0.00007 0.00000 0.00027 0.00028 0.00028 0.00021 0.00021 0.00021 0.00014 O1W 0.84814 0.04306 1.08646 1.00000 0.03071 0.02047 0.03350 0.00349 0.01669 0.00083 0.02667 0.00371 0.00021 0.00008 0.00025 0.00000 0.00099 0.00093 0.00101 0.00076 0.00081 0.00075 0.00039 H1W 0.90839 0.05797 1.03222 1.00000 0.04475 0.06179 0.00328 0.00124 0.00391 0.00000 0.00959 H2W 0.87474 0.00598 1.10921 1.00000 0.05426 0.06603 0.00380 0.00086 0.00437 0.00000 0.01075 Final Structure Factor Calculation for 2009src0244p21c in P2(1)/c Total number of l.s. parameters = 190 Maximum vector length = 511 Memory required = 2387 / 25039 wR2 = 0.1041 before cycle 5 for 3407 data and 0 / 190 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.88 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0482 for 2948 Fo > 4sig(Fo) and 0.0579 for all 3407 data wR2 = 0.1041, GooF = S = 1.053, Restrained GooF = 1.052 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0234 0.0218 0.0170 C2 0.0311 0.0262 0.0186 C3 0.0349 0.0239 0.0152 C4 0.0283 0.0190 0.0159 C5 0.0198 0.0180 0.0121 C6 0.0211 0.0174 0.0136 C7 0.0248 0.0201 0.0156 C22 0.0332 0.0200 0.0166 C23 0.0334 0.0209 0.0179 C24 0.0308 0.0190 0.0156 C25 0.0208 0.0195 0.0116 C26 0.0216 0.0179 0.0145 C27 0.0274 0.0241 0.0175 C31 0.0181 0.0164 0.0149 N1 0.0185 0.0176 0.0136 N21 0.0254 0.0180 0.0145 O6 0.0276 0.0176 0.0145 O26 0.0166 0.0153 0.0150 Si1 0.0254 0.0201 0.0186 Cl1 0.0387 0.0227 0.0186 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.025 0.036 0.049 0.063 0.079 0.099 0.126 0.169 1.000 Number in group 360. 340. 341. 341. 324. 353. 325. 347. 333. 343. GooF 1.064 1.088 1.110 1.134 1.037 1.109 0.974 1.020 0.969 1.000 K 2.001 1.173 1.067 1.015 0.990 1.002 0.996 1.008 1.005 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 347. 342. 339. 343. 333. 342. 338. 340. 341. 342. GooF 1.121 1.139 1.058 1.099 1.011 1.009 0.804 0.864 1.089 1.254 K 1.021 1.023 1.024 1.026 1.015 1.011 0.995 0.994 0.995 1.011 R1 0.112 0.103 0.094 0.080 0.068 0.060 0.040 0.036 0.039 0.029 Recommended weighting scheme: WGHT 0.0000 2.8697 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 3 3 331.71 209.02 4.30 0.076 1.85 9 3 1 324.92 506.68 4.11 0.118 0.90 -2 26 4 97.22 196.08 3.73 0.074 0.78 -6 7 9 246.88 433.30 3.64 0.110 0.81 -6 6 3 23.85 0.47 3.63 0.004 1.33 -3 7 3 7.38 39.58 3.38 0.033 1.82 5 1 7 95.48 193.30 3.33 0.073 0.82 1 2 3 2977.73 2614.42 3.29 0.269 2.21 1 2 7 495.69 668.26 3.25 0.136 1.03 5 3 1 65.40 25.89 3.21 0.027 1.54 6 18 4 35.26 100.53 3.21 0.053 0.78 -2 3 9 70.65 23.00 3.21 0.025 0.87 -4 2 3 814.75 660.26 3.16 0.135 1.89 3 26 0 591.57 416.91 3.16 0.107 0.81 -7 1 8 291.30 182.94 3.12 0.071 0.88 -1 12 1 802.12 984.18 3.09 0.165 1.77 4 17 6 27.16 80.69 3.09 0.047 0.78 3 24 0 51.72 9.93 3.08 0.017 0.87 -4 12 4 34.97 80.36 3.05 0.047 1.24 -5 9 8 602.75 453.08 3.02 0.112 0.88 -6 23 1 12.35 52.57 2.99 0.038 0.80 -4 1 10 98.43 41.78 2.98 0.034 0.79 9 7 3 63.60 129.81 2.90 0.060 0.79 1 23 1 124.68 67.81 2.90 0.043 0.94 -9 4 3 23.23 2.46 2.89 0.008 0.97 4 25 1 32.36 2.34 2.88 0.008 0.80 -3 1 2 37.19 13.26 2.88 0.019 2.64 1 2 0 29.15 66.44 2.86 0.043 6.75 -1 11 3 240.25 328.46 2.84 0.095 1.60 -11 4 5 94.33 44.01 2.83 0.035 0.78 -1 19 4 -3.36 13.68 2.79 0.019 1.00 -3 2 4 572.34 460.67 2.78 0.113 1.81 -5 21 4 272.04 385.54 2.76 0.103 0.86 2 0 2 2295.86 2601.53 2.75 0.268 2.51 -1 7 2 5227.92 5752.27 2.74 0.399 2.45 -5 5 4 160.06 230.02 2.73 0.080 1.41 5 0 6 62.21 15.38 2.72 0.021 0.90 -6 6 9 79.22 27.28 2.71 0.027 0.81 -1 16 8 60.07 17.14 2.70 0.022 0.79 -2 12 3 26.40 61.15 2.67 0.041 1.48 -2 27 3 -5.80 22.86 2.67 0.025 0.78 6 9 3 60.59 19.86 2.63 0.023 1.01 -5 5 9 81.46 149.48 2.62 0.064 0.84 2 22 5 12.04 54.44 2.60 0.039 0.80 -1 0 4 2106.98 1855.29 2.60 0.227 1.97 2 17 4 20.51 56.46 2.60 0.040 1.00 -9 5 7 25.51 2.06 2.59 0.008 0.82 -3 19 6 20.79 55.82 2.58 0.039 0.87 -1 22 4 1312.94 1072.35 2.57 0.172 0.89 8 16 0 21.69 57.73 2.56 0.040 0.84 Bond lengths and angles C2 - Distance Angles N1 1.3629 (0.0029) C3 1.3658 (0.0033) 120.08 (0.22) H2 0.9500 119.96 119.96 C2 - N1 C3 C3 - Distance Angles C2 1.3658 (0.0033) C4 1.4044 (0.0036) 118.93 (0.23) H3 0.9500 120.53 120.53 C3 - C2 C4 C4 - Distance Angles C5 1.3703 (0.0034) C3 1.4044 (0.0036) 120.76 (0.22) H4 0.9500 119.62 119.62 C4 - C5 C3 C5 - Distance Angles C4 1.3703 (0.0034) C6 1.4027 (0.0031) 119.14 (0.21) H5 0.9500 120.43 120.43 C5 - C4 C6 C6 - Distance Angles O6 1.3011 (0.0027) N1 1.3614 (0.0028) 116.24 (0.19) C5 1.4027 (0.0031) 124.84 (0.20) 118.92 (0.20) C6 - O6 N1 C7 - Distance Angles N1 1.4758 (0.0027) Si1 1.8878 (0.0023) 107.14 (0.14) H7A 0.9900 110.29 110.29 H7B 0.9900 110.29 110.29 108.54 C7 - N1 Si1 H7A C22 - Distance Angles N21 1.3579 (0.0028) C23 1.3647 (0.0033) 120.43 (0.21) H22 0.9500 119.79 119.79 C22 - N21 C23 C23 - Distance Angles C22 1.3647 (0.0033) C24 1.4046 (0.0035) 119.18 (0.22) H23 0.9500 120.41 120.41 C23 - C22 C24 C24 - Distance Angles C25 1.3737 (0.0034) C23 1.4046 (0.0035) 120.30 (0.22) H24 0.9500 119.85 119.85 C24 - C25 C23 C25 - Distance Angles C24 1.3737 (0.0034) C26 1.4073 (0.0031) 119.21 (0.22) H25 0.9500 120.40 120.40 C25 - C24 C26 C26 - Distance Angles O26 1.2932 (0.0027) N21 1.3626 (0.0028) 116.62 (0.19) C25 1.4073 (0.0031) 124.40 (0.21) 118.97 (0.20) C26 - O26 N21 C27 - Distance Angles N21 1.4757 (0.0027) Si1 1.8923 (0.0023) 107.81 (0.14) H27A 0.9900 110.15 110.14 H27B 0.9900 110.14 110.14 108.46 C27 - N21 Si1 H27A C31 - Distance Angles Si1 1.8617 (0.0024) 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 C6 1.3614 (0.0028) C2 1.3629 (0.0029) 122.13 (0.19) C7 1.4758 (0.0027) 114.40 (0.18) 123.46 (0.18) N1 - C6 C2 N21 - Distance Angles C22 1.3579 (0.0029) C26 1.3626 (0.0028) 121.89 (0.19) C27 1.4757 (0.0027) 123.27 (0.18) 114.61 (0.18) N21 - C22 C26 O6 - Distance Angles C6 1.3011 (0.0027) Si1 1.8750 (0.0016) 113.60 (0.14) O6 - C6 O26 - Distance Angles C26 1.2932 (0.0027) Si1 1.8684 (0.0016) 114.84 (0.14) O26 - C26 Si1 - Distance Angles C31 1.8617 (0.0024) O26 1.8684 (0.0016) 94.57 (0.09) O6 1.8750 (0.0016) 95.35 (0.09) 170.08 (0.08) C7 1.8878 (0.0023) 119.36 (0.11) 89.33 (0.09) 85.43 (0.08) C27 1.8923 (0.0023) 117.83 (0.11) 86.00 (0.08) 89.76 (0.08) 122.80 (0.10) Si1 - C31 O26 O6 C7 O1W - Distance Angles H1W 0.8413 (0.0167) H2W 0.8564 (0.0171) 107.60 (2.28) O1W - H1W Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.841(17) 2.371(17) 3.2119(18) 177(3) O1W-H1W...Cl1 0.856(17) 2.309(18) 3.1603(19) 172(3) O1W-H2W...Cl1_$1 FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 24 -2 2.381 1 2 R1 = 0.0577 for 3407 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.3560 0.6605 0.6311 [ 0.88 A from C27 ] Deepest hole -0.32 at 0.3590 0.2585 0.1983 [ 0.25 A from H31B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2678 / 30522 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6440 0.1605 0.8689 1.00000 0.05 0.49 0.88 C27 1.05 SI1 1.42 H27A 1.56 H27B Q2 1 0.4756 0.1085 0.8444 1.00000 0.05 0.36 0.81 C7 1.10 SI1 1.47 H7B 1.55 H7A Q3 1 0.4064 0.0898 0.4613 1.00000 0.05 0.31 0.72 C5 0.72 C6 1.46 H5 1.80 N1 Q4 1 0.7684 0.1678 1.2859 1.00000 0.05 0.30 0.74 C25 0.75 C26 1.57 H25 1.69 N21 Q5 1 0.8693 0.1517 1.4210 1.00000 0.05 0.30 0.71 C24 0.77 C25 1.39 H24 1.45 H25 Q6 1 1.0173 0.1017 1.5975 1.00000 0.05 0.29 1.47 H24 1.90 C24 2.05 CL1 2.26 H3 Q7 1 0.7661 0.1668 1.1415 1.00000 0.05 0.29 0.68 N21 0.69 C26 1.70 O26 1.82 C22 Q8 1 0.9877 0.1974 1.2549 1.00000 0.05 0.29 0.70 C22 0.76 C23 1.45 H22 1.50 H23 Q9 1 0.3971 0.0787 0.6176 1.00000 0.05 0.27 0.60 N1 0.77 C6 1.76 O6 1.77 C2 Q10 1 1.0143 0.0539 0.8552 1.00000 0.05 0.27 1.07 CL1 1.63 H2W 1.89 H1W 2.21 H3 Shortest distances between peaks (including symmetry equivalents) 4 7 1.13 4 5 1.24 3 9 1.28 2 9 1.85 1 2 1.85 5 6 1.96 7 8 2.04 1 7 2.13 4 8 2.13 5 8 2.15 5 7 2.16 6 10 2.30 2 3 2.94 Time profile in seconds ----------------------- 0.03: 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. 0.70: 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 0.67: Structure factors and derivatives 0.83: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0244p21c finished at 10:58:30 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++