+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 05src0140 started at 09:42:28 on 10-Feb-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 05src0140 in P2(1)/c CELL 0.71073 11.2450 9.0486 34.6489 90.000 97.632 90.000 ZERR 4.00 0.0007 0.0008 0.0018 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL FE UNIT 132 192 8 8 12 4 V = 3494.35 F(000) = 1412.0 Mu = 0.69 mm-1 Cell Wt = 2667.74 Rho = 1.268 MERG 2 OMIT -3.00 55.00 OMIT 0 1 5 OMIT 0 3 5 SHEL 7 0.77 DELU 0.02 C41 > CL52 SIMU 0.02 C41 > CL52 SIMU 0.005 C41 C51 FMAP 2 PLAN 10 SIZE 0.08 0.22 0.32 ACTA BOND $H WGHT 0.04410 3.86610 L.S. 40 TEMP -153.00 FVAR 0.39918 0.57386 MOLE 1 C1 1 -0.065031 0.537300 0.263005 11.00000 0.02158 0.02893 = 0.02609 -0.00299 0.00482 0.00520 AFIX 23 H1A 2 -0.065248 0.640510 0.253515 11.00000 -1.20000 H1B 2 -0.081033 0.538094 0.290420 11.00000 -1.20000 AFIX 0 C2 1 -0.159713 0.446699 0.237972 11.00000 0.01808 0.03398 = 0.02867 -0.00144 0.00538 0.00317 AFIX 23 H2A 2 -0.177658 0.355504 0.251891 11.00000 -1.20000 H2B 2 -0.234697 0.504512 0.232158 11.00000 -1.20000 AFIX 0 C3 1 0.121056 0.431129 0.290899 11.00000 0.01951 0.02116 = 0.02324 -0.00410 0.00420 -0.00558 AFIX 43 H3 2 0.094646 0.451191 0.315297 11.00000 -1.20000 AFIX 0 C4 1 0.237090 0.362596 0.291246 11.00000 0.01970 0.02130 = 0.02290 -0.00065 0.00083 -0.00293 C5 1 0.283922 0.323345 0.256519 11.00000 0.01991 0.01458 = 0.02313 0.00239 -0.00012 -0.00341 C6 1 0.401502 0.265464 0.258976 11.00000 0.01820 0.01362 = 0.02621 -0.00059 0.00144 -0.00503 C7 1 0.466361 0.251218 0.295839 11.00000 0.01831 0.01612 = 0.03163 0.00231 -0.00016 -0.00106 AFIX 43 H7 2 0.545973 0.214293 0.297548 11.00000 -1.20000 AFIX 0 C8 1 0.422525 0.287520 0.330666 11.00000 0.02476 0.01704 = 0.02504 0.00056 -0.00239 -0.00448 C9 1 0.306676 0.341956 0.327485 11.00000 0.02680 0.02469 = 0.02196 0.00027 0.00362 -0.00492 AFIX 43 H9 2 0.273399 0.365998 0.350500 11.00000 -1.20000 AFIX 0 C10 1 0.454735 0.221796 0.222027 11.00000 0.01735 0.01964 = 0.02740 0.00117 0.00381 0.00110 C11 1 0.379755 0.095028 0.201497 11.00000 0.02077 0.02477 = 0.03067 -0.00527 0.00496 -0.00032 AFIX 137 H11A 2 0.296536 0.127714 0.194664 11.00000 -1.50000 H11B 2 0.382067 0.009669 0.218990 11.00000 -1.50000 H11C 2 0.412965 0.067059 0.177779 11.00000 -1.50000 AFIX 0 C12 1 0.456059 0.353522 0.194014 11.00000 0.02229 0.02671 = 0.03359 0.00467 0.00872 0.00363 AFIX 137 H12A 2 0.509307 0.430665 0.206346 11.00000 -1.50000 H12B 2 0.374633 0.393132 0.187871 11.00000 -1.50000 H12C 2 0.485082 0.320679 0.169982 11.00000 -1.50000 AFIX 0 C13 1 0.583920 0.168407 0.231187 11.00000 0.02152 0.02530 = 0.03577 -0.00144 0.00680 0.00101 AFIX 137 H13A 2 0.615207 0.144078 0.206878 11.00000 -1.50000 H13B 2 0.586520 0.080281 0.247719 11.00000 -1.50000 H13C 2 0.633115 0.246526 0.244856 11.00000 -1.50000 AFIX 0 C14 1 0.497015 0.267368 0.370691 11.00000 0.02890 0.03020 = 0.02481 0.00292 -0.00680 -0.00412 C15 1 0.445350 0.136048 0.391376 11.00000 0.04828 0.04779 = 0.03308 0.01226 -0.00928 -0.01388 AFIX 137 H15A 2 0.361591 0.156499 0.394515 11.00000 -1.50000 H15B 2 0.492221 0.121731 0.417033 11.00000 -1.50000 H15C 2 0.449375 0.046385 0.375738 11.00000 -1.50000 AFIX 0 C16 1 0.491387 0.408304 0.395178 11.00000 0.03579 0.04510 = 0.02433 -0.00454 -0.00489 -0.00183 AFIX 137 H16A 2 0.521954 0.492165 0.381540 11.00000 -1.50000 H16B 2 0.540561 0.395139 0.420491 11.00000 -1.50000 H16C 2 0.408060 0.427431 0.399109 11.00000 -1.50000 AFIX 0 C17 1 0.629252 0.233136 0.367672 11.00000 0.02946 0.04719 = 0.03518 -0.00152 -0.00880 0.00272 AFIX 137 H17A 2 0.635048 0.137907 0.354580 11.00000 -1.50000 H17B 2 0.674462 0.228593 0.393850 11.00000 -1.50000 H17C 2 0.662614 0.311068 0.352660 11.00000 -1.50000 AFIX 0 C18 1 -0.187442 0.376092 0.171259 11.00000 0.01683 0.02819 = 0.03130 -0.00030 0.00182 0.00259 AFIX 43 H18 2 -0.270416 0.384808 0.173531 11.00000 -1.20000 AFIX 0 C19 1 -0.156426 0.327422 0.134297 11.00000 0.02594 0.02521 = 0.02620 -0.00005 -0.00015 0.00077 C20 1 -0.037737 0.293774 0.128689 11.00000 0.02245 0.02413 = 0.02793 -0.00171 -0.00343 0.00623 C21 1 -0.015350 0.241272 0.091625 11.00000 0.03188 0.04519 = 0.02936 -0.00690 -0.00165 0.01739 C22 1 -0.112139 0.234236 0.062474 11.00000 0.04026 0.04735 = 0.02561 -0.00765 -0.00350 0.01735 AFIX 43 H22 2 -0.096773 0.204505 0.037310 11.00000 -1.20000 AFIX 0 C23 1 -0.231914 0.267835 0.067259 11.00000 0.03328 0.03606 = 0.02921 -0.00370 -0.00664 0.01211 C24 1 -0.251774 0.311507 0.103473 11.00000 0.02527 0.03059 = 0.03394 -0.00110 -0.00423 0.00645 AFIX 43 H24 2 -0.331487 0.331787 0.108175 11.00000 -1.20000 AFIX 0 C25 1 0.111249 0.192091 0.085147 11.00000 0.03583 0.09834 = 0.03183 -0.02442 -0.00348 0.02853 C26 1 0.148438 0.059349 0.111567 11.00000 0.05447 0.07984 = 0.06270 -0.02745 -0.02188 0.04036 AFIX 137 H26A 2 0.229258 0.027372 0.107676 11.00000 -1.50000 H26B 2 0.091761 -0.021981 0.105064 11.00000 -1.50000 H26C 2 0.148049 0.087867 0.138835 11.00000 -1.50000 AFIX 0 C27 1 0.114605 0.140712 0.042932 11.00000 0.05734 0.19676 = 0.04132 -0.04699 -0.00594 0.06608 AFIX 137 H27A 2 0.098449 0.224966 0.025241 11.00000 -1.50000 H27B 2 0.053481 0.064443 0.036213 11.00000 -1.50000 H27C 2 0.194021 0.100030 0.040479 11.00000 -1.50000 AFIX 0 C28 1 0.202532 0.317093 0.093639 11.00000 0.03858 0.13578 = 0.05347 -0.00633 0.01863 0.01015 AFIX 137 H28A 2 0.177283 0.402172 0.077048 11.00000 -1.50000 H28B 2 0.281443 0.283183 0.088251 11.00000 -1.50000 H28C 2 0.207359 0.346015 0.121059 11.00000 -1.50000 AFIX 0 C29 1 -0.331357 0.258010 0.032383 11.00000 0.03933 0.05832 = 0.03044 -0.00798 -0.01376 0.01738 C30 1 -0.326053 0.107744 0.012449 11.00000 0.06548 0.10216 = 0.05835 -0.05120 -0.03160 0.03624 AFIX 137 H30A 2 -0.395217 0.097367 -0.007785 11.00000 -1.50000 H30B 2 -0.327724 0.028899 0.031760 11.00000 -1.50000 H30C 2 -0.251820 0.100706 0.000601 11.00000 -1.50000 AFIX 0 C31 1 -0.456120 0.273197 0.044414 11.00000 0.03681 0.05362 = 0.04521 -0.00977 -0.01621 0.00864 AFIX 137 H31A 2 -0.465595 0.372527 0.054858 11.00000 -1.50000 H31B 2 -0.466512 0.199544 0.064431 11.00000 -1.50000 H31C 2 -0.516592 0.257299 0.021698 11.00000 -1.50000 AFIX 0 C32 1 -0.312357 0.385536 0.004507 11.00000 0.05816 0.12983 = 0.05117 0.03989 -0.01526 0.00292 AFIX 137 H32A 2 -0.373903 0.381025 -0.018312 11.00000 -1.50000 H32B 2 -0.232742 0.376771 -0.003846 11.00000 -1.50000 H32C 2 -0.318319 0.480079 0.017913 11.00000 -1.50000 AFIX 0 N1 3 0.050868 0.466982 0.259969 11.00000 0.01996 0.02151 = 0.02513 -0.00187 0.00338 -0.00028 N2 3 -0.112325 0.409004 0.201649 11.00000 0.01933 0.02626 = 0.02442 -0.00061 0.00254 0.00271 O1 4 0.218444 0.339903 0.222124 11.00000 0.01743 0.02576 = 0.02154 -0.00070 0.00160 0.00277 O2 4 0.051433 0.305893 0.157523 11.00000 0.02287 0.03434 = 0.02583 -0.00752 -0.00156 0.00902 CL1 5 0.097540 0.660481 0.181923 11.00000 0.04035 0.02731 = 0.03804 0.00620 0.00978 0.00243 FE1 6 0.072801 0.428863 0.202007 11.00000 0.01720 0.02215 = 0.02233 -0.00071 0.00209 0.00244 MOLE 2 PART 2 C41 1 0.065010 0.337908 -0.081034 21.00000 0.07855 0.08783 = 0.10106 0.03076 0.04028 0.03114 AFIX 23 H41A 2 0.031943 0.347057 -0.108870 21.00000 -1.20000 H41B 2 0.115373 0.425958 -0.073844 21.00000 -1.20000 AFIX 0 CL41 5 0.151179 0.185681 -0.074925 21.00000 0.05605 0.07788 = 0.07728 0.03107 0.03842 0.02517 CL42 5 -0.055113 0.334460 -0.052629 21.00000 0.07752 0.10364 = 0.08110 0.01160 0.02464 0.03140 PART 1 C51 1 0.059409 0.350283 -0.080954 -21.00000 0.07397 0.05939 = 0.02716 0.02588 -0.00897 -0.00517 AFIX 23 H51A 2 -0.009696 0.342925 -0.101781 -21.00000 -1.20000 H51B 2 0.112128 0.431200 -0.087752 -21.00000 -1.20000 AFIX 0 CL51 5 0.140526 0.180091 -0.077214 -21.00000 0.16141 0.18408 = 0.19816 0.04429 0.07274 0.07426 CL52 5 0.008769 0.388572 -0.036678 -21.00000 0.13615 0.08869 = 0.09122 0.02431 0.04774 0.03242 HKLF 4 Covalent radii and connectivity table for 05src0140 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 FE 1.240 C1 - N1 C2 C2 - N2 C1 C3 - N1 C4 C4 - C9 C5 C3 C5 - O1 C6 C4 C6 - C7 C5 C10 C7 - C6 C8 C8 - C9 C7 C14 C9 - C8 C4 C10 - C13 C6 C12 C11 C11 - C10 C12 - C10 C13 - C10 C14 - C8 C17 C16 C15 C15 - C14 C16 - C14 C17 - C14 C18 - N2 C19 C19 - C20 C24 C18 C20 - O2 C19 C21 C21 - C22 C20 C25 C22 - C21 C23 C23 - C24 C22 C29 C24 - C23 C19 C25 - C28 C26 C21 C27 C26 - C25 C27 - C25 C28 - C25 C29 - C31 C30 C23 C32 C30 - C29 C31 - C29 C32 - C29 N1 - C3 C1 Fe1 N2 - C18 C2 Fe1 O1 - C5 Fe1 O2 - C20 Fe1 Cl1 - Fe1 Fe1 - O1 O2 N1 N2 Cl1 C41_b - Cl41_b Cl42_b Cl41_b - C41_b Cl42_b - C41_b C51_a - Cl52_a Cl51_a Cl51_a - C51_a Cl52_a - C51_a h k l Fo^2 Sigma Why rejected -6 0 3 22.73 5.16 observed but should be systematically absent 29735 Reflections read, of which 1237 rejected -14 =< h =< 14, -8 =< k =< 11, -38 =< l =< 44, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 9 2 55.15 8.76 4 45.02 9 3 9 122.59 6.21 6 39.07 1 5 15 29.45 1.57 3 9.44 8 1 17 400.49 14.78 4 89.73 5 2 25 181.63 11.75 3 147.77 -3 3 30 90.16 6.18 5 59.35 6 Inconsistent equivalents 7994 Unique reflections, of which 0 suppressed R(int) = 0.0601 R(sigma) = 0.0819 Friedel opposites merged Maximum memory for data reduction = 4470 / 79336 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 = 5702 / 529134 wR2 = 0.1322 before cycle 1 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0284 0.0050 SIMU U22 C41_b C51_a 0.0739 0.0050 SIMU U33 C41_b C51_a 0.0493 0.0050 SIMU U13 C41_b C51_a 0.0363 0.0050 SIMU U12 C41_b C51_a -0.1209 0.0400 SIMU U33 Cl41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.053 0.000 0.000 GooF = S = 1.045; Restrained GooF = 1.072 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39911 0.00060 -0.109 OSF 2 0.57299 0.01575 -0.055 FVAR 2 362 0.07958 0.00444 -4.833 U33 C41_b 364 0.02148 0.00372 -5.058 U13 C41_b 391 0.00407 0.00366 3.561 U13 C51_a 392 0.00755 0.00417 3.049 U12 C51_a Mean shift/esd = 0.092 Maximum = -5.058 for U13 C41_b Max. shift = 0.028 A for C51_a Max. dU =-0.011 for C41_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1324 before cycle 2 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0417 0.0050 SIMU U33 C41_b C51_a 0.0174 0.0050 SIMU U13 C41_b C51_a -0.1207 0.0400 SIMU U33 Cl41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.031 0.054 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.054 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39910 0.00059 -0.018 OSF 2 0.57035 0.01558 -0.169 FVAR 2 362 0.06094 0.00405 -4.601 U33 C41_b 389 0.05501 0.00373 4.586 U33 C51_a Mean shift/esd = 0.061 Maximum = -4.601 for U33 C41_b Max. shift = 0.028 A for H51A_a Max. dU =-0.007 for C41_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 3 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.1363 0.0400 SIMU U33 C41_b Cl51_a -0.1201 0.0400 SIMU U33 Cl41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.031 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39912 0.00059 0.022 OSF 2 0.56810 0.01561 -0.144 FVAR 2 Mean shift/esd = 0.034 Maximum = 0.824 for U22 C51_a Max. shift = 0.064 A for C51_a Max. dU = 0.003 for C51_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 4 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.1376 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.023 OSF 2 0.56627 0.01561 -0.117 FVAR 2 Mean shift/esd = 0.026 Maximum = 0.625 for U13 C51_a Max. shift = 0.036 A for C51_a Max. dU = 0.002 for C51_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 5 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.1340 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.029 0.054 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.007 OSF 2 0.56663 0.01572 0.023 FVAR 2 Mean shift/esd = 0.008 Maximum = -0.251 for U33 C51_a Max. shift = 0.008 A for H51A_a Max. dU =-0.001 for C41_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 6 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint -0.1353 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 -0.008 OSF 2 0.56674 0.01569 0.007 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.140 for U33 C51_a Max. shift = 0.003 A for C51_a Max. dU = 0.000 for C51_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 7 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint -0.1361 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 -0.003 OSF 2 0.56679 0.01569 0.003 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.051 for U33 C41_b Max. shift = 0.002 A for C51_a Max. dU = 0.000 for C51_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 8 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint -0.1364 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56679 0.01569 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.025 for z C41_b Max. shift = 0.002 A for C51_a Max. dU = 0.000 for C51_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 9 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint -0.1366 0.0400 SIMU U33 C41_b Cl51_a 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. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 -0.001 OSF 2 0.56677 0.01569 -0.002 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.016 for x C41_b Max. shift = 0.001 A for C51_a Max. dU = 0.000 for C41_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 10 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.001 OSF 2 0.56676 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.005 for z C51_a Max. shift = 0.000 A for C51_a Max. dU = 0.000 for C51_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 11 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for U11 C41_b Max. shift = 0.000 A for C51_a Max. dU = 0.000 for C41_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 12 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.001 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.002 for x C41_b Max. shift = 0.000 A for H51A_a Max. dU = 0.000 for C41_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 13 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for U11 C41_b Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 14 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56673 0.01569 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for x C51_a Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 15 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl52_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 16 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl52_a Least-squares cycle 17 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 17 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl52_a Least-squares cycle 18 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 18 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 19 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 19 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U11 Cl41_b Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl52_a Least-squares cycle 20 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 20 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U11 Cl52_a Max. shift = 0.000 A for H51A_a Max. dU = 0.000 for Cl52_a Least-squares cycle 21 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 21 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 22 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 22 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 22 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 23 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 23 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 23 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 24 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 24 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 24 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 25 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 25 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 25 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 26 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 26 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 26 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 27 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 27 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 27 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 27 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 28 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 28 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 28 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 28 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 29 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 29 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 29 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 29 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 30 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 30 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 30 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 30 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 31 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 31 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 31 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 31 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56673 0.01569 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 32 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 32 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 32 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 32 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56673 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl41_b Least-squares cycle 33 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 33 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 33 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 33 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U22 Cl51_a Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl51_a Least-squares cycle 34 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 34 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 34 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 34 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 35 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 35 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 35 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 35 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56675 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 36 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 36 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 36 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 36 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl51_a Least-squares cycle 37 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 37 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 37 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 37 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Fe1 Max. shift = 0.000 A for C51_a Max. dU = 0.000 for Cl51_a Least-squares cycle 38 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 38 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 38 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 38 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl51_a Least-squares cycle 39 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 39 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 39 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 39 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for Cl52_a Max. dU = 0.000 for Cl52_a Least-squares cycle 40 Maximum vector length = 511 Memory required = 5702 / 529134 wR2 = 0.1325 before cycle 40 for 7994 data and 410 / 410 parameters Disagreeable restraints before cycle 40 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 40 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39913 0.00059 0.000 OSF 2 0.56674 0.01569 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H51A_a Max. dU = 0.000 for Cl52_a Largest correlation matrix elements -0.988 y C51_a / y C41_b 0.877 x Cl52_a / y Cl42_b -0.849 U33 C41_b / z C41_b -0.985 z C51_a / z C41_b 0.875 x Cl52_a / z Cl42_b -0.838 U13 Cl52_a / FVAR 2 -0.983 x C51_a / x C41_b -0.868 y Cl51_a / y Cl41_b -0.834 U33 C51_a / z C41_b 0.936 x Cl52_a / FVAR 2 0.867 y Cl42_b / FVAR 2 0.828 U33 C51_a / z C51_a 0.901 z Cl52_a / FVAR 2 0.860 z Cl42_b / FVAR 2 -0.825 U13 Cl52_a / y Cl42_b 0.892 z Cl52_a / x Cl52_a 0.859 z C51_a / U33 C41_b -0.824 U13 Cl52_a / z Cl52_a 0.889 x Cl42_b / FVAR 2 0.859 z Cl52_a / y Cl42_b -0.822 U11 Cl52_a / FVAR 2 0.883 z Cl52_a / x Cl42_b 0.852 x Cl52_a / x Cl42_b 0.820 y Cl52_a / FVAR 2 Idealized hydrogen atom generation before cycle 41 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0652 0.6405 0.2535 23 0.990 0.000 C1 N1 C2 H1B -0.0810 0.5381 0.2904 23 0.990 0.000 C1 N1 C2 H2A -0.1777 0.3555 0.2519 23 0.990 0.000 C2 N2 C1 H2B -0.2347 0.5045 0.2322 23 0.990 0.000 C2 N2 C1 H3 0.0946 0.4512 0.3153 43 0.950 0.000 C3 N1 C4 H7 0.5460 0.2143 0.2975 43 0.950 0.000 C7 C6 C8 H9 0.2734 0.3660 0.3505 43 0.950 0.000 C9 C8 C4 H11A 0.2965 0.1277 0.1947 137 0.980 0.000 C11 C10 H11A H11B 0.3821 0.0096 0.2190 137 0.980 0.000 C11 C10 H11A H11C 0.4129 0.0671 0.1778 137 0.980 0.000 C11 C10 H11A H12A 0.5094 0.4306 0.2063 137 0.980 0.000 C12 C10 H12A H12B 0.3746 0.3932 0.1879 137 0.980 0.000 C12 C10 H12A H12C 0.4850 0.3207 0.1700 137 0.980 0.000 C12 C10 H12A H13A 0.6152 0.1440 0.2069 137 0.980 0.000 C13 C10 H13A H13B 0.5865 0.0803 0.2477 137 0.980 0.000 C13 C10 H13A H13C 0.6331 0.2465 0.2448 137 0.980 0.000 C13 C10 H13A H15A 0.3616 0.1566 0.3945 137 0.980 0.000 C15 C14 H15A H15B 0.4923 0.1217 0.4170 137 0.980 0.000 C15 C14 H15A H15C 0.4493 0.0464 0.3757 137 0.980 0.000 C15 C14 H15A H16A 0.5220 0.4922 0.3815 137 0.980 0.000 C16 C14 H16A H16B 0.5405 0.3951 0.4205 137 0.980 0.000 C16 C14 H16A H16C 0.4081 0.4275 0.3991 137 0.980 0.000 C16 C14 H16A H17A 0.6351 0.1379 0.3546 137 0.980 0.000 C17 C14 H17A H17B 0.6745 0.2287 0.3938 137 0.980 0.000 C17 C14 H17A H17C 0.6626 0.3110 0.3526 137 0.980 0.000 C17 C14 H17A H18 -0.2704 0.3848 0.1735 43 0.950 0.000 C18 N2 C19 H22 -0.0968 0.2045 0.0373 43 0.950 0.000 C22 C21 C23 H24 -0.3315 0.3317 0.1082 43 0.950 0.000 C24 C23 C19 H26A 0.2293 0.0274 0.1077 137 0.980 0.000 C26 C25 H26A H26B 0.0918 -0.0220 0.1050 137 0.980 0.000 C26 C25 H26A H26C 0.1480 0.0878 0.1388 137 0.980 0.000 C26 C25 H26A H27A 0.0981 0.2250 0.0252 137 0.980 0.000 C27 C25 H27A H27B 0.0537 0.0642 0.0362 137 0.980 0.000 C27 C25 H27A H27C 0.1941 0.1004 0.0404 137 0.980 0.000 C27 C25 H27A H28A 0.1773 0.4021 0.0770 137 0.980 0.000 C28 C25 H28A H28B 0.2814 0.2832 0.0883 137 0.980 0.000 C28 C25 H28A H28C 0.2073 0.3461 0.1211 137 0.980 0.000 C28 C25 H28A H30A -0.3951 0.0975 -0.0078 137 0.980 0.000 C30 C29 H30A H30B -0.3278 0.0289 0.0317 137 0.980 0.000 C30 C29 H30A H30C -0.2517 0.1007 0.0006 137 0.980 0.000 C30 C29 H30A H31A -0.4656 0.3725 0.0549 137 0.980 0.000 C31 C29 H31A H31B -0.4665 0.1995 0.0644 137 0.980 0.000 C31 C29 H31A H31C -0.5166 0.2574 0.0217 137 0.980 0.000 C31 C29 H31A H32A -0.3739 0.3811 -0.0183 137 0.980 0.000 C32 C29 H32A H32B -0.2327 0.3768 -0.0038 137 0.980 0.000 C32 C29 H32A H32C -0.3183 0.4801 0.0179 137 0.980 0.000 C32 C29 H32A H41A 0.0344 0.3547 -0.1078 23 0.990 0.000 C41_b Cl41_b Cl42_b H41B 0.1166 0.4276 -0.0716 23 0.990 0.000 C41_b Cl41_b Cl42_b H51A 0.1102 0.4282 -0.0900 23 0.990 0.000 C51_a Cl52_a Cl51_a H51B -0.0109 0.3367 -0.1031 23 0.990 0.000 C51_a Cl52_a Cl51_a 05src0140 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.06503 0.53729 0.26300 1.00000 0.02157 0.02883 0.02603 -0.00303 0.00476 0.00515 0.02533 0.00522 0.00025 0.00034 0.00008 0.00000 0.00150 0.00176 0.00158 0.00131 0.00125 0.00129 0.00069 H1A -0.06524 0.64050 0.25352 1.00000 0.03040 0.00000 0.00000 H1B -0.08103 0.53807 0.29042 1.00000 0.03040 0.00000 0.00000 C2 -0.15971 0.44671 0.23797 1.00000 0.01807 0.03393 0.02868 -0.00144 0.00539 0.00321 0.02669 0.00530 0.00025 0.00035 0.00008 0.00000 0.00145 0.00184 0.00160 0.00142 0.00124 0.00136 0.00070 H2A -0.17767 0.35552 0.25189 1.00000 0.03203 0.00000 0.00000 H2B -0.23469 0.50453 0.23215 1.00000 0.03203 0.00000 0.00000 C3 0.12105 0.43112 0.29090 1.00000 0.01948 0.02114 0.02331 -0.00407 0.00421 -0.00555 0.02119 0.00489 0.00024 0.00032 0.00008 0.00000 0.00139 0.00152 0.00147 0.00132 0.00120 0.00129 0.00061 H3 0.09464 0.45118 0.31530 1.00000 0.02542 0.00000 0.00000 C4 0.23710 0.36257 0.29124 1.00000 0.01970 0.02135 0.02288 -0.00062 0.00083 -0.00294 0.02149 0.00500 0.00025 0.00032 0.00008 0.00000 0.00144 0.00156 0.00150 0.00126 0.00121 0.00126 0.00064 C5 0.28392 0.32334 0.25652 1.00000 0.01989 0.01457 0.02314 0.00236 -0.00012 -0.00339 0.01947 0.00493 0.00025 0.00030 0.00008 0.00000 0.00142 0.00146 0.00148 0.00121 0.00120 0.00119 0.00061 C6 0.40150 0.26546 0.25898 1.00000 0.01820 0.01365 0.02620 -0.00054 0.00144 -0.00508 0.01949 0.00490 0.00024 0.00030 0.00008 0.00000 0.00139 0.00143 0.00154 0.00122 0.00120 0.00118 0.00061 C7 0.46637 0.25122 0.29584 1.00000 0.01833 0.01607 0.03164 0.00225 -0.00012 -0.00107 0.02232 0.00507 0.00026 0.00031 0.00008 0.00000 0.00141 0.00149 0.00166 0.00130 0.00127 0.00121 0.00064 H7 0.54598 0.21430 0.29755 1.00000 0.02679 0.00000 0.00000 C8 0.42252 0.28752 0.33066 1.00000 0.02477 0.01700 0.02502 0.00054 -0.00240 -0.00451 0.02278 0.00504 0.00026 0.00031 0.00008 0.00000 0.00156 0.00151 0.00156 0.00126 0.00127 0.00127 0.00065 C9 0.30667 0.34195 0.32749 1.00000 0.02676 0.02470 0.02196 0.00022 0.00362 -0.00489 0.02444 0.00518 0.00026 0.00033 0.00008 0.00000 0.00159 0.00166 0.00149 0.00131 0.00127 0.00136 0.00066 H9 0.27338 0.36599 0.35050 1.00000 0.02932 0.00000 0.00000 C10 0.45473 0.22179 0.22203 1.00000 0.01737 0.01969 0.02734 0.00119 0.00379 0.00110 0.02139 0.00515 0.00024 0.00031 0.00008 0.00000 0.00142 0.00153 0.00156 0.00128 0.00121 0.00123 0.00063 C11 0.37976 0.09504 0.20150 1.00000 0.02078 0.02479 0.03066 -0.00521 0.00496 -0.00031 0.02527 0.00509 0.00025 0.00033 0.00009 0.00000 0.00147 0.00168 0.00163 0.00136 0.00127 0.00130 0.00068 H11A 0.29653 0.12769 0.19469 1.00000 0.03791 0.00000 0.00000 H11B 0.38214 0.00964 0.21898 1.00000 0.03791 0.00000 0.00000 H11C 0.41293 0.06714 0.17777 1.00000 0.03791 0.00000 0.00000 C12 0.45606 0.35353 0.19401 1.00000 0.02228 0.02667 0.03356 0.00465 0.00871 0.00369 0.02705 0.00575 0.00026 0.00034 0.00009 0.00000 0.00155 0.00170 0.00172 0.00142 0.00134 0.00134 0.00070 H12A 0.50935 0.43064 0.20634 1.00000 0.04058 0.00000 0.00000 H12B 0.37465 0.39319 0.18788 1.00000 0.04058 0.00000 0.00000 H12C 0.48504 0.32068 0.16997 1.00000 0.04058 0.00000 0.00000 C13 0.58393 0.16839 0.23119 1.00000 0.02151 0.02528 0.03570 -0.00144 0.00678 0.00099 0.02723 0.00557 0.00025 0.00034 0.00009 0.00000 0.00153 0.00170 0.00175 0.00143 0.00134 0.00133 0.00070 H13A 0.61520 0.14400 0.20688 1.00000 0.04084 0.00000 0.00000 H13B 0.58653 0.08029 0.24773 1.00000 0.04084 0.00000 0.00000 H13C 0.63314 0.24652 0.24484 1.00000 0.04084 0.00000 0.00000 C14 0.49701 0.26735 0.37069 1.00000 0.02893 0.03014 0.02483 0.00291 -0.00683 -0.00412 0.02890 0.00537 0.00028 0.00035 0.00009 0.00000 0.00168 0.00179 0.00161 0.00139 0.00134 0.00144 0.00072 C15 0.44536 0.13607 0.39138 1.00000 0.04834 0.04782 0.03309 0.01225 -0.00927 -0.01395 0.04440 0.00630 0.00033 0.00042 0.00010 0.00000 0.00222 0.00230 0.00190 0.00174 0.00168 0.00186 0.00095 H15A 0.36162 0.15656 0.39453 1.00000 0.06660 0.00000 0.00000 H15B 0.49227 0.12172 0.41702 1.00000 0.06660 0.00000 0.00000 H15C 0.44933 0.04642 0.37573 1.00000 0.06660 0.00000 0.00000 C16 0.49139 0.40832 0.39518 1.00000 0.03577 0.04518 0.02434 -0.00460 -0.00488 -0.00184 0.03589 0.00570 0.00030 0.00039 0.00009 0.00000 0.00183 0.00214 0.00163 0.00158 0.00141 0.00166 0.00080 H16A 0.52202 0.49216 0.38155 1.00000 0.05384 0.00000 0.00000 H16B 0.54051 0.39513 0.42050 1.00000 0.05384 0.00000 0.00000 H16C 0.40805 0.42750 0.39909 1.00000 0.05384 0.00000 0.00000 C17 0.62926 0.23315 0.36767 1.00000 0.02946 0.04713 0.03515 -0.00153 -0.00876 0.00276 0.03843 0.00600 0.00028 0.00041 0.00010 0.00000 0.00180 0.00220 0.00190 0.00170 0.00150 0.00165 0.00085 H17A 0.63507 0.13789 0.35459 1.00000 0.05764 0.00000 0.00000 H17B 0.67448 0.22868 0.39385 1.00000 0.05764 0.00000 0.00000 H17C 0.66259 0.31105 0.35264 1.00000 0.05764 0.00000 0.00000 C18 -0.18743 0.37608 0.17126 1.00000 0.01687 0.02816 0.03124 -0.00029 0.00184 0.00257 0.02555 0.00537 0.00026 0.00033 0.00009 0.00000 0.00144 0.00170 0.00169 0.00139 0.00130 0.00129 0.00068 H18 -0.27041 0.38478 0.17354 1.00000 0.03066 0.00000 0.00000 C19 -0.15642 0.32744 0.13430 1.00000 0.02596 0.02525 0.02616 -0.00004 -0.00014 0.00082 0.02611 0.00537 0.00027 0.00033 0.00008 0.00000 0.00158 0.00168 0.00159 0.00136 0.00131 0.00138 0.00068 C20 -0.03774 0.29378 0.12869 1.00000 0.02243 0.02411 0.02793 -0.00177 -0.00341 0.00621 0.02543 0.00535 0.00026 0.00033 0.00009 0.00000 0.00154 0.00166 0.00163 0.00135 0.00131 0.00131 0.00068 C21 -0.01536 0.24126 0.09162 1.00000 0.03187 0.04507 0.02966 -0.00678 -0.00146 0.01733 0.03603 0.00617 0.00029 0.00040 0.00009 0.00000 0.00181 0.00214 0.00176 0.00159 0.00146 0.00163 0.00083 C22 -0.11215 0.23423 0.06246 1.00000 0.04006 0.04731 0.02564 -0.00763 -0.00355 0.01729 0.03838 0.00620 0.00031 0.00040 0.00009 0.00000 0.00197 0.00222 0.00172 0.00161 0.00151 0.00175 0.00086 H22 -0.09678 0.20451 0.03730 1.00000 0.04606 0.00000 0.00000 C23 -0.23192 0.26782 0.06726 1.00000 0.03333 0.03604 0.02921 -0.00366 -0.00661 0.01216 0.03383 0.00591 0.00029 0.00038 0.00009 0.00000 0.00182 0.00196 0.00175 0.00152 0.00144 0.00157 0.00079 C24 -0.25177 0.31149 0.10347 1.00000 0.02523 0.03056 0.03397 -0.00113 -0.00420 0.00650 0.03065 0.00560 0.00028 0.00035 0.00009 0.00000 0.00164 0.00182 0.00177 0.00150 0.00139 0.00143 0.00074 H24 -0.33149 0.33174 0.10818 1.00000 0.03678 0.00000 0.00000 C25 0.11126 0.19210 0.08515 1.00000 0.03584 0.09821 0.03189 -0.02443 -0.00348 0.02855 0.05604 0.00737 0.00033 0.00054 0.00010 0.00000 0.00209 0.00351 0.00200 0.00218 0.00164 0.00229 0.00123 C26 0.14843 0.05936 0.11157 1.00000 0.05450 0.07984 0.06276 -0.02761 -0.02198 0.04041 0.06838 0.00773 0.00038 0.00051 0.00012 0.00000 0.00258 0.00332 0.00274 0.00252 0.00218 0.00248 0.00143 H26A 0.22928 0.02744 0.10770 1.00000 0.10258 0.00000 0.00000 H26B 0.09179 -0.02200 0.10505 1.00000 0.10258 0.00000 0.00000 H26C 0.14796 0.08785 0.13883 1.00000 0.10258 0.00000 0.00000 C27 0.11462 0.14076 0.04293 1.00000 0.05731 0.19701 0.04124 -0.04696 -0.00588 0.06625 0.09964 0.00976 0.00041 0.00077 0.00012 0.00000 0.00285 0.00638 0.00246 0.00328 0.00213 0.00358 0.00225 H27A 0.09815 0.22495 0.02523 1.00000 0.14946 0.00000 0.00000 H27B 0.05371 0.06422 0.03624 1.00000 0.14946 0.00000 0.00000 H27C 0.19413 0.10044 0.04045 1.00000 0.14946 0.00000 0.00000 C28 0.20252 0.31710 0.09364 1.00000 0.03851 0.13561 0.05349 -0.00644 0.01858 0.01016 0.07474 0.00856 0.00035 0.00063 0.00012 0.00000 0.00239 0.00481 0.00263 0.00293 0.00206 0.00281 0.00154 H28A 0.17729 0.40215 0.07703 1.00000 0.11212 0.00000 0.00000 H28B 0.28144 0.28317 0.08827 1.00000 0.11212 0.00000 0.00000 H28C 0.20731 0.34607 0.12105 1.00000 0.11212 0.00000 0.00000 C29 -0.33137 0.25800 0.03239 1.00000 0.03935 0.05827 0.03037 -0.00793 -0.01374 0.01739 0.04432 0.00643 0.00032 0.00044 0.00010 0.00000 0.00204 0.00249 0.00186 0.00179 0.00158 0.00188 0.00095 C30 -0.32603 0.10777 0.01244 1.00000 0.06551 0.10220 0.05819 -0.05116 -0.03152 0.03619 0.07888 0.00735 0.00041 0.00057 0.00013 0.00000 0.00293 0.00392 0.00273 0.00276 0.00232 0.00280 0.00167 H30A -0.39513 0.09746 -0.00782 1.00000 0.11833 0.00000 0.00000 H30B -0.32782 0.02890 0.03174 1.00000 0.11833 0.00000 0.00000 H30C -0.25174 0.10071 0.00063 1.00000 0.11833 0.00000 0.00000 C31 -0.45611 0.27319 0.04441 1.00000 0.03678 0.05362 0.04509 -0.00979 -0.01623 0.00861 0.04712 0.00640 0.00031 0.00045 0.00011 0.00000 0.00205 0.00244 0.00216 0.00191 0.00169 0.00184 0.00098 H31A -0.46556 0.37248 0.05488 1.00000 0.07067 0.00000 0.00000 H31B -0.46653 0.19947 0.06441 1.00000 0.07067 0.00000 0.00000 H31C -0.51657 0.25738 0.02169 1.00000 0.07067 0.00000 0.00000 C32 -0.31234 0.38557 0.00451 1.00000 0.05805 0.12991 0.05119 0.03986 -0.01523 0.00302 0.08174 0.00935 0.00041 0.00065 0.00013 0.00000 0.00287 0.00473 0.00268 0.00297 0.00225 0.00300 0.00166 H32A -0.37386 0.38106 -0.01831 1.00000 0.12262 0.00000 0.00000 H32B -0.23271 0.37682 -0.00383 1.00000 0.12262 0.00000 0.00000 H32C -0.31833 0.48010 0.01792 1.00000 0.12262 0.00000 0.00000 N1 0.05086 0.46698 0.25997 1.00000 0.01992 0.02148 0.02509 -0.00188 0.00335 -0.00034 0.02213 0.00417 0.00020 0.00026 0.00007 0.00000 0.00123 0.00134 0.00130 0.00106 0.00105 0.00103 0.00055 N2 -0.11232 0.40899 0.20165 1.00000 0.01928 0.02622 0.02444 -0.00069 0.00253 0.00269 0.02335 0.00431 0.00020 0.00027 0.00007 0.00000 0.00122 0.00140 0.00128 0.00112 0.00103 0.00109 0.00055 O1 0.21845 0.33989 0.22213 1.00000 0.01741 0.02578 0.02154 -0.00071 0.00160 0.00276 0.02166 0.00339 0.00016 0.00021 0.00005 0.00000 0.00098 0.00113 0.00102 0.00089 0.00083 0.00087 0.00044 O2 0.05143 0.30588 0.15753 1.00000 0.02287 0.03432 0.02584 -0.00756 -0.00156 0.00899 0.02811 0.00360 0.00017 0.00023 0.00006 0.00000 0.00109 0.00126 0.00110 0.00097 0.00090 0.00095 0.00050 Cl1 0.09754 0.66048 0.18192 1.00000 0.04033 0.02731 0.03801 0.00621 0.00977 0.00242 0.03480 0.00154 0.00007 0.00009 0.00002 0.00000 0.00047 0.00043 0.00045 0.00036 0.00037 0.00037 0.00021 Fe1 0.07280 0.42886 0.20201 1.00000 0.01719 0.02214 0.02233 -0.00071 0.00209 0.00245 0.02060 0.00073 0.00004 0.00005 0.00001 0.00000 0.00021 0.00023 0.00022 0.00019 0.00016 0.00019 0.00012 C41_b 0.06575 0.34114 -0.08000 0.56674 0.07512 0.07711 0.05925 0.02803 0.01392 0.01434 0.07004 0.09396 0.00445 0.00652 0.00147 0.01569 0.00589 0.00514 0.00702 0.00456 0.00473 0.00483 0.00305 H41A_b 0.03438 0.35474 -0.10785 0.56674 0.08405 0.01569 0.00000 H41B_b 0.11656 0.42763 -0.07156 0.56674 0.08405 0.01569 0.00000 Cl41_b 0.15124 0.18571 -0.07492 0.56674 0.05570 0.07748 0.07698 0.03094 0.03852 0.02500 0.06737 0.00994 0.00040 0.00056 0.00013 0.01569 0.00208 0.00270 0.00246 0.00194 0.00168 0.00180 0.00147 Cl42_b -0.05536 0.33414 -0.05270 0.56674 0.07659 0.10309 0.08047 0.01081 0.02394 0.03084 0.08550 0.01860 0.00058 0.00080 0.00018 0.01569 0.00281 0.00298 0.00247 0.00232 0.00209 0.00224 0.00182 C51_a 0.05859 0.34727 -0.08250 0.43326 0.07559 0.07664 0.05791 0.02947 0.01226 0.01250 0.06974 0.12006 0.00605 0.00855 0.00188 0.01569 0.00629 0.00546 0.00729 0.00493 0.00504 0.00528 0.00325 H51A_a 0.11016 0.42820 -0.09000 0.43326 0.08369 0.01569 0.00000 H51B_a -0.01092 0.33672 -0.10307 0.43326 0.08369 0.01569 0.00000 Cl51_a 0.14069 0.18013 -0.07715 0.43326 0.15960 0.18247 0.19579 0.04475 0.07105 0.07368 0.17501 0.02874 0.00112 0.00156 0.00037 0.01569 0.00851 0.00959 0.00935 0.00730 0.00682 0.00709 0.00504 Cl52_a 0.00818 0.38822 -0.03681 0.43326 0.13910 0.08955 0.09269 0.02533 0.04997 0.03399 0.10399 0.03243 0.00136 0.00090 0.00031 0.01569 0.00753 0.00360 0.00451 0.00308 0.00523 0.00435 0.00368 Final Structure Factor Calculation for 05src0140 in P2(1)/c Total number of l.s. parameters = 410 Maximum vector length = 511 Memory required = 5292 / 25039 wR2 = 0.1325 before cycle 41 for 7994 data and 0 / 410 parameters Disagreeable restraints before cycle 41 Observed Target Error Sigma Restraint -0.1365 0.0400 SIMU U33 C41_b Cl51_a Summary of restraints applied in cycle 41 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 6. 30. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.036 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.055 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.049 for 36 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0441 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0552 for 5161 Fo > 4sig(Fo) and 0.1069 for all 7994 data wR2 = 0.1325, GooF = S = 1.047, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0325 0.0261 0.0174 C1 0.0348 0.0288 0.0165 C2 0.0284 0.0206 0.0146 C3 0.0246 0.0228 0.0171 C4 0.0268 0.0189 0.0127 C5 0.0268 0.0213 0.0103 C6 0.0334 0.0180 0.0155 C7 0.0324 0.0211 0.0147 C8 0.0308 0.0222 0.0204 C9 0.0275 0.0198 0.0168 C10 0.0337 0.0221 0.0200 C11 0.0376 0.0244 0.0192 C12 0.0361 0.0255 0.0201 C13 0.0416 0.0276 0.0175 C14 0.0742 0.0342 0.0248 C15 0.0462 0.0418 0.0197 C16 0.0506 0.0443 0.0204 C17 0.0318 0.0286 0.0163 C18 0.0303 0.0253 0.0228 C19 0.0361 0.0241 0.0161 C20 0.0609 0.0273 0.0199 C21 0.0661 0.0261 0.0230 C22 0.0533 0.0287 0.0196 C23 0.0422 0.0307 0.0191 C24 0.1195 0.0268 0.0218 C25 0.1385 0.0425 0.0241 C26 0.2402 0.0373 0.0213 C27 may be split into 0.1208 0.1630 0.0411 and 0.1085 0.1185 0.0448 0.1371 0.0591 0.0280 C28 0.0774 0.0379 0.0176 C29 0.1714 0.0440 0.0212 C30 0.0753 0.0446 0.0214 C31 0.1480 0.0727 0.0246 C32 0.0259 0.0207 0.0198 N1 0.0275 0.0242 0.0183 N2 0.0269 0.0215 0.0166 O1 0.0449 0.0215 0.0179 O2 0.0451 0.0349 0.0244 Cl1 0.0239 0.0217 0.0162 Fe1 0.1028 0.0686 0.0387 C41_b 0.1243 0.0477 0.0301 Cl41_b 0.1270 0.0762 0.0533 Cl42_b 0.1017 0.0712 0.0363 C51_a 0.2819 0.1502 0.0930 Cl51_a 0.1725 0.0744 0.0651 Cl52_a Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.023 0.035 0.047 0.061 0.077 0.096 0.126 0.180 1.000 Number in group 854. 770. 828. 749. 795. 804. 803. 797. 794. 800. GooF 1.114 1.079 1.067 1.032 1.075 1.031 1.000 0.963 1.030 1.062 K 4.960 1.454 1.222 0.996 0.968 1.017 0.993 1.002 1.005 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 802. 815. 802. 776. 801. 796. 808. 799. 789. 806. GooF 0.955 0.879 0.956 0.893 0.913 0.966 0.985 0.976 1.052 1.659 K 1.007 1.014 1.003 1.014 1.022 1.025 1.018 1.015 1.010 0.997 R1 0.306 0.251 0.213 0.152 0.120 0.100 0.075 0.052 0.036 0.039 Recommended weighting scheme: WGHT 0.0441 3.8738 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)/esd Fc/Fc(max) Resolution(A) 0 6 11 221.18 3.90 8.10 0.008 1.36 2 4 10 138.90 4.75 7.49 0.009 1.75 -2 2 2 95.18 1.68 7.39 0.005 3.50 -1 3 2 127.53 14.86 6.78 0.015 2.89 0 1 4 509.09 204.71 6.41 0.057 6.23 1 4 4 82.25 0.50 6.34 0.003 2.13 0 5 1 126.42 1.89 6.25 0.006 1.81 1 4 10 251.16 77.34 6.01 0.035 1.84 2 4 0 2168.29 1453.67 5.88 0.153 2.10 -1 5 1 204.92 58.06 5.87 0.030 1.79 -3 5 1 748.13 296.89 5.71 0.069 1.63 9 0 6 1878.43 2916.99 5.50 0.216 1.18 3 5 1 382.85 151.95 5.47 0.049 1.62 1 1 4 1702.16 2466.48 5.45 0.199 5.23 -1 2 10 202.05 72.02 5.38 0.034 2.72 -1 5 3 793.94 474.78 5.36 0.087 1.77 1 1 1 27.76 182.71 5.14 0.054 6.77 2 2 3 231.23 444.18 4.95 0.084 3.28 0 4 12 109.10 28.35 4.86 0.021 1.77 2 2 6 50.36 1.62 4.78 0.005 2.89 1 4 2 594.39 363.45 4.65 0.076 2.19 4 0 10 1970.22 1407.80 4.60 0.150 2.04 2 1 8 2678.89 2018.37 4.56 0.180 3.02 -3 5 3 599.04 348.48 4.50 0.075 1.62 6 3 3 134.28 12.71 4.31 0.014 1.54 0 6 13 100.73 7.82 4.29 0.011 1.31 2 2 0 88.21 24.66 4.28 0.020 3.51 2 1 1 99.21 31.60 4.27 0.022 4.63 -5 6 13 226.66 55.83 4.18 0.030 1.16 2 4 2 1651.96 1225.25 4.15 0.140 2.07 -1 1 4 5317.10 6674.29 4.09 0.327 5.67 -1 3 4 150.36 64.64 4.06 0.032 2.79 -2 0 14 205.70 375.15 4.05 0.077 2.36 -8 3 3 112.32 10.08 3.99 0.013 1.27 4 3 3 445.73 261.92 3.90 0.065 1.98 -10 7 8 263.87 18.24 3.88 0.017 0.84 -5 3 15 148.20 40.32 3.87 0.025 1.49 2 0 14 2530.86 1952.30 3.86 0.177 2.14 -6 4 14 179.35 63.08 3.83 0.032 1.30 4 2 9 83.82 16.80 3.82 0.016 1.92 -1 3 10 51.41 136.02 3.79 0.047 2.26 4 1 12 252.73 129.82 3.73 0.046 1.84 -4 7 10 127.17 0.56 3.68 0.003 1.13 6 4 13 145.04 38.48 3.67 0.025 1.21 -4 2 11 66.62 5.15 3.53 0.009 2.00 -1 0 6 6522.89 7942.19 3.53 0.357 5.39 3 1 12 7553.75 6261.04 3.52 0.317 2.08 -1 7 4 83.45 12.97 3.50 0.014 1.27 -2 2 9 1758.14 2215.53 3.42 0.188 2.70 1 4 20 119.13 6.12 3.28 0.010 1.34 Bond lengths and angles C1 - Distance Angles N1 1.4665 (0.0035) C2 1.5207 (0.0040) 106.67 (0.23) H1A 0.9900 110.39 110.39 H1B 0.9900 110.39 110.39 108.61 C1 - N1 C2 H1A C2 - Distance Angles N2 1.4705 (0.0035) C1 1.5207 (0.0040) 107.90 (0.23) H2A 0.9900 110.12 110.12 H2B 0.9900 110.12 110.12 108.44 C2 - N2 C1 H2A C3 - Distance Angles N1 1.2853 (0.0035) C4 1.4435 (0.0039) 124.73 (0.26) H3 0.9500 117.64 117.64 C3 - N1 C4 C4 - Distance Angles C9 1.4010 (0.0039) C5 1.4210 (0.0039) 120.01 (0.26) C3 1.4435 (0.0039) 117.46 (0.26) 122.45 (0.25) C4 - C9 C5 C5 - Distance Angles O1 1.3234 (0.0032) C6 1.4141 (0.0039) 120.01 (0.25) C4 1.4210 (0.0039) 120.65 (0.25) 119.35 (0.25) C5 - O1 C6 C6 - Distance Angles C7 1.3902 (0.0038) C5 1.4141 (0.0039) 117.52 (0.26) C10 1.5353 (0.0038) 121.82 (0.25) 120.66 (0.24) C6 - C7 C5 C7 - Distance Angles C6 1.3902 (0.0038) C8 1.4018 (0.0039) 124.58 (0.27) H7 0.9500 117.71 117.71 C7 - C6 C8 C8 - Distance Angles C9 1.3834 (0.0040) C7 1.4018 (0.0039) 116.75 (0.26) C14 1.5329 (0.0040) 120.67 (0.27) 122.58 (0.26) C8 - C9 C7 C9 - Distance Angles C8 1.3834 (0.0040) C4 1.4010 (0.0039) 121.78 (0.27) H9 0.9500 119.11 119.11 C9 - C8 C4 C10 - Distance Angles C13 1.5240 (0.0039) C6 1.5353 (0.0038) 111.98 (0.24) C12 1.5386 (0.0040) 106.75 (0.23) 111.36 (0.23) C11 1.5404 (0.0039) 107.95 (0.23) 109.07 (0.22) 109.64 (0.24) C10 - C13 C6 C12 C11 - Distance Angles C10 1.5404 (0.0040) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5386 (0.0040) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C13 - Distance Angles C10 1.5240 (0.0039) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C10 H13A H13B C14 - Distance Angles C8 1.5329 (0.0040) C17 1.5361 (0.0044) 112.33 (0.26) C16 1.5380 (0.0045) 110.05 (0.25) 108.41 (0.26) C15 1.5404 (0.0045) 108.56 (0.25) 107.73 (0.28) 109.71 (0.27) C14 - C8 C17 C16 C15 - Distance Angles C14 1.5404 (0.0045) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C16 - Distance Angles C14 1.5380 (0.0045) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C14 H16A H16B C17 - Distance Angles C14 1.5361 (0.0044) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C14 H17A H17B C18 - Distance Angles N2 1.2940 (0.0036) C19 1.4403 (0.0041) 125.80 (0.27) H18 0.9500 117.10 117.10 C18 - N2 C19 C19 - Distance Angles C20 1.4073 (0.0041) C24 1.4166 (0.0041) 120.70 (0.28) C18 1.4403 (0.0041) 122.34 (0.27) 116.95 (0.27) C19 - C20 C24 C20 - Distance Angles O2 1.3228 (0.0033) C19 1.4073 (0.0041) 121.03 (0.26) C21 1.4228 (0.0042) 120.15 (0.26) 118.79 (0.27) C20 - O2 C19 C21 - Distance Angles C22 1.3846 (0.0044) C20 1.4228 (0.0042) 117.24 (0.29) C25 1.5363 (0.0046) 122.28 (0.29) 120.46 (0.27) C21 - C22 C20 C22 - Distance Angles C21 1.3846 (0.0044) C23 1.4119 (0.0045) 125.02 (0.30) H22 0.9500 117.49 117.49 C22 - C21 C23 C23 - Distance Angles C24 1.3618 (0.0043) C22 1.4119 (0.0045) 116.53 (0.28) C29 1.5361 (0.0044) 123.38 (0.30) 120.07 (0.29) C23 - C24 C22 C24 - Distance Angles C23 1.3618 (0.0043) C19 1.4166 (0.0041) 121.59 (0.30) H24 0.9500 119.20 119.20 C24 - C23 C19 C25 - Distance Angles C28 1.5293 (0.0063) C26 1.5342 (0.0060) 109.97 (0.33) C21 1.5363 (0.0046) 111.66 (0.34) 108.90 (0.35) C27 1.5401 (0.0050) 107.78 (0.40) 106.95 (0.38) 111.48 (0.29) C25 - C28 C26 C21 C26 - Distance Angles C25 1.5342 (0.0060) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5401 (0.0050) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C25 H27A H27B C28 - Distance Angles C25 1.5293 (0.0063) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C25 H28A H28B C29 - Distance Angles C31 1.5216 (0.0050) C30 1.5298 (0.0055) 107.27 (0.34) C23 1.5361 (0.0044) 112.37 (0.28) 109.79 (0.29) C32 1.5381 (0.0059) 108.32 (0.32) 111.48 (0.36) 107.65 (0.33) C29 - C31 C30 C23 C30 - Distance Angles C29 1.5298 (0.0055) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C29 H30A H30B C31 - Distance Angles C29 1.5216 (0.0050) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C29 H31A H31B C32 - Distance Angles C29 1.5381 (0.0059) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C29 H32A H32B N1 - Distance Angles C3 1.2853 (0.0035) C1 1.4665 (0.0035) 120.19 (0.24) Fe1 2.0844 (0.0024) 128.57 (0.20) 111.16 (0.17) N1 - C3 C1 N2 - Distance Angles C18 1.2940 (0.0036) C2 1.4705 (0.0035) 118.57 (0.24) Fe1 2.0879 (0.0023) 124.56 (0.20) 116.70 (0.17) N2 - C18 C2 O1 - Distance Angles C5 1.3234 (0.0032) Fe1 1.8744 (0.0019) 137.53 (0.18) O1 - C5 O2 - Distance Angles C20 1.3228 (0.0033) Fe1 1.8903 (0.0020) 131.77 (0.18) O2 - C20 Cl1 - Distance Angles Fe1 2.2373 (0.0009) Cl1 - Fe1 - Distance Angles O1 1.8744 (0.0019) O2 1.8903 (0.0020) 93.47 (0.08) N1 2.0844 (0.0024) 85.53 (0.09) 149.83 (0.09) N2 2.0879 (0.0023) 141.86 (0.09) 85.74 (0.09) 76.97 (0.09) Cl1 2.2373 (0.0009) 112.30 (0.07) 107.79 (0.07) 100.38 (0.07) 104.12 (0.07) Fe1 - O1 O2 N1 N2 C41_b - Distance Angles Cl41_b 1.6994 (0.0576) Cl42_b 1.7594 (0.0502) 112.47 (3.09) H41A_b 0.9900 109.11 109.11 H41B_b 0.9900 109.11 109.11 107.85 C41_b - Cl41_b Cl42_b H41A_b Cl41_b - Distance Angles C41_b 1.6994 (0.0576) Cl41_b - Cl42_b - Distance Angles C41_b 1.7594 (0.0502) Cl42_b - C51_a - Distance Angles Cl52_a 1.7901 (0.0661) Cl51_a 1.7687 (0.0777) 107.85 (3.73) H51A_a 0.9900 110.14 110.14 H51B_a 0.9900 110.14 110.14 108.45 C51_a - Cl52_a Cl51_a H51A_a Cl51_a - Distance Angles C51_a 1.7687 (0.0777) Cl51_a - Cl52_a - Distance Angles C51_a 1.7901 (0.0662) Cl52_a - FMAP and GRID set by program FMAP 2 3 40 GRID -0.676 -2 -2 0.676 2 2 R1 = 0.1046 for 7994 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.7771 0.4367 0.0019 [ 0.58 A from H32B ] Deepest hole -0.40 at 0.0204 0.4340 0.1843 [ 0.79 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4832 / 30309 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2229 0.4367 0.0019 1.00000 0.05 0.35 0.58 H32B 1.12 C32 1.33 H32C 1.82 H32A Q2 1 0.0558 0.6570 0.2220 1.00000 0.05 0.33 1.52 CL1 1.86 H1A 2.17 N1 2.19 FE1 Q3 1 0.0848 0.1881 0.0229 1.00000 0.05 0.33 0.37 H27A 0.85 C27 1.28 H27B 1.52 H27C Q4 1 0.4585 0.2772 0.2102 1.00000 0.05 0.31 0.65 C10 0.89 C12 1.51 H12A 1.52 H12C Q5 1 -0.3567 0.0883 0.0101 1.00000 0.05 0.30 0.39 C30 0.71 H30A 0.95 H30B 1.27 H30C Q6 1 -0.2619 0.0440 0.0101 1.00000 0.05 0.30 0.63 H30C 0.94 C30 1.13 H30B 1.62 H30A Q7 1 0.1316 0.6647 0.2119 1.00000 0.05 0.29 1.06 CL1 2.16 H2A 2.25 FE1 2.68 N1 Q8 1 0.1964 0.4332 0.0830 1.00000 0.05 0.28 0.39 H28A 1.11 C28 1.53 H28C 1.66 H28B Q9 1 -0.3839 0.2835 0.0369 1.00000 0.05 0.28 0.67 C29 0.89 C31 1.43 H31A 1.53 H31C Q10 1 0.4637 0.3314 0.3777 1.00000 0.05 0.28 0.75 C14 0.95 C16 1.35 H16C 1.59 H16A Shortest distances between peaks (including symmetry equivalents) 2 7 0.96 5 6 1.14 5 9 2.04 1 9 2.69 6 9 2.79 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.01: 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. 1.08: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.01: Generate idealized H-atoms 31.24: Structure factors and derivatives 79.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 5.35: Solve l.s. equations 0.00: Generate HTAB table 0.20: Other dependent quantities, CIF, tables 0.15: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 05src0140 finished at 09:44:35 Total CPU time: 119.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++