+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0344 started at 11:39:44 on 06-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0344 in P2(1)/c CELL 0.71073 9.0871 7.3467 21.0204 90.000 101.787 90.000 ZERR 4.00 0.0003 0.0002 0.0006 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F SI CL UNIT 36 36 4 4 12 4 12 V = 1373.73 F(000) = 680.0 Mu = 0.77 mm-1 Cell Wt = 1354.45 Rho = 1.637 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 1.75 0.02 Si1b C22B EADP C22 C22b FMAP 2 PLAN 10 SIZE 0.08 0.27 0.37 ACTA BOND $H WGHT 0.12640 6.04530 L.S. 20 TEMP -153.00 FVAR 0.66626 0.80750 0.52876 PART 1 C21 1 0.350805 0.305967 0.043053 21.00000 0.02573 0.06910 = 0.03261 0.01525 0.00181 -0.00477 AFIX 23 H21A 2 0.249057 0.356690 0.041131 21.00000 -1.20000 H21B 2 0.393607 0.362627 0.008130 21.00000 -1.20000 AFIX 0 C22 1 0.509367 0.598700 0.145166 21.00000 0.04687 0.03454 = 0.07380 -0.00806 0.02766 -0.00043 AFIX 137 H22A 2 0.559334 0.655275 0.113035 21.00000 -1.50000 H22B 2 0.573606 0.609890 0.188511 21.00000 -1.50000 H22C 2 0.413291 0.659956 0.144566 21.00000 -1.50000 AFIX 0 SI1 6 0.475079 0.354721 0.125094 21.00000 0.02036 0.03017 = 0.02907 -0.00113 0.00595 -0.00132 CL1 7 0.288155 0.320794 0.179187 21.00000 0.03374 0.05118 = 0.04815 -0.00552 0.02108 -0.00005 CL2 7 0.340617 0.062575 0.032533 21.00000 0.06345 0.10203 = 0.07478 -0.05959 -0.00532 -0.00064 F8A 5 1.015500 -0.266618 0.234647 31.00000 0.09463 F8B 5 1.005398 -0.360871 0.134201 31.00000 0.07094 F8C 5 1.173643 -0.186798 0.179685 31.00000 0.09218 PART 2 C21B 1 0.445180 0.547987 0.106934 -21.00000 0.03779 0.04277 = 0.03969 -0.00676 0.00250 -0.00028 AFIX 23 H21C 2 0.469340 0.599533 0.066771 -21.00000 -1.20000 H21D 2 0.345364 0.594229 0.111261 -21.00000 -1.20000 AFIX 0 C22B 1 0.332170 0.197579 0.030681 -21.00000 0.04687 0.03454 = 0.07380 -0.00806 0.02766 -0.00043 AFIX 33 H22D 2 0.375469 0.079546 0.022842 -21.00000 -1.50000 H22E 2 0.332228 0.277957 -0.006521 -21.00000 -1.50000 H22F 2 0.228736 0.180187 0.036401 -21.00000 -1.50000 AFIX 0 SI1B 6 0.441334 0.297603 0.102128 -21.00000 0.01773 0.03747 = 0.03411 -0.00136 0.00531 -0.00245 CL1B 7 0.266753 0.269559 0.163533 -21.00000 0.02782 0.06100 = 0.05139 -0.00587 0.02438 -0.00828 CL2B 7 0.585429 0.616299 0.176286 -21.00000 0.07022 0.04683 = 0.07407 -0.01326 0.00213 -0.01366 F8D 5 0.953242 -0.353446 0.207334 -31.00000 0.08150 F8E 5 1.095073 -0.302266 0.135886 -31.00000 0.10361 F8F 5 1.135750 -0.178887 0.224502 -31.00000 0.09825 MOLE 1 PART 0 C2 1 0.805097 -0.027569 0.174448 11.00000 0.03912 0.03561 = 0.03029 0.00258 0.00227 0.00894 AFIX 43 H2 2 0.780944 -0.100610 0.208181 11.00000 -1.20000 AFIX 0 C3 1 0.930994 -0.063510 0.151574 11.00000 0.04308 0.04840 = 0.03490 0.00124 0.00327 0.01711 C4 1 0.967848 0.046119 0.101949 11.00000 0.03223 0.04514 = 0.04116 -0.00807 0.00852 0.00569 AFIX 43 H4 2 1.056799 0.023361 0.086092 11.00000 -1.20000 AFIX 0 C5 1 0.875069 0.183794 0.077286 11.00000 0.03074 0.03313 = 0.03812 -0.00039 0.01082 -0.00151 C6 1 0.742008 0.220714 0.100654 11.00000 0.02588 0.02648 = 0.03693 0.00131 0.00910 0.00006 C7 1 0.575369 0.156610 0.172653 11.00000 0.02440 0.04369 = 0.03581 0.00764 0.00899 0.00405 AFIX 23 H7A 2 0.601101 0.188258 0.219391 11.00000 -1.20000 H7B 2 0.508018 0.049357 0.167516 11.00000 -1.20000 AFIX 0 C8 1 1.027697 -0.224242 0.177342 11.00000 0.05999 0.11027 = 0.04399 0.01657 0.01358 0.03758 N1 3 0.713366 0.111524 0.149668 11.00000 0.02435 0.03225 = 0.02949 0.00104 0.00611 0.00241 O6 4 0.648047 0.345558 0.080957 11.00000 0.02896 0.04135 = 0.05485 0.01922 0.01884 0.00848 CL5 7 0.908332 0.315983 0.014505 11.00000 0.04221 0.04508 = 0.06753 0.01190 0.03252 0.00171 HKLF 4 Covalent radii and connectivity table for 2009src0344 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 SI 1.170 CL 0.990 C21_a - Cl2_a Si1_a C22_a - Si1_a Si1_a - C22_a C7 C21_a O6 Cl1_a Cl1_a - Si1_a Cl2_a - C21_a F8A_a - C8 F8B_a - C8 F8C_a - C8 C21B_b - Cl2B_b Si1B_b C22B_b - Si1B_b Si1B_b - C22B_b C21B_b C7 O6 Cl1B_b Cl1B_b - Si1B_b Cl2B_b - C21B_b F8D_b - C8 F8E_b - C8 F8F_b - C8 C2 - N1 C3 C3 - C2 C4 C8 C4 - C5 C3 C5 - C4 C6 Cl5 C6 - O6 N1 C5 C7 - N1 Si1_a Si1B_b C8 - F8A_a F8F_b F8E_b F8B_a F8C_a F8D_b C3 N1 - C2 C6 C7 O6 - C6 Si1_a Si1B_b Cl5 - C5 20770 Reflections read, of which 945 rejected -11 =< h =< 11, -9 =< k =< 9, -27 =< l =< 27, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 3152 Unique reflections, of which 0 suppressed R(int) = 0.0476 R(sigma) = 0.0349 Friedel opposites merged Maximum memory for data reduction = 2207 / 31459 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 = 2769 / 253412 wR2 = 0.2637 before cycle 1 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.071 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66568 0.00354 -0.163 OSF 2 0.80633 0.00568 -0.206 FVAR 2 3 0.52832 0.01191 -0.037 FVAR 3 Mean shift/su = 0.070 Maximum = -0.611 for z Cl2_a Max. shift = 0.019 A for C22B_b Max. dU = 0.000 for Cl2_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 2 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66565 0.00354 -0.009 OSF 2 0.80566 0.00568 -0.119 FVAR 2 3 0.52804 0.01188 -0.023 FVAR 3 Mean shift/su = 0.036 Maximum = -0.332 for z Cl2_a Max. shift = 0.007 A for H22F_b Max. dU = 0.000 for C21B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 3 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66568 0.00354 0.009 OSF 2 0.80561 0.00568 -0.007 FVAR 2 3 0.52780 0.01188 -0.021 FVAR 3 Mean shift/su = 0.010 Maximum = 0.097 for x Cl2_a Max. shift = 0.002 A for H22B_a Max. dU = 0.000 for C21B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 4 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66571 0.00354 0.009 OSF 2 0.80559 0.00569 -0.005 FVAR 2 3 0.52761 0.01188 -0.015 FVAR 3 Mean shift/su = 0.006 Maximum = -0.050 for z F8F_b Max. shift = 0.001 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 5 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66572 0.00354 0.002 OSF 2 0.80557 0.00569 -0.002 FVAR 2 3 0.52747 0.01188 -0.012 FVAR 3 Mean shift/su = 0.003 Maximum = -0.037 for z F8C_a Max. shift = 0.001 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 6 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.001 OSF 2 0.80556 0.00569 -0.003 FVAR 2 3 0.52736 0.01188 -0.010 FVAR 3 Mean shift/su = 0.002 Maximum = -0.031 for z F8C_a Max. shift = 0.001 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 7 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.001 OSF 2 0.80555 0.00569 -0.002 FVAR 2 3 0.52727 0.01188 -0.007 FVAR 3 Mean shift/su = 0.002 Maximum = -0.026 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 8 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.000 OSF 2 0.80554 0.00569 -0.001 FVAR 2 3 0.52720 0.01188 -0.006 FVAR 3 Mean shift/su = 0.001 Maximum = -0.021 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 9 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.001 OSF 2 0.80553 0.00569 -0.001 FVAR 2 3 0.52715 0.01188 -0.005 FVAR 3 Mean shift/su = 0.001 Maximum = -0.017 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 10 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.000 OSF 2 0.80553 0.00569 -0.001 FVAR 2 3 0.52710 0.01188 -0.004 FVAR 3 Mean shift/su = 0.001 Maximum = -0.014 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 11 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.000 OSF 2 0.80553 0.00569 -0.001 FVAR 2 3 0.52707 0.01188 -0.003 FVAR 3 Mean shift/su = 0.001 Maximum = -0.011 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 12 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66573 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52704 0.01188 -0.002 FVAR 3 Mean shift/su = 0.001 Maximum = -0.009 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 13 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52701 0.01188 -0.002 FVAR 3 Mean shift/su = 0.001 Maximum = -0.007 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 14 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52699 0.01188 -0.002 FVAR 3 Mean shift/su = 0.000 Maximum = -0.006 for z F8C_a Max. shift = 0.000 A for F8F_b Max. dU = 0.000 for C21B_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 15 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52698 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.005 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for C21B_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 16 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52696 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.004 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for C21B_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 17 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80552 0.00569 0.000 FVAR 2 3 0.52695 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.003 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for C21B_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 18 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80551 0.00569 0.000 FVAR 2 3 0.52694 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.003 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for C21B_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 19 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80551 0.00569 0.000 FVAR 2 3 0.52694 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.002 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for C21B_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 2769 / 253412 wR2 = 0.2635 before cycle 20 for 3152 data and 202 / 202 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.66574 0.00354 0.000 OSF 2 0.80551 0.00569 0.000 FVAR 2 3 0.52693 0.01188 -0.001 FVAR 3 Mean shift/su = 0.000 Maximum = -0.002 for z F8C_a Max. shift = 0.000 A for F8A_a Max. dU = 0.000 for F8C_a Largest correlation matrix elements -0.775 U33 Cl1B_b / z Cl1_a -0.685 U13 Cl1B_b / x Cl1_a 0.657 U33 Cl1B_b / U33 Cl1_a 0.763 x Cl1B_b / U11 Cl1_a 0.684 U13 Cl1B_b / U11 Cl1B_b 0.654 U13 Cl1_a / U11 Cl1_a 0.753 z Cl1B_b / U33 Cl1_a 0.674 y Cl1B_b / U22 Cl1_a 0.643 U11 F8B_a / FVAR 3 -0.751 x Cl1B_b / x Cl1_a 0.672 U12 Cl1B_b / x Cl1B_b -0.643 U33 Cl1_a / z Cl1_a -0.723 U22 Cl1B_b / y Cl1_a 0.669 x Cl1B_b / U13 Cl1_a 0.636 U33 Cl1B_b / z Cl1B_b 0.707 U22 Cl1B_b / U22 Cl1_a 0.666 y Cl1B_b / z Cl1_a 0.632 y Si1B_b / z Si1_a -0.700 U11 Cl1B_b / x Cl1_a 0.665 U12 Cl1B_b / U11 Cl1_a 0.625 U11 F8C_a / FVAR 3 0.693 z Cl1B_b / y Cl1_a 0.658 U13 Cl1B_b / x Cl1B_b -0.623 U22 Cl1_a / y Cl1_a Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H21A 0.2490 0.3570 0.0413 23 0.990 0.000 C21_a Cl2_a Si1_a H21B 0.3934 0.3635 0.0082 23 0.990 0.000 C21_a Cl2_a Si1_a H22A 0.5578 0.6557 0.1126 137 0.980 0.000 C22_a Si1_a H22A_a H22B 0.5747 0.6101 0.1882 137 0.980 0.000 C22_a Si1_a H22A_a H22C 0.4133 0.6596 0.1451 137 0.980 0.000 C22_a Si1_a H22A_a H21C 0.4693 0.5997 0.0668 23 0.990 0.000 C21B_b Cl2B_b Si1B_b H21D 0.3452 0.5944 0.1112 23 0.990 0.000 C21B_b Cl2B_b Si1B_b H22D 0.3758 0.0825 0.0221 33 0.980 0.000 C22B_b Si1B_b H22D_b H22E 0.3343 0.2820 -0.0066 33 0.980 0.000 C22B_b Si1B_b H22D_b H22F 0.2292 0.1839 0.0354 33 0.980 0.000 C22B_b Si1B_b H22D_b H2 0.7808 -0.1007 0.2082 43 0.950 0.000 C2 N1 C3 H4 1.0568 0.0235 0.0861 43 0.950 0.000 C4 C5 C3 H7A 0.6010 0.1882 0.2194 23 0.990 0.000 C7 N1 Si1_a H7B 0.5079 0.0494 0.1675 23 0.990 0.000 C7 N1 Si1_a 2009src0344 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C21_a 0.35075 0.30648 0.04310 0.80551 0.02584 0.06730 0.03266 0.01389 0.00227 -0.00494 0.04246 0.01334 0.00072 0.00111 0.00031 0.00569 0.00291 0.00477 0.00304 0.00316 0.00236 0.00298 0.00167 H21A_a 0.24896 0.35697 0.04127 0.80551 0.05095 0.00569 0.00000 H21B_a 0.39339 0.36351 0.00820 0.80551 0.05095 0.00569 0.00000 C22_a 0.50926 0.59878 0.14509 0.80551 0.04568 0.03530 0.07236 -0.00841 0.02621 -0.00022 0.04910 0.02149 0.00112 0.00102 0.00055 0.00569 0.00448 0.00374 0.00590 0.00399 0.00445 0.00345 0.00181 H22A_a 0.55781 0.65572 0.11256 0.80551 0.07365 0.00569 0.00000 H22B_a 0.57474 0.61009 0.18815 0.80551 0.07365 0.00569 0.00000 H22C_a 0.41328 0.65958 0.14512 0.80551 0.07365 0.00569 0.00000 Si1_a 0.47513 0.35477 0.12512 0.80551 0.02029 0.03003 0.02888 -0.00127 0.00584 -0.00143 0.02628 0.00526 0.00024 0.00031 0.00012 0.00569 0.00091 0.00103 0.00103 0.00076 0.00075 0.00072 0.00048 Cl1_a 0.28819 0.32081 0.17920 0.80551 0.03361 0.05095 0.04801 -0.00555 0.02097 -0.00008 0.04239 0.00634 0.00045 0.00051 0.00019 0.00569 0.00142 0.00182 0.00172 0.00109 0.00120 0.00113 0.00071 Cl2_a 0.34086 0.06291 0.03240 0.80551 0.06426 0.10275 0.07528 -0.06053 -0.00621 -0.00009 0.08367 0.00374 0.00028 0.00041 0.00012 0.00569 0.00143 0.00213 0.00153 0.00147 0.00110 0.00128 0.00105 F8A_a 1.01588 -0.26591 0.23480 0.52693 0.09455 0.02387 0.00133 0.00165 0.00055 0.01188 0.00363 F8B_a 1.00527 -0.36096 0.13423 0.52693 0.07083 0.01793 0.00112 0.00125 0.00042 0.01188 0.00276 F8C_a 1.17375 -0.18668 0.17942 0.52693 0.09147 0.02040 0.00125 0.00142 0.00057 0.01188 0.00363 C21B_b 0.44509 0.54820 0.10694 0.19449 0.03906 0.04400 0.03997 -0.00481 0.00357 -0.00021 0.04165 0.05822 0.00338 0.00416 0.00145 0.00569 0.01450 0.01568 0.01398 0.01250 0.01198 0.01217 0.00618 H21C_b 0.46935 0.59968 0.06679 0.19449 0.04998 0.00569 0.00000 H21D_b 0.34522 0.59438 0.11122 0.19449 0.04998 0.00569 0.00000 C22B_b 0.33300 0.20064 0.03018 0.19449 0.04568 0.03530 0.07236 -0.00841 0.02621 -0.00022 0.04910 0.04065 0.00328 0.00453 0.00127 0.00569 0.00448 0.00374 0.00590 0.00399 0.00445 0.00345 0.00181 H22D_b 0.37578 0.08250 0.02208 0.19449 0.07365 0.00569 0.00000 H22E_b 0.33434 0.28197 -0.00665 0.19449 0.07365 0.00569 0.00000 H22F_b 0.22916 0.18386 0.03544 0.19449 0.07365 0.00569 0.00000 Si1B_b 0.44151 0.29799 0.10226 0.19449 0.01791 0.03770 0.03453 -0.00046 0.00558 -0.00203 0.03001 0.02307 0.00095 0.00144 0.00052 0.00569 0.00363 0.00480 0.00472 0.00362 0.00322 0.00312 0.00199 Cl1B_b 0.26682 0.26964 0.16360 0.19449 0.02769 0.06144 0.05149 -0.00578 0.02411 -0.00842 0.04460 0.02592 0.00178 0.00227 0.00079 0.00569 0.00475 0.00882 0.00754 0.00493 0.00494 0.00486 0.00302 Cl2B_b 0.58494 0.61638 0.17621 0.19449 0.07096 0.04726 0.07453 -0.01332 0.00268 -0.01314 0.06598 0.01973 0.00143 0.00128 0.00054 0.00569 0.00670 0.00474 0.00660 0.00430 0.00539 0.00448 0.00307 F8D_b 0.95356 -0.35314 0.20746 0.47307 0.08110 0.02305 0.00131 0.00156 0.00055 0.01188 0.00350 F8E_b 1.09495 -0.30253 0.13579 0.47307 0.10413 0.02787 0.00179 0.00188 0.00067 0.01188 0.00448 F8F_b 1.13624 -0.17871 0.22429 0.47307 0.09851 0.02443 0.00152 0.00171 0.00067 0.01188 0.00436 C2 0.80502 -0.02760 0.17446 1.00000 0.03906 0.03563 0.03023 0.00255 0.00227 0.00891 0.03566 0.00928 0.00057 0.00069 0.00023 0.00000 0.00258 0.00253 0.00218 0.00191 0.00190 0.00204 0.00106 H2 0.78082 -0.10066 0.20818 1.00000 0.04279 0.00000 0.00000 C3 0.93102 -0.06351 0.15156 1.00000 0.04259 0.04836 0.03478 0.00135 0.00315 0.01702 0.04259 0.01064 0.00063 0.00080 0.00024 0.00000 0.00282 0.00302 0.00243 0.00226 0.00209 0.00240 0.00123 C4 0.96786 0.04621 0.10194 1.00000 0.03208 0.04513 0.04101 -0.00817 0.00841 0.00581 0.03927 0.00958 0.00057 0.00076 0.00025 0.00000 0.00245 0.00285 0.00258 0.00222 0.00203 0.00210 0.00114 H4 1.05684 0.02355 0.08609 1.00000 0.04713 0.00000 0.00000 C5 0.87503 0.18379 0.07727 1.00000 0.03059 0.03282 0.03802 -0.00045 0.01089 -0.00160 0.03326 0.00911 0.00055 0.00065 0.00024 0.00000 0.00233 0.00236 0.00240 0.00190 0.00190 0.00184 0.00101 C6 0.74204 0.22081 0.10067 1.00000 0.02568 0.02660 0.03693 0.00129 0.00902 0.00009 0.02936 0.00858 0.00050 0.00061 0.00022 0.00000 0.00211 0.00213 0.00228 0.00178 0.00177 0.00169 0.00093 C7 0.57529 0.15663 0.17265 1.00000 0.02438 0.04374 0.03569 0.00762 0.00898 0.00404 0.03420 0.00981 0.00053 0.00071 0.00024 0.00000 0.00217 0.00263 0.00235 0.00203 0.00182 0.00190 0.00103 H7A_a 0.60100 0.18822 0.21940 1.00000 0.04104 0.00000 0.00000 H7B_a 0.50792 0.04940 0.16749 1.00000 0.04104 0.00000 0.00000 C8 1.02748 -0.22431 0.17731 1.00000 0.05987 0.11069 0.04355 0.01619 0.01344 0.03795 0.07096 0.01719 0.00086 0.00131 0.00033 0.00000 0.00417 0.00639 0.00324 0.00378 0.00298 0.00431 0.00225 N1 0.71341 0.11154 0.14966 1.00000 0.02427 0.03225 0.02944 0.00112 0.00614 0.00243 0.02856 0.00694 0.00041 0.00053 0.00018 0.00000 0.00179 0.00192 0.00180 0.00152 0.00145 0.00148 0.00081 O6 0.64804 0.34555 0.08094 1.00000 0.02887 0.04129 0.05488 0.01920 0.01892 0.00853 0.04021 0.00761 0.00039 0.00050 0.00019 0.00000 0.00173 0.00194 0.00213 0.00165 0.00157 0.00145 0.00088 Cl5 0.90832 0.31599 0.01449 1.00000 0.04217 0.04503 0.06743 0.01192 0.03248 0.00170 0.04852 0.00310 0.00016 0.00019 0.00008 0.00000 0.00075 0.00075 0.00092 0.00062 0.00066 0.00055 0.00043 Final Structure Factor Calculation for 2009src0344 in P2(1)/c Total number of l.s. parameters = 202 Maximum vector length = 511 Memory required = 2567 / 26061 wR2 = 0.2635 before cycle 21 for 3152 data and 0 / 202 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1264 * P )^2 + 6.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0947 for 2466 Fo > 4sig(Fo) and 0.1116 for all 3152 data wR2 = 0.2635, GooF = S = 1.070, Restrained GooF = 1.070 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0739 0.0286 0.0248 C21_a 0.0775 0.0390 0.0308 C22_a 0.0309 0.0281 0.0198 Si1_a 0.0569 0.0476 0.0226 Cl1_a 0.1577 0.0684 0.0249 Cl2_a 0.0488 0.0416 0.0346 C21B_b 0.0775 0.0390 0.0308 C22B_b 0.0379 0.0346 0.0175 Si1B_b 0.0678 0.0510 0.0150 Cl1B_b 0.0882 0.0735 0.0362 Cl2B_b 0.0476 0.0341 0.0253 C2 0.0638 0.0367 0.0272 C3 0.0533 0.0374 0.0272 C4 0.0392 0.0330 0.0276 C5 0.0373 0.0265 0.0243 C6 0.0487 0.0311 0.0228 C7 0.1317 0.0437 0.0375 C8 0.0332 0.0291 0.0234 N1 0.0703 0.0278 0.0225 O6 0.0793 0.0432 0.0230 Cl5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.030 0.042 0.056 0.073 0.096 0.129 0.190 1.000 Number in group 341. 311. 297. 311. 329. 313. 315. 308. 314. 313. GooF 0.942 0.998 0.977 1.054 1.145 1.013 1.274 1.125 1.164 0.957 K 4.617 1.489 1.139 1.086 1.058 0.983 1.034 1.026 1.043 0.996 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 329. 307. 310. 315. 325. 308. 312. 318. 311. 317. GooF 0.738 0.813 0.854 0.920 0.994 1.086 1.197 1.238 1.268 1.391 K 0.984 1.063 1.031 1.031 1.041 1.036 1.055 1.037 1.042 0.983 R1 0.181 0.171 0.168 0.147 0.133 0.125 0.114 0.099 0.087 0.070 Recommended weighting scheme: WGHT 0.1248 6.1193 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 4592.42 10551.34 4.96 0.710 5.98 3 3 3 213.04 59.62 4.96 0.053 1.76 4 3 5 60.75 3.91 4.34 0.014 1.45 2 3 3 505.52 235.50 4.26 0.106 1.99 4 4 1 57.54 3.79 4.15 0.013 1.40 2 3 6 152.27 37.12 4.14 0.042 1.74 4 4 6 61.23 8.45 3.81 0.020 1.25 5 5 5 200.97 454.28 3.66 0.147 1.06 -1 0 14 53.20 6.61 3.59 0.018 1.50 4 4 4 356.36 175.09 3.58 0.091 1.32 -3 1 16 98.30 27.48 3.58 0.036 1.26 3 1 2 156.62 61.84 3.40 0.054 2.54 -2 0 14 124.06 296.19 3.39 0.119 1.49 4 5 4 26.92 115.66 3.37 0.074 1.16 -2 3 4 142.46 54.66 3.35 0.051 2.05 -3 1 9 472.85 258.25 3.35 0.111 1.95 3 2 4 30.32 118.74 3.30 0.075 1.99 4 3 2 114.06 270.09 3.29 0.114 1.59 0 1 1 30.87 120.63 3.25 0.076 6.92 0 2 3 45.66 7.61 3.20 0.019 3.24 4 5 5 29.74 1.54 3.18 0.009 1.14 -2 2 1 698.54 415.87 3.18 0.141 2.86 -6 0 8 39.43 129.67 3.13 0.079 1.42 4 5 7 285.61 144.53 3.11 0.083 1.09 4 5 3 288.15 154.20 2.97 0.086 1.18 5 6 3 196.32 93.04 2.95 0.067 0.98 1 5 1 91.65 32.80 2.94 0.040 1.44 0 0 12 1125.68 724.79 2.94 0.186 1.71 5 5 7 167.91 78.54 2.89 0.061 1.01 -1 4 2 31.33 3.90 2.88 0.014 1.78 7 3 4 134.93 58.89 2.87 0.053 1.06 6 6 5 81.05 24.46 2.87 0.034 0.90 7 1 6 84.99 29.55 2.85 0.038 1.11 -5 5 3 57.56 15.56 2.84 0.027 1.14 4 4 0 34.98 5.20 2.84 0.016 1.42 0 2 1 71.49 24.27 2.75 0.034 3.62 3 4 15 29.53 2.33 2.75 0.011 0.98 0 2 7 33.40 100.96 2.72 0.069 2.30 6 2 6 43.60 118.38 2.70 0.075 1.20 2 3 8 877.47 576.39 2.70 0.166 1.57 2 3 2 95.27 38.71 2.69 0.043 2.06 -7 4 2 67.46 19.60 2.68 0.031 1.06 -2 4 17 100.89 41.07 2.67 0.044 1.02 -4 5 13 34.78 5.87 2.66 0.017 1.03 -6 2 5 978.49 651.29 2.65 0.176 1.39 4 0 4 2663.72 1848.39 2.64 0.297 1.90 -7 0 10 1357.42 909.90 2.63 0.208 1.20 -1 3 2 654.40 424.46 2.63 0.142 2.33 -4 6 8 74.86 27.24 2.62 0.036 1.03 4 1 4 931.45 622.30 2.62 0.172 1.84 Bond lengths and angles C21_a - Distance Angles Cl2_a 1.8035 (0.0086) Si1_a 1.8920 (0.0070) 107.75 (0.35) H21A_a 0.9900 110.16 110.16 H21B_a 0.9900 110.16 110.16 108.46 C21_a - Cl2_a Si1_a H21A_a C22_a - Distance Angles Si1_a 1.8528 (0.0088) H22A_a 0.9800 109.47 H22B_a 0.9800 109.47 109.47 H22C_a 0.9800 109.47 109.47 109.47 C22_a - Si1_a H22A_a H22B_a Si1_a - Distance Angles C22_a 1.8528 (0.0089) C7 1.8906 (0.0051) 125.80 (0.45) C21_a 1.8920 (0.0070) 115.41 (0.46) 118.08 (0.32) O6 1.9829 (0.0038) 91.56 (0.28) 83.06 (0.19) 87.13 (0.25) Cl1_a 2.2426 (0.0044) 95.85 (0.26) 88.81 (0.19) 93.88 (0.23) 171.24 (0.18) Si1_a - C22_a C7 C21_a O6 Cl1_a - Distance Angles Si1_a 2.2426 (0.0044) Cl1_a - Cl2_a - Distance Angles C21_a 1.8035 (0.0086) Cl2_a - F8A_a - Distance Angles C8 1.2715 (0.0124) F8A_a - F8B_a - Distance Angles C8 1.3394 (0.0123) F8B_a - F8C_a - Distance Angles C8 1.3495 (0.0135) F8C_a - C21B_b - Distance Angles Cl2B_b 1.7972 (0.0323) Si1B_b 1.8407 (0.0322) 108.88 (1.59) H21C_b 0.9900 109.91 109.91 H21D_b 0.9900 109.91 109.91 108.31 C21B_b - Cl2B_b Si1B_b H21C_b C22B_b - Distance Angles Si1B_b 1.7801 (0.0185) H22D_b 0.9800 109.47 H22E_b 0.9800 109.47 109.47 H22F_b 0.9800 109.47 109.47 109.47 C22B_b - Si1B_b H22D_b H22E_b Si1B_b - Distance Angles C22B_b 1.7801 (0.0185) C21B_b 1.8407 (0.0322) 116.58 (1.56) C7 2.0027 (0.0097) 124.58 (1.33) 118.48 (1.15) O6 2.0466 (0.0084) 104.80 (1.16) 80.46 (1.02) 78.75 (0.34) Cl1B_b 2.2498 (0.0171) 96.75 (1.15) 93.94 (1.08) 85.50 (0.59) 158.00 (0.67) Si1B_b - C22B_b C21B_b C7 O6 Cl1B_b - Distance Angles Si1B_b 2.2498 (0.0171) Cl1B_b - Cl2B_b - Distance Angles C21B_b 1.7972 (0.0323) Cl2B_b - F8D_b - Distance Angles C8 1.3865 (0.0140) F8D_b - F8E_b - Distance Angles C8 1.2988 (0.0155) F8E_b - F8F_b - Distance Angles C8 1.2905 (0.0142) F8F_b - C2 - Distance Angles N1 1.3537 (0.0059) C3 1.3555 (0.0075) 120.52 (0.47) H2 0.9500 119.74 119.74 C2 - N1 C3 C3 - Distance Angles C2 1.3555 (0.0075) C4 1.4116 (0.0080) 119.76 (0.47) C8 1.5044 (0.0087) 119.83 (0.53) 120.37 (0.51) C3 - C2 C4 C4 - Distance Angles C5 1.3503 (0.0071) C3 1.4116 (0.0080) 119.17 (0.47) H4 0.9500 120.42 120.42 C4 - C5 C3 C5 - Distance Angles C4 1.3503 (0.0071) C6 1.4210 (0.0065) 121.27 (0.45) Cl5 1.7144 (0.0050) 121.67 (0.39) 117.02 (0.37) C5 - C4 C6 C6 - Distance Angles O6 1.2636 (0.0055) N1 1.3719 (0.0058) 116.84 (0.40) C5 1.4210 (0.0065) 126.22 (0.43) 116.93 (0.40) C6 - O6 N1 C7 - Distance Angles N1 1.4719 (0.0058) Si1_a 1.8906 (0.0051) 110.52 (0.32) Si1B_b 2.0027 (0.0097) 107.68 (0.38) 19.30 (0.30) H7A_a 0.9900 109.55 109.55 126.60 H7B_a 0.9900 109.55 109.55 93.62 108.10 C7 - N1 Si1_a Si1B_b H7A_a C8 - Distance Angles F8A_a 1.2715 (0.0124) F8F_b 1.2905 (0.0142) 62.25 (0.82) F8E_b 1.2988 (0.0155) 132.42 (1.04) 103.66 (1.03) F8B_a 1.3394 (0.0123) 115.60 (1.02) 134.27 (0.91) 40.59 (0.68) F8C_a 1.3495 (0.0136) 106.88 (0.88) 47.66 (0.71) 61.03 (0.83) 100.78 (0.77) F8D_b 1.3865 (0.0140) 42.24 (0.63) 101.20 (0.86) 110.15 (1.07) 77.13 (0.83) 133.69 (0.84) C3 1.5044 (0.0087) 112.05 (0.75) 111.74 (0.92) 115.21 (0.78) 110.43 (0.64) 110.40 (0.82) 113.54 (0.70) C8 - F8A_a F8F_b F8E_b F8B_a F8C_a F8D_b N1 - Distance Angles C2 1.3537 (0.0059) C6 1.3719 (0.0058) 122.34 (0.40) C7 1.4719 (0.0058) 122.83 (0.40) 114.83 (0.37) N1 - C2 C6 O6 - Distance Angles C6 1.2636 (0.0056) Si1_a 1.9829 (0.0038) 114.73 (0.30) Si1B_b 2.0466 (0.0085) 113.14 (0.37) 18.82 (0.30) O6 - C6 Si1_a Cl5 - Distance Angles C5 1.7144 (0.0050) Cl5 - FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -1 2.500 2 1 R1 = 0.1112 for 3152 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.68 at 0.4087 0.0902 0.0104 [ 0.43 A from H22D ] Deepest hole -0.91 at 0.2771 0.0191 0.0508 [ 0.82 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 2764 / 26809 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4087 0.0902 0.0104 1.00000 0.05 1.68 0.43 H22D 0.87 CL2 1.19 C22B 1.57 H22E Q2 1 1.0806 -0.1862 0.2494 1.00000 0.05 1.46 0.80 F8F 0.84 F8A 1.52 C8 1.79 F8D Q3 1 0.9672 -0.3787 0.1694 1.00000 0.05 1.43 0.86 F8D 0.89 F8B 1.26 C8 1.58 F8E Q4 1 1.1692 -0.2060 0.1505 1.00000 0.05 1.25 0.62 F8C 0.98 F8E 1.51 C8 1.65 F8F Q5 1 1.1785 -0.1635 0.2064 1.00000 0.05 1.18 0.59 F8C 0.60 F8F 1.45 C8 1.83 F8E Q6 1 0.9690 -0.3117 0.2265 1.00000 0.05 1.12 0.50 F8D 0.54 F8A 1.41 C8 1.82 F8F Q7 1 1.1941 -0.1581 0.1588 1.00000 0.05 0.99 0.55 F8C 1.41 F8E 1.58 F8F 1.71 C8 Q8 1 1.0433 -0.3379 0.1246 1.00000 0.05 0.87 0.47 F8B 0.55 F8E 1.42 C8 1.85 F8C Q9 1 0.3487 0.0317 0.0498 1.00000 0.05 0.66 0.42 CL2 0.77 H22D 1.31 C22B 1.54 H22F Q10 1 0.6002 0.2898 0.0480 1.00000 0.05 0.50 0.84 O6 1.60 C6 1.97 H21B 2.01 SI1B Shortest distances between peaks (including symmetry equivalents) 4 7 0.43 5 7 1.04 1 9 1.16 4 5 1.20 3 6 1.29 3 8 1.31 2 6 1.38 2 5 1.40 4 8 1.51 7 8 1.93 1 1 2.23 2 3 2.28 1 10 2.29 5 8 2.29 5 6 2.31 3 4 2.33 2 7 2.35 6 8 2.38 2 4 2.38 3 5 2.49 3 7 2.67 4 6 2.77 2 8 2.81 2 6 2.85 1 9 2.90 2 3 2.92 6 7 2.94 9 10 2.97 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 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.02: 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 3.13: Structure factors and derivatives 4.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 0.58: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0344 finished at 11:39:54 Total CPU time: 9.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++