+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0288cc started at 10:50:02 on 25-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0288cc in Cc CELL 0.71073 10.6695 17.3082 7.7714 90.000 116.560 90.000 ZERR 4.00 0.0009 0.0017 0.0006 0.000 0.003 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O SI CL UNIT 36 48 8 12 4 8 V = 1283.69 F(000) = 608.0 Mu = 0.60 mm-1 Cell Wt = 1180.78 Rho = 1.527 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 SADI Si1 C10 Si1 C11 Si1 C20 Si1 C21 EADP C10 C11 C20 C21 FMAP 2 PLAN 10 SIZE 0.02 0.05 0.12 ACTA BOND $H WGHT 0.05140 3.64360 L.S. 8 TEMP -153.00 FVAR 0.53696 0.64592 PART 1 C10 1 0.310549 0.779176 0.128739 21.00000 0.04239 0.05502 = 0.03961 0.01295 0.01146 -0.01148 AFIX 23 H10A 2 0.411911 0.767151 0.195048 21.00000 -1.20000 H10B 2 0.259958 0.732619 0.137889 21.00000 -1.20000 AFIX 0 CL1 6 0.266897 0.794192 -0.103773 21.00000 0.07219 0.05883 = 0.04307 -0.00810 0.03069 0.00662 C11 1 0.371612 0.951090 0.293337 21.00000 0.04239 0.05502 = 0.03961 0.01295 0.01146 -0.01148 AFIX 137 H11A 2 0.472643 0.940994 0.353512 21.00000 -1.50000 H11B 2 0.349542 0.986289 0.374773 21.00000 -1.50000 H11C 2 0.343267 0.974723 0.166757 21.00000 -1.50000 AFIX 0 PART 2 C20 1 0.368296 0.949095 0.258626 -21.00000 0.04239 0.05502 = 0.03961 0.01295 0.01146 -0.01148 AFIX 23 H20A 2 0.464106 0.950552 0.366170 -21.00000 -1.20000 H20B 2 0.374202 0.953853 0.135510 -21.00000 -1.20000 AFIX 0 CL2 6 0.271234 1.017133 0.280389 -21.00000 0.07493 0.03823 = 0.05006 -0.00307 0.02655 -0.00290 C21 1 0.300990 0.770024 0.146651 -21.00000 0.04239 0.05502 = 0.03961 0.01295 0.01146 -0.01148 AFIX 137 H21A 2 0.270731 0.780341 0.009782 -21.00000 -1.50000 H21B 2 0.245167 0.727674 0.160404 -21.00000 -1.50000 H21C 2 0.400257 0.755533 0.207837 -21.00000 -1.50000 AFIX 0 MOLE 1 PART 0 C2 1 -0.118240 0.867291 0.217858 11.00000 0.04127 0.04135 = 0.03538 -0.00351 0.01763 -0.00277 AFIX 43 H2 2 -0.112866 0.852783 0.338868 11.00000 -1.20000 AFIX 0 C3 1 -0.247298 0.882472 0.069495 11.00000 0.03427 0.05714 = 0.04266 -0.00466 0.01797 0.00104 C4 1 -0.248813 0.902580 -0.108652 11.00000 0.03515 0.03773 = 0.03964 -0.00151 0.00573 0.00293 AFIX 43 H4 2 -0.335588 0.912691 -0.217425 11.00000 -1.20000 AFIX 0 C5 1 -0.127605 0.907518 -0.125277 11.00000 0.03646 0.03395 = 0.02967 -0.00061 0.00611 -0.00229 C6 1 0.004686 0.891670 0.031466 11.00000 0.03362 0.04084 = 0.03563 0.00212 0.00915 -0.00628 C7 1 -0.379340 0.878452 0.088873 11.00000 0.03519 0.09489 = 0.05449 -0.00566 0.01686 0.00861 AFIX 137 H7A 2 -0.399096 0.929116 0.127550 11.00000 -1.50000 H7B 2 -0.369527 0.839978 0.186627 11.00000 -1.50000 H7C 2 -0.456598 0.863606 -0.034762 11.00000 -1.50000 AFIX 0 C9 1 0.139295 0.852063 0.356876 11.00000 0.02992 0.05948 = 0.03246 0.01278 0.00602 -0.00588 AFIX 23 H9A 2 0.137377 0.798959 0.402969 11.00000 -1.20000 H9B 2 0.163191 0.888051 0.466113 11.00000 -1.20000 AFIX 0 N1 3 0.000248 0.871939 0.200253 11.00000 0.03886 0.04230 = 0.02484 -0.00019 0.00834 -0.00761 N8 3 -0.136240 0.926622 -0.312100 11.00000 0.04782 0.04067 = 0.03217 0.00585 0.01028 -0.00250 O6 4 0.121901 0.893696 0.032073 11.00000 0.02743 0.08215 = 0.03846 0.02054 0.00627 -0.01013 O8A 4 -0.251919 0.928125 -0.450865 11.00000 0.04596 0.06387 = 0.03925 0.01242 -0.00275 -0.00697 O8B 4 -0.029254 0.941014 -0.326618 11.00000 0.05096 0.09425 = 0.04010 0.01873 0.01590 0.00463 SI1 5 0.275816 0.858852 0.264889 11.00000 0.02913 0.06704 = 0.03249 0.01254 0.00407 -0.01024 CL3 6 0.436082 0.811182 0.554448 11.00000 0.03649 0.05709 = 0.03592 0.00818 0.00156 -0.00435 HKLF 4 Covalent radii and connectivity table for 2009src0288cc in Cc C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C10_a - Cl1_a Si1 Cl1_a - C10_a C11_a - Si1 C20_b - Cl2_b Si1 Cl2_b - C20_b C21_b - Si1 C2 - N1 C3 C3 - C2 C4 C7 C4 - C5 C3 C5 - C4 C6 N8 C6 - O6 N1 C5 C7 - C3 C9 - N1 Si1 N1 - C2 C6 C9 N8 - O8B O8A C5 O6 - C6 Si1 O8A - N8 O8B - N8 Si1 - C11_a C20_b C21_b C10_a C9 O6 Cl3 Cl3 - Si1 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 0 -1 6.28 1.11 observed but should be systematically absent 11095 Reflections read, of which 235 rejected -13 =< h =< 13, -22 =< k =< 22, -10 =< l =< 10, Max. 2-theta = 54.95 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -8 8 -4 88.20 9.89 2 64.40 7 3 1 85.44 2.58 4 21.05 6 8 2 133.73 4.13 4 35.32 3 Inconsistent equivalents 2873 Unique reflections, of which 0 suppressed R(int) = 0.0713 R(sigma) = 0.0652 Friedel opposites not merged Maximum memory for data reduction = 2005 / 35466 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 = 2514 / 210075 wR2 = 0.1554 before cycle 1 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53694 0.00157 -0.015 OSF 2 0.64593 0.00472 0.001 FVAR 2 Mean shift/su = 0.002 Maximum = -0.015 for OSF Max. shift = 0.000 A for H21C_b Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 2 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 -0.003 OSF 2 0.64593 0.00472 0.001 FVAR 2 Mean shift/su = 0.001 Maximum = -0.003 for tors H11A_a Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for Cl2_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 3 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 -0.001 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = -0.002 for tors H11A_a Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for C10_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 4 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 0.000 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = -0.001 for tors H11A_a Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for C10_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 5 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 0.000 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for tors H11A_a Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for C10_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 6 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 0.000 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for y Cl2_b Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for C10_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 7 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 0.000 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for y Cl2_b Max. shift = 0.000 A for H11A_a Max. dU = 0.000 for C10_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2514 / 210075 wR2 = 0.1554 before cycle 8 for 2873 data and 167 / 167 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53693 0.00157 0.000 OSF 2 0.64593 0.00472 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for y Cl2_b Max. shift = 0.000 A for H21B_b Max. dU = 0.000 for C10_a Largest correlation matrix elements -0.897 z C21_b / z C10_a -0.752 x C21_b / z C10_a 0.690 U33 C10_a / z C10_a -0.896 x C21_b / x C10_a -0.751 z C21_b / x C10_a 0.633 x C20_b / U13 C10_a -0.884 x C20_b / x C11_a -0.747 z C11_a / U33 C10_a -0.614 y C21_b / y C10_a -0.834 z C20_b / z C11_a -0.746 y C20_b / x C20_b 0.610 U13 Cl1_a / U11 Cl1_a -0.791 y C20_b / y C11_a -0.737 z C21_b / U33 C10_a 0.609 U13 Cl1_a / U33 Cl1_a 0.789 z C10_a / x C10_a -0.707 y C11_a / x C11_a -0.607 x C11_a / U13 C10_a 0.787 z C21_b / x C21_b 0.705 y C20_b / x C11_a -0.594 z C21_b / z C20_b 0.777 z C20_b / U33 C10_a 0.691 x C20_b / y C11_a -0.574 z C21_b / y C21_b Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H10A 0.4119 0.7672 0.1950 23 0.990 0.000 C10_a Cl1_a Si1 H10B 0.2600 0.7326 0.1379 23 0.990 0.000 C10_a Cl1_a Si1 H11A 0.4726 0.9410 0.3536 137 0.980 0.000 C11_a Si1 H11A_a H11B 0.3495 0.9863 0.3747 137 0.980 0.000 C11_a Si1 H11A_a H11C 0.3433 0.9747 0.1668 137 0.980 0.000 C11_a Si1 H11A_a H20A 0.4641 0.9505 0.3661 23 0.990 0.000 C20_b Cl2_b Si1 H20B 0.3742 0.9539 0.1355 23 0.990 0.000 C20_b Cl2_b Si1 H21A 0.2708 0.7803 0.0098 137 0.980 0.000 C21_b Si1 H21A_b H21B 0.2451 0.7277 0.1603 137 0.980 0.000 C21_b Si1 H21A_b H21C 0.4002 0.7555 0.2079 137 0.980 0.000 C21_b Si1 H21A_b H2 -0.1129 0.8528 0.3389 43 0.950 0.000 C2 N1 C3 H4 -0.3356 0.9127 -0.2174 43 0.950 0.000 C4 C5 C3 H7A -0.3991 0.9291 0.1275 137 0.980 0.000 C7 C3 H7A H7B -0.3695 0.8400 0.1866 137 0.980 0.000 C7 C3 H7A H7C -0.4566 0.8636 -0.0348 137 0.980 0.000 C7 C3 H7A H9A 0.1374 0.7990 0.4030 23 0.990 0.000 C9 N1 Si1 H9B 0.1632 0.8881 0.4661 23 0.990 0.000 C9 N1 Si1 2009src0288cc in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C10_a 0.31056 0.77918 0.12874 0.64593 0.04238 0.05504 0.03957 0.01294 0.01146 -0.01148 0.04822 0.04147 0.00227 0.00066 0.00284 0.00472 0.00258 0.00296 0.00477 0.00280 0.00269 0.00229 0.00197 H10A_a 0.41192 0.76716 0.19505 0.64593 0.05786 0.00472 0.00000 H10B_a 0.25997 0.73262 0.13790 0.64593 0.05786 0.00472 0.00000 Cl1_a 0.26690 0.79419 -0.10377 0.64593 0.07219 0.05882 0.04307 -0.00810 0.03069 0.00662 0.05619 0.00532 0.00028 0.00014 0.00032 0.00472 0.00170 0.00157 0.00135 0.00108 0.00124 0.00121 0.00083 C11_a 0.37161 0.95110 0.29336 0.64593 0.04238 0.05504 0.03957 0.01294 0.01146 -0.01148 0.04822 0.03048 0.00212 0.00087 0.00247 0.00472 0.00258 0.00296 0.00477 0.00280 0.00269 0.00229 0.00197 H11A_a 0.47264 0.94101 0.35363 0.64593 0.07233 0.00472 0.00000 H11B_a 0.34948 0.98631 0.37471 0.64593 0.07233 0.00472 0.00000 H11C_a 0.34332 0.97471 0.16677 0.64593 0.07233 0.00472 0.00000 C20_b 0.36830 0.94909 0.25860 0.35407 0.04238 0.05504 0.03957 0.01294 0.01146 -0.01148 0.04822 0.05853 0.00386 0.00150 0.00493 0.00472 0.00258 0.00296 0.00477 0.00280 0.00269 0.00229 0.00197 H20A_b 0.46412 0.95055 0.36612 0.35407 0.05786 0.00472 0.00000 H20B_b 0.37418 0.95385 0.13547 0.35407 0.05786 0.00472 0.00000 Cl2_b 0.27124 1.01713 0.28039 0.35407 0.07493 0.03821 0.05006 -0.00306 0.02655 -0.00289 0.05492 0.00988 0.00055 0.00024 0.00066 0.00472 0.00311 0.00241 0.00256 0.00193 0.00221 0.00220 0.00150 C21_b 0.30097 0.77002 0.14664 0.35407 0.04238 0.05504 0.03957 0.01294 0.01146 -0.01148 0.04822 0.07569 0.00409 0.00120 0.00561 0.00472 0.00258 0.00296 0.00477 0.00280 0.00269 0.00229 0.00197 H21A_b 0.27075 0.78035 0.00979 0.35407 0.07233 0.00472 0.00000 H21B_b 0.24511 0.72768 0.16034 0.35407 0.07233 0.00472 0.00000 H21C_b 0.40023 0.75551 0.20786 0.35407 0.07233 0.00472 0.00000 C2 -0.11824 0.86729 0.21786 1.00000 0.04127 0.04136 0.03538 -0.00350 0.01763 -0.00277 0.03915 0.01150 0.00058 0.00032 0.00079 0.00000 0.00298 0.00307 0.00271 0.00234 0.00237 0.00238 0.00120 H2 -0.11286 0.85279 0.33887 1.00000 0.04698 0.00000 0.00000 C3 -0.24730 0.88247 0.06950 1.00000 0.03427 0.05715 0.04265 -0.00466 0.01796 0.00105 0.04441 0.01218 0.00056 0.00036 0.00082 0.00000 0.00282 0.00373 0.00331 0.00264 0.00250 0.00256 0.00139 C4 -0.24881 0.90258 -0.10866 1.00000 0.03513 0.03775 0.03965 -0.00150 0.00573 0.00293 0.04161 0.01170 0.00059 0.00031 0.00083 0.00000 0.00279 0.00283 0.00288 0.00236 0.00225 0.00228 0.00124 H4 -0.33559 0.91269 -0.21743 1.00000 0.04993 0.00000 0.00000 C5 -0.12760 0.90752 -0.12528 1.00000 0.03647 0.03396 0.02968 -0.00062 0.00611 -0.00229 0.03660 0.01064 0.00054 0.00032 0.00071 0.00000 0.00278 0.00287 0.00258 0.00213 0.00216 0.00217 0.00119 C6 0.00468 0.89167 0.03146 1.00000 0.03361 0.04084 0.03563 0.00213 0.00914 -0.00628 0.03906 0.01085 0.00054 0.00033 0.00073 0.00000 0.00286 0.00313 0.00286 0.00228 0.00229 0.00222 0.00123 C7 -0.37934 0.87845 0.08887 1.00000 0.03517 0.09491 0.05447 -0.00566 0.01685 0.00860 0.06271 0.01441 0.00064 0.00047 0.00095 0.00000 0.00327 0.00562 0.00412 0.00371 0.00311 0.00333 0.00193 H7A -0.39911 0.92911 0.12752 1.00000 0.09406 0.00000 0.00000 H7B -0.36952 0.83998 0.18664 1.00000 0.09406 0.00000 0.00000 H7C -0.45659 0.86359 -0.03476 1.00000 0.09406 0.00000 0.00000 C9 0.13929 0.85207 0.35688 1.00000 0.02992 0.05950 0.03247 0.01279 0.00603 -0.00589 0.04358 0.01180 0.00052 0.00037 0.00076 0.00000 0.00265 0.00378 0.00265 0.00260 0.00224 0.00248 0.00137 H9A 0.13738 0.79896 0.40298 1.00000 0.05229 0.00000 0.00000 H9B 0.16319 0.88805 0.46611 1.00000 0.05229 0.00000 0.00000 N1 0.00025 0.87194 0.20025 1.00000 0.03886 0.04231 0.02485 -0.00019 0.00835 -0.00761 0.03754 0.00873 0.00046 0.00026 0.00058 0.00000 0.00235 0.00266 0.00211 0.00189 0.00179 0.00206 0.00103 N8 -0.13624 0.92662 -0.31210 1.00000 0.04783 0.04068 0.03217 0.00585 0.01029 -0.00250 0.04305 0.00973 0.00051 0.00028 0.00061 0.00000 0.00288 0.00263 0.00250 0.00192 0.00228 0.00218 0.00116 O6 0.12190 0.89370 0.03207 1.00000 0.02744 0.08217 0.03846 0.02056 0.00628 -0.01013 0.05251 0.00838 0.00037 0.00027 0.00055 0.00000 0.00199 0.00322 0.00217 0.00209 0.00168 0.00197 0.00117 O8A -0.25192 0.92813 -0.45087 1.00000 0.04595 0.06388 0.03925 0.01242 -0.00275 -0.00697 0.05782 0.00881 0.00043 0.00027 0.00059 0.00000 0.00243 0.00278 0.00231 0.00200 0.00192 0.00206 0.00124 O8B -0.02925 0.94102 -0.32662 1.00000 0.05097 0.09424 0.04009 0.01873 0.01590 0.00463 0.06343 0.00996 0.00046 0.00031 0.00059 0.00000 0.00270 0.00384 0.00239 0.00238 0.00204 0.00247 0.00133 Si1 0.27582 0.85885 0.26489 1.00000 0.02913 0.06704 0.03249 0.01254 0.00407 -0.01024 0.04650 0.00304 0.00015 0.00011 0.00019 0.00000 0.00073 0.00114 0.00074 0.00078 0.00059 0.00072 0.00043 Cl3 0.43608 0.81118 0.55445 1.00000 0.03648 0.05709 0.03592 0.00817 0.00156 -0.00435 0.04861 0.00280 0.00014 0.00009 0.00019 0.00000 0.00066 0.00086 0.00065 0.00066 0.00052 0.00065 0.00038 Final Structure Factor Calculation for 2009src0288cc in Cc Total number of l.s. parameters = 167 Maximum vector length = 511 Memory required = 2349 / 27090 wR2 = 0.1554 before cycle 9 for 2873 data and 2 / 167 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.104; Restrained GooF = 1.103 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 3.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0664 for 2166 Fo > 4sig(Fo) and 0.0982 for all 2873 data wR2 = 0.1554, GooF = S = 1.104, Restrained GooF = 1.103 for all data Flack x parameter = 0.1351 with su 0.1409 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0775 0.0367 0.0305 C10_a 0.0761 0.0606 0.0319 Cl1_a 0.0775 0.0367 0.0305 C11_a 0.0775 0.0367 0.0305 C20_b 0.0774 0.0499 0.0375 Cl2_b 0.0775 0.0367 0.0305 C21_b 0.0442 0.0397 0.0335 C2 0.0591 0.0413 0.0329 C3 0.0583 0.0371 0.0294 C4 0.0496 0.0340 0.0262 C5 0.0519 0.0362 0.0291 C6 0.0988 0.0557 0.0336 C7 0.0720 0.0336 0.0252 C9 0.0526 0.0357 0.0243 N1 0.0596 0.0404 0.0291 N8 0.0999 0.0323 0.0253 O6 0.0935 0.0533 0.0266 O8A 0.1006 0.0555 0.0342 O8B 0.0814 0.0342 0.0240 Si1 0.0721 0.0478 0.0259 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.035 0.044 0.056 0.068 0.083 0.105 0.135 0.204 1.000 Number in group 297. 308. 258. 298. 291. 287. 272. 291. 285. 286. GooF 1.152 1.130 1.208 1.182 1.101 1.042 1.092 0.922 1.094 1.100 K 2.517 1.138 1.094 1.091 1.016 0.982 1.010 0.994 1.004 1.028 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.67 inf Number in group 300. 278. 289. 285. 289. 291. 280. 285. 292. 284. GooF 1.177 1.127 1.111 1.211 1.099 1.176 0.914 0.937 0.999 1.237 K 1.144 1.126 1.052 1.054 1.078 1.025 1.007 0.995 1.008 1.025 R1 0.327 0.256 0.206 0.167 0.125 0.100 0.063 0.049 0.041 0.035 Recommended weighting scheme: WGHT 0.0514 3.6332 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 6 0 1647.65 1042.08 5.84 0.183 2.88 0 4 0 32891.80 23668.87 5.56 0.872 4.33 -10 12 3 100.95 4.50 3.44 0.012 0.86 0 12 -1 2277.03 1626.16 3.37 0.228 1.41 7 13 1 -34.93 105.26 3.37 0.058 0.91 6 20 -1 192.74 56.88 3.34 0.043 0.77 0 12 0 1228.82 881.86 3.30 0.168 1.44 -12 2 4 106.62 3.59 3.22 0.011 0.88 -10 10 -1 113.34 30.43 3.20 0.031 0.79 -8 10 7 -37.26 69.90 3.17 0.047 0.88 -9 15 5 202.12 78.12 3.13 0.050 0.80 -3 11 -6 30.10 156.15 2.99 0.071 0.82 5 13 -6 120.24 34.25 2.94 0.033 0.92 -11 1 9 3.00 66.80 2.93 0.046 0.77 -8 16 -1 237.81 57.60 2.93 0.043 0.77 4 4 -8 80.80 14.40 2.90 0.022 0.94 -7 17 2 -7.81 87.02 2.87 0.053 0.85 0 12 1 2144.40 1687.66 2.87 0.233 1.41 10 0 -2 1623.17 1173.70 2.85 0.194 1.05 -3 11 -4 125.47 234.18 2.84 0.087 1.00 3 21 -2 138.84 15.73 2.78 0.022 0.80 4 8 5 49.96 156.83 2.77 0.071 0.92 -11 3 1 63.93 194.53 2.77 0.079 0.90 -10 0 8 158.84 38.81 2.77 0.035 0.86 5 17 -4 100.43 14.95 2.75 0.022 0.88 2 0 -4 846.81 637.02 2.75 0.143 1.93 -6 2 -2 24.92 77.51 2.72 0.050 1.24 6 16 -2 -24.66 40.17 2.71 0.036 0.92 -12 6 4 -32.19 35.10 2.68 0.034 0.85 -12 8 7 81.89 18.60 2.66 0.024 0.77 2 22 0 -33.26 36.82 2.65 0.034 0.78 -12 4 2 211.76 82.74 2.62 0.052 0.85 8 16 -3 20.33 114.05 2.61 0.061 0.84 -2 0 4 803.98 616.95 2.61 0.141 1.93 -7 11 7 64.73 196.73 2.60 0.079 0.88 11 7 -5 92.53 4.99 2.60 0.013 0.89 -1 5 -1 1290.21 1043.21 2.59 0.183 2.79 3 3 -3 105.62 51.60 2.59 0.041 2.27 -10 2 5 169.63 88.86 2.59 0.053 1.02 2 8 6 209.44 100.51 2.59 0.057 0.93 -1 19 -1 -20.11 37.76 2.58 0.035 0.89 4 20 -3 113.20 41.35 2.57 0.036 0.81 -6 0 -2 3.46 54.74 2.55 0.042 1.25 1 11 0 1116.99 853.88 2.55 0.166 1.55 -5 15 -1 174.17 96.12 2.54 0.056 0.95 -3 3 3 102.77 53.16 2.54 0.041 2.27 8 12 -6 -16.62 38.59 2.53 0.035 0.88 -6 12 -4 81.84 3.84 2.53 0.011 0.81 8 12 -2 10.49 78.08 2.49 0.050 0.98 11 13 -5 280.37 105.98 2.49 0.058 0.77 Bond lengths and angles C10_a - Distance Angles Cl1_a 1.6724 (0.0184) Si1 1.8733 (0.0099) 117.77 (0.96) H10A_a 0.9900 107.86 107.86 H10B_a 0.9900 107.86 107.86 107.17 C10_a - Cl1_a Si1 H10A_a Cl1_a - Distance Angles C10_a 1.6724 (0.0185) Cl1_a - C11_a - Distance Angles Si1 1.8548 (0.0090) H11A_a 0.9800 109.47 H11B_a 0.9800 109.47 109.47 H11C_a 0.9800 109.47 109.47 109.47 C11_a - Si1 H11A_a H11B_a C20_b - Distance Angles Cl2_b 1.6263 (0.0420) Si1 1.8598 (0.0140) 103.61 (1.76) H20A_b 0.9900 111.04 111.04 H20B_b 0.9900 111.04 111.04 109.02 C20_b - Cl2_b Si1 H20A_b Cl2_b - Distance Angles C20_b 1.6263 (0.0422) Cl2_b - C21_b - Distance Angles Si1 1.8711 (0.0138) H21A_b 0.9800 109.47 H21B_b 0.9800 109.47 109.47 H21C_b 0.9800 109.47 109.47 109.47 C21_b - Si1 H21A_b H21B_b C2 - Distance Angles N1 1.3334 (0.0068) C3 1.3692 (0.0076) 123.00 (0.52) H2 0.9500 118.50 118.50 C2 - N1 C3 C3 - Distance Angles C2 1.3692 (0.0077) C4 1.4206 (0.0083) 115.89 (0.50) C7 1.4839 (0.0081) 123.27 (0.55) 120.85 (0.54) C3 - C2 C4 C4 - Distance Angles C5 1.3586 (0.0078) C3 1.4206 (0.0083) 120.77 (0.50) H4 0.9500 119.62 119.62 C4 - C5 C3 C5 - Distance Angles C4 1.3586 (0.0078) C6 1.4190 (0.0068) 122.00 (0.49) N8 1.4512 (0.0068) 118.17 (0.46) 119.78 (0.47) C5 - C4 C6 C6 - Distance Angles O6 1.2490 (0.0066) N1 1.3766 (0.0066) 117.67 (0.47) C5 1.4190 (0.0068) 127.43 (0.50) 114.91 (0.48) C6 - O6 N1 C7 - Distance Angles C3 1.4839 (0.0081) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C3 H7A H7B C9 - Distance Angles N1 1.4785 (0.0065) Si1 1.8915 (0.0056) 109.46 (0.36) H9A 0.9900 109.78 109.78 H9B 0.9900 109.78 109.78 108.24 C9 - N1 Si1 H9A N1 - Distance Angles C2 1.3334 (0.0068) C6 1.3766 (0.0067) 123.43 (0.46) C9 1.4785 (0.0065) 123.36 (0.44) 113.13 (0.44) N1 - C2 C6 N8 - Distance Angles O8B 1.2219 (0.0060) O8A 1.2234 (0.0057) 122.02 (0.45) C5 1.4512 (0.0068) 119.66 (0.43) 118.33 (0.47) N8 - O8B O8A O6 - Distance Angles C6 1.2490 (0.0066) Si1 1.9176 (0.0039) 115.37 (0.36) O6 - C6 O8A - Distance Angles N8 1.2234 (0.0057) O8A - O8B - Distance Angles N8 1.2219 (0.0060) O8B - Si1 - Distance Angles C11_a 1.8548 (0.0090) C20_b 1.8598 (0.0141) 7.98 (1.54) C21_b 1.8711 (0.0138) 124.99 (1.25) 118.87 (1.20) C10_a 1.8733 (0.0099) 117.60 (0.68) 111.23 (1.43) 7.97 (1.22) C9 1.8915 (0.0056) 119.00 (0.71) 124.71 (1.30) 116.00 (0.88) 123.23 (0.51) O6 1.9176 (0.0039) 92.04 (0.65) 87.23 (1.17) 92.60 (1.38) 90.05 (0.73) 84.08 (0.21) Cl3 2.2864 (0.0019) 93.64 (0.61) 99.02 (1.15) 88.77 (1.36) 92.32 (0.70) 88.23 (0.16) 171.99 (0.14) Si1 - C11_a C20_b C21_b C10_a C9 O6 Cl3 - Distance Angles Si1 2.2864 (0.0019) Cl3 - FMAP and GRID set by program FMAP 2 3 24 GRID -2.381 -2 -1 2.381 2 1 R1 = 0.0867 for 1476 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.72 at 0.9560 0.2423 0.1897 [ 0.65 A from H10A ] Deepest hole -0.36 at 0.7637 0.3981 0.3258 [ 0.87 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2647 / 20346 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4560 0.7423 0.1897 1.00000 0.05 0.72 0.65 H10A 0.71 H21C 1.54 C10 1.61 C21 Q2 1 0.1806 0.8539 0.2722 1.00000 0.05 0.38 0.94 C9 1.05 SI1 1.60 H9A 1.70 H9B Q3 1 -0.2808 0.9284 -0.3474 1.00000 0.05 0.38 0.98 O8A 1.40 H4 1.44 N8 1.79 C4 Q4 1 -0.0348 0.8907 -0.3343 1.00000 0.05 0.34 0.87 O8B 1.32 N8 2.17 O8A 2.27 C5 Q5 1 -0.1448 0.9300 -0.4574 1.00000 0.05 0.32 1.09 N8 1.17 O8A 1.21 O8B 2.21 H2 Q6 1 -0.3005 0.8883 0.0941 1.00000 0.05 0.31 0.68 C3 0.84 C7 1.38 H7A 1.49 H7B Q7 1 0.1425 0.8705 -0.0191 1.00000 0.05 0.31 0.67 O6 1.72 C6 2.02 H21A 2.03 SI1 Q8 1 0.4253 0.7465 -0.0741 1.00000 0.05 0.29 1.80 CL1 1.83 H2 2.11 H21A 2.19 H10A Q9 1 0.2004 0.8740 0.1361 1.00000 0.05 0.29 0.93 O6 1.00 SI1 1.90 C6 2.03 C10 Q10 1 -0.2448 0.8825 -0.0017 1.00000 0.05 0.29 0.57 C3 0.88 C4 1.60 H4 1.66 C2 Shortest distances between peaks (including symmetry equivalents) 7 9 1.08 6 10 1.15 2 9 1.22 4 5 1.32 1 8 1.93 3 5 1.99 2 7 2.13 1 4 2.31 4 7 2.36 3 10 2.66 3 4 2.66 4 8 2.93 1 7 2.98 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 0.59: 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 1.20: Structure factors and derivatives 0.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.14: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0288cc finished at 10:50:07 Total CPU time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++