+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:05:05 on 30-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SRC072 in C2/c CELL 0.71073 11.8621 17.9099 24.1232 90.000 90.952 90.000 ZERR 8.00 0.0024 0.0036 0.0048 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O FE UNIT 224 176 32 24 8 V = 5124.24 F(000) = 2144.0 Mu = 0.62 mm-1 Cell Wt = 4146.77 Rho = 1.344 L.S. 4 BOND FMAP 2 PLAN 10 OMIT -3 1 3 OMIT -3 1 2 OMIT -6 4 1 OMIT 0 2 3 OMIT -1 5 9 OMIT 0 2 8 OMIT 3 3 1 OMIT 1 5 5 OMIT -1 1 5 OMIT -3 55 ISOR C03 C03' C04 C01 C01' WGHT 0.100000 FVAR 0.10743 FE1 5 0.286264 0.588802 0.805009 11.00000 0.02290 0.02881 = 0.06895 0.00874 -0.00238 -0.00042 O1 4 0.339759 0.729798 0.698693 11.00000 0.02789 0.04277 = 0.03396 -0.00185 0.00553 0.00183 O2 4 0.426619 0.582331 0.945410 11.00000 0.02567 0.09042 = 0.05416 0.04238 0.00855 0.00676 N1 3 0.159050 0.759757 0.723307 11.00000 0.02596 0.03468 = 0.03376 0.00206 -0.00158 0.00051 AFIX 43 H1 2 0.114058 0.758893 0.750890 11.00000 -1.20000 AFIX 0 N2 3 0.007422 0.811439 0.677666 11.00000 0.02856 0.03118 = 0.03767 -0.00082 -0.00556 -0.00326 N3 3 0.569247 0.616809 0.888681 11.00000 0.02346 0.04896 = 0.04098 0.01874 0.00302 0.00139 AFIX 43 H3 2 0.583709 0.640665 0.858688 11.00000 -1.20000 AFIX 0 N4 3 0.760244 0.607686 0.896999 11.00000 0.02477 0.07753 = 0.08709 0.04926 0.00672 0.00627 C1 1 0.235102 0.535960 0.734136 11.00000 0.06580 0.03961 = 0.10574 -0.02336 -0.02566 -0.00168 AFIX 43 H1A 2 0.208964 0.558922 0.701822 11.00000 -1.20000 AFIX 0 C2 1 0.348493 0.517848 0.746589 11.00000 0.05118 0.04417 = 0.13193 -0.03079 -0.00247 0.01144 AFIX 43 H2 2 0.409906 0.526833 0.724068 11.00000 -1.20000 AFIX 0 C3 1 0.352080 0.484007 0.798788 11.00000 0.05510 0.02856 = 0.15514 0.00891 -0.01846 0.00753 AFIX 43 H3A 2 0.416443 0.466184 0.816914 11.00000 -1.20000 AFIX 0 C4 1 0.239037 0.481418 0.819767 11.00000 0.05762 0.03729 = 0.14659 0.02689 -0.01237 -0.01413 AFIX 43 H4 2 0.217255 0.462271 0.853787 11.00000 -1.20000 AFIX 0 C5 1 0.167914 0.513394 0.778944 11.00000 0.04046 0.04448 = 0.14241 0.00385 -0.01110 -0.01312 AFIX 43 H5 2 0.090126 0.518739 0.781102 11.00000 -1.20000 AFIX 0 C6 1 0.391204 0.677967 0.810309 11.00000 0.02146 0.03117 = 0.03563 0.00302 0.00341 -0.00076 AFIX 43 H6 2 0.459449 0.683099 0.792268 11.00000 -1.20000 AFIX 0 C7 1 0.375809 0.646648 0.863907 11.00000 0.02491 0.04158 = 0.04242 0.01365 0.00218 0.00418 C8 1 0.258111 0.648690 0.875126 11.00000 0.02700 0.05680 = 0.04695 0.02128 0.01037 0.00637 AFIX 43 H8 2 0.224657 0.631503 0.907301 11.00000 -1.20000 AFIX 0 C9 1 0.201220 0.680854 0.829687 11.00000 0.02220 0.03764 = 0.04906 0.01102 0.00788 0.00633 AFIX 43 H9 2 0.123814 0.688358 0.826443 11.00000 -1.20000 AFIX 0 C10 1 0.282912 0.700118 0.789193 11.00000 0.02592 0.02597 = 0.03895 0.00167 0.00158 0.00177 C11 1 0.264808 0.730922 0.732727 11.00000 0.02862 0.02139 = 0.03648 -0.00137 -0.00366 -0.00119 C12 1 0.115486 0.790765 0.673404 11.00000 0.02978 0.03176 = 0.03316 0.00051 -0.00613 -0.00456 C13 1 0.176917 0.797695 0.625297 11.00000 0.03732 0.06005 = 0.04006 0.00489 -0.00157 0.00245 AFIX 43 H13 2 0.250912 0.780905 0.623192 11.00000 -1.20000 AFIX 0 C14 1 0.121954 0.831135 0.580282 11.00000 0.05153 0.08275 = 0.03803 0.01681 0.00207 -0.00502 AFIX 43 H14 2 0.159635 0.837386 0.547101 11.00000 -1.20000 AFIX 0 C15 1 0.013132 0.854767 0.584607 11.00000 0.04687 0.06194 = 0.04612 0.01833 -0.01074 -0.00215 AFIX 43 H15 2 -0.023039 0.877594 0.554600 11.00000 -1.20000 AFIX 0 C16 1 -0.043174 0.844665 0.633743 11.00000 0.03346 0.03769 = 0.04552 0.00624 -0.01269 -0.00246 C17 1 -0.163304 0.869154 0.640642 11.00000 0.04125 0.04885 = 0.05855 0.01162 -0.01477 0.00386 AFIX 137 H17A 2 -0.213024 0.828552 0.631434 11.00000 -1.50000 H17B 2 -0.179004 0.910617 0.616504 11.00000 -1.50000 H17C 2 -0.174620 0.883935 0.678395 11.00000 -1.50000 AFIX 0 C18 1 0.457860 0.611899 0.902976 11.00000 0.02281 0.05503 = 0.04819 0.01432 0.00385 0.00393 C19 1 0.661932 0.586825 0.918071 11.00000 0.02529 0.04101 = 0.04551 0.01088 0.00307 0.00084 C20 1 0.653073 0.539947 0.962857 11.00000 0.02952 0.04193 = 0.04073 0.00817 0.00168 -0.00090 AFIX 43 H20 2 0.582875 0.526133 0.976064 11.00000 -1.20000 AFIX 0 C21 1 0.750708 0.513942 0.987689 11.00000 0.03197 0.06560 = 0.06378 0.03267 -0.00475 0.00188 AFIX 43 H21 2 0.747703 0.482552 1.018340 11.00000 -1.20000 AFIX 0 C22 1 0.851938 0.534897 0.966669 11.00000 0.02795 0.11917 = 0.13991 0.08552 -0.01365 0.00388 AFIX 43 H22 2 0.918816 0.517925 0.982909 11.00000 -1.20000 AFIX 0 C23 1 0.854458 0.582171 0.920440 11.00000 0.02490 0.10384 = 0.11384 0.07162 0.00449 0.00310 C24 1 0.963183 0.606479 0.894918 11.00000 0.02134 0.18596 = 0.20274 0.13546 0.01161 0.00675 AFIX 137 H24A 2 0.950412 0.617417 0.856365 11.00000 -1.50000 H24B 2 1.017852 0.567184 0.898543 11.00000 -1.50000 H24C 2 0.990740 0.650365 0.913542 11.00000 -1.50000 AFIX 0 O01 4 1.017257 0.290896 0.932716 10.50000 0.10329 0.03156 = 0.10318 -0.01638 0.02446 -0.00816 O01' 4 0.903965 0.328431 0.923238 10.50000 0.09613 0.08039 = 0.13545 -0.03650 -0.03475 0.00785 C01 1 0.998980 0.344658 0.875755 10.80000 0.05373 0.09265 = 0.22698 -0.08178 0.03387 -0.01660 C01' 1 1.035460 0.375258 0.909872 10.20000 0.10674 0.05924 = 0.15879 0.02623 0.11003 0.04430 C02 1 0.957860 0.384498 0.829047 10.40000 0.04432 0.06134 = 0.08343 0.02882 -0.00076 -0.03848 C02' 1 0.948586 0.430127 0.880526 10.60000 0.01148 0.01698 = 0.06164 -0.00968 0.00235 -0.00176 C03 1 1.011084 0.307016 0.943164 10.50000 0.37328 0.87906 = 0.50563 -0.54727 -0.18960 0.38604 C03' 1 0.939916 0.303511 0.971132 10.50000 0.14618 0.08006 = 0.13031 0.02148 -0.02844 0.01553 C04 1 0.825920 0.277925 0.997468 11.00000 0.39197 0.18519 = 0.16080 -0.04459 -0.07989 0.05475 HKLF 4 Covalent radii and connectivity table for 00SRC072 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 Fe1 - C9 C6 C10 C8 C4 C1 C3 C5 C7 C2 O1 - C11 O2 - C18 N1 - C11 C12 N2 - C12 C16 N3 - C18 C19 N4 - C23 C19 C1 - C2 C5 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 C18 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C9 C6 C11 Fe1 C11 - O1 N1 C10 C12 - N2 C13 N1 C13 - C12 C14 C14 - C15 C13 C15 - C14 C16 C16 - N2 C15 C17 C17 - C16 C18 - O2 N3 C7 C19 - N4 C20 N3 C20 - C19 C21 C21 - C22 C20 C22 - C21 C23 C23 - N4 C22 C24 C24 - C23 O01 - C03' O01' C01' C01 O01' - C03' C03 O01 C01 C01' C01 - C01' C02 O01' C02' O01 C03 C01' - C01 C03 C02' O01 O01' C02 - C01 C02' C02' - C02 C01' C01 C03 - C03' O01' C01' C01 C03' - C03 O01' O01 C04 C04 - C03' h k l Fo^2 Sigma Why rejected 4 0 1 2.26 0.45 observed but should be systematically absent -2 0 1 5.13 0.56 observed but should be systematically absent -2 0 1 16.99 1.59 observed but should be systematically absent -2 0 1 13.13 1.57 observed but should be systematically absent -2 0 3 6.61 0.78 observed but should be systematically absent -2 0 3 6.78 0.90 observed but should be systematically absent -2 0 3 7.70 0.89 observed but should be systematically absent -2 0 3 15.66 2.46 observed but should be systematically absent -2 0 1 5.47 0.45 observed but should be systematically absent -2 0 1 12.60 1.93 observed but should be systematically absent -2 0 1 28.94 7.15 observed but should be systematically absent 4 0 1 2.27 0.45 observed but should be systematically absent 26025 Reflections read, of which 1619 rejected -15 =< h =< 14, -23 =< k =< 23, -30 =< l =< 29, Max. 2-theta = 55.00 12 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 12 14 0 11.50 2.41 2 12.50 -2 4 1 120.68 2.97 4 18.28 -12 2 18 2.16 1.75 2 9.92 3 Inconsistent equivalents 5830 Unique reflections, of which 0 suppressed R(int) = 0.0744 R(sigma) = 0.0753 Friedel opposites merged Maximum memory for data reduction = 3309 / 69160 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 4257 / 461795 wR2 = 0.1878 before cycle 1 for 5830 data and 363 / 363 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.5473 0.1000 ISOR U23 C03 -0.3860 0.1000 ISOR U12 C03 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. 0. 0. 30. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.155 0.000 GooF = S = 1.124; Restrained GooF = 1.127 for 30 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10718 0.00030 -0.821 OSF 341 0.51305 0.08711 -4.202 U22 C03 343 -0.28841 0.06111 4.236 U23 C03 344 -0.03657 0.04419 3.463 U13 C03 345 0.18382 0.05533 -3.655 U12 C03 Mean shift/esd = 0.213 Maximum = 4.236 for U23 C03 Max. shift = 0.039 A for C03 Max. dU =-0.203 for C03 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4257 / 461795 wR2 = 0.1879 before cycle 2 for 5830 data and 363 / 363 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.087 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 30 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10707 0.00030 -0.353 OSF Mean shift/esd = 0.109 Maximum = -1.241 for U23 C03 Max. shift = 0.096 A for C03 Max. dU = 0.043 for C03 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4257 / 461795 wR2 = 0.1875 before cycle 3 for 5830 data and 363 / 363 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.3471 0.1000 ISOR U23 C03 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. 0. 0. 30. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.101 0.000 GooF = S = 1.123; Restrained GooF = 1.123 for 30 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10707 0.00030 -0.010 OSF Mean shift/esd = 0.074 Maximum = 1.106 for y C03 Max. shift = 0.105 A for C03 Max. dU = 0.030 for C03 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4257 / 461795 wR2 = 0.1873 before cycle 4 for 5830 data and 363 / 363 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.3883 0.1000 ISOR U23 C03 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. 0. 0. 30. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.111 0.000 GooF = S = 1.122; Restrained GooF = 1.122 for 30 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.10708 0.00030 0.022 OSF 303 0.87382 0.00068 -1.384 z C01 305 0.10927 0.00818 1.077 U22 C01 311 0.36858 0.00199 -1.262 y C01' 314 0.09040 0.01937 1.119 U22 C01' 316 0.07853 0.02304 1.174 U23 C01' 318 0.09825 0.02053 1.174 U12 C01' 338 0.32153 0.00468 1.252 y C03 339 0.93609 0.00289 -1.016 z C03 Mean shift/esd = 0.089 Maximum = -1.384 for z C01 Max. shift = 0.129 A for C03 Max. dU = 0.014 for C01' Largest correlation matrix elements 0.778 U13 C01' / U33 C01' 0.665 U12 C01' / U11 C01' 0.596 U12 C01' / U22 C01' 0.778 U13 C01' / U11 C01' 0.655 U13 C01' / U23 C01' 0.590 U12 C01' / U13 C01' 0.772 z C01' / x C01' 0.642 U23 C24 / U33 C24 0.584 U23 C01' / U33 C01' 0.724 U12 C01' / U23 C01' 0.632 U23 C24 / U22 C24 0.565 U11 Fe1 / OSF -0.686 U23 C01 / U33 C01 -0.628 U23 C03 / U22 C03 0.553 z C01' / U23 C01 -0.685 z C03 / y C03 0.620 y C01' / x C01' 0.550 U23 C23 / U22 C23 -0.683 U23 C03 / U33 C03 0.606 U23 C22 / U22 C22 -0.548 x C03 / x O01 -0.677 U23 C01 / U22 C01 0.604 z C01' / y C01' -0.544 U12 C03 / U13 C03 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1141 0.7590 0.7509 43 0.860 0.000 N1 C11 C12 H3 0.5837 0.6406 0.8587 43 0.860 0.000 N3 C18 C19 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1A 0.2091 0.5589 0.7018 43 0.930 0.000 C1 C2 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.4099 0.5270 0.7241 43 0.930 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3A 0.4164 0.4661 0.8169 43 0.930 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.2172 0.4622 0.8538 43 0.930 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.0902 0.5186 0.7811 43 0.930 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.4595 0.6832 0.7923 43 0.930 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.2246 0.6317 0.9073 43 0.930 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.1238 0.6884 0.8265 43 0.930 0.000 C9 C8 C10 H13 0.2508 0.7808 0.6233 43 0.930 0.000 C13 C12 C14 H14 0.1597 0.8373 0.5471 43 0.930 0.000 C14 C15 C13 H15 -0.0231 0.8775 0.5546 43 0.930 0.000 C15 C14 C16 H17A -0.2130 0.8286 0.6313 137 0.960 0.000 C17 C16 H17A H17B -0.1788 0.9107 0.6165 137 0.960 0.000 C17 C16 H17A H17C -0.1746 0.8839 0.6784 137 0.960 0.000 C17 C16 H17A H20 0.5828 0.5261 0.9761 43 0.930 0.000 C20 C19 C21 H21 0.7477 0.4826 1.0184 43 0.930 0.000 C21 C22 C20 H22 0.9188 0.5180 0.9829 43 0.930 0.000 C22 C21 C23 H24A 0.9501 0.6180 0.8563 137 0.960 0.000 C24 C23 H24A H24B 1.0174 0.5665 0.8977 137 0.960 0.000 C24 C23 H24A H24C 0.9919 0.6496 0.9137 137 0.960 0.000 C24 C23 H24A 00SRC072 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.28626 0.58881 0.80501 1.00000 0.02243 0.02867 0.06883 0.00877 -0.00238 -0.00044 0.04001 0.00085 0.00004 0.00003 0.00002 0.00000 0.00027 0.00030 0.00038 0.00022 0.00022 0.00019 0.00020 O1 0.33974 0.72978 0.69871 1.00000 0.02730 0.04266 0.03383 -0.00189 0.00562 0.00179 0.03454 0.00370 0.00016 0.00012 0.00008 0.00000 0.00107 0.00132 0.00109 0.00093 0.00092 0.00095 0.00051 O2 0.42661 0.58234 0.94542 1.00000 0.02544 0.08993 0.05354 0.04228 0.00853 0.00683 0.05622 0.00501 0.00019 0.00016 0.00010 0.00000 0.00115 0.00211 0.00146 0.00140 0.00106 0.00120 0.00077 N1 0.15909 0.75980 0.72327 1.00000 0.02551 0.03456 0.03352 0.00197 -0.00158 0.00070 0.03122 0.00427 0.00020 0.00014 0.00010 0.00000 0.00123 0.00147 0.00132 0.00107 0.00102 0.00110 0.00057 H1 0.11415 0.75899 0.75088 1.00000 0.03746 0.00000 0.00000 N2 0.00744 0.81137 0.67762 1.00000 0.02825 0.03107 0.03743 -0.00065 -0.00544 -0.00302 0.03232 0.00429 0.00020 0.00014 0.00010 0.00000 0.00130 0.00142 0.00135 0.00109 0.00106 0.00111 0.00058 N3 0.56924 0.61680 0.88871 1.00000 0.02350 0.04869 0.04081 0.01888 0.00296 0.00138 0.03764 0.00493 0.00020 0.00016 0.00011 0.00000 0.00126 0.00169 0.00143 0.00124 0.00111 0.00120 0.00065 H3 0.58369 0.64062 0.85870 1.00000 0.04517 0.00000 0.00000 N4 0.76022 0.60771 0.89701 1.00000 0.02474 0.07663 0.08726 0.04884 0.00676 0.00596 0.06281 0.00699 0.00023 0.00021 0.00015 0.00000 0.00148 0.00244 0.00233 0.00197 0.00153 0.00150 0.00102 C1 0.23522 0.53598 0.73408 1.00000 0.06623 0.03875 0.10530 -0.02362 -0.02509 -0.00137 0.07039 0.00699 0.00038 0.00024 0.00022 0.00000 0.00274 0.00237 0.00348 0.00230 0.00255 0.00211 0.00126 H1A 0.20910 0.55895 0.70176 1.00000 0.08447 0.00000 0.00000 C2 0.34851 0.51793 0.74657 1.00000 0.05063 0.04409 0.13140 -0.03121 -0.00307 0.01125 0.07542 0.00775 0.00036 0.00025 0.00024 0.00000 0.00250 0.00263 0.00433 0.00274 0.00262 0.00206 0.00143 H2 0.40995 0.52699 0.72408 1.00000 0.09051 0.00000 0.00000 C3 0.35208 0.48395 0.79879 1.00000 0.05473 0.02798 0.15458 0.00871 -0.01832 0.00754 0.07932 0.00878 0.00038 0.00023 0.00025 0.00000 0.00266 0.00227 0.00500 0.00263 0.00288 0.00195 0.00153 H3A 0.41643 0.46608 0.81690 1.00000 0.09518 0.00000 0.00000 C4 0.23903 0.48135 0.81975 1.00000 0.05746 0.03713 0.14613 0.02674 -0.01258 -0.01438 0.08040 0.00882 0.00038 0.00024 0.00025 0.00000 0.00266 0.00245 0.00447 0.00265 0.00280 0.00211 0.00148 H4 0.21721 0.46220 0.85377 1.00000 0.09648 0.00000 0.00000 C5 0.16798 0.51333 0.77892 1.00000 0.04067 0.04430 0.14198 0.00381 -0.01085 -0.01266 0.07579 0.00791 0.00036 0.00024 0.00023 0.00000 0.00218 0.00256 0.00447 0.00264 0.00261 0.00198 0.00141 H5 0.09019 0.51864 0.78105 1.00000 0.09095 0.00000 0.00000 C6 0.39122 0.67801 0.81030 1.00000 0.02079 0.03099 0.03559 0.00287 0.00322 -0.00082 0.02909 0.00515 0.00023 0.00017 0.00012 0.00000 0.00134 0.00167 0.00157 0.00125 0.00117 0.00125 0.00065 H6 0.45946 0.68319 0.79226 1.00000 0.03491 0.00000 0.00000 C7 0.37582 0.64663 0.86394 1.00000 0.02445 0.04127 0.04242 0.01378 0.00242 0.00436 0.03603 0.00587 0.00024 0.00019 0.00013 0.00000 0.00149 0.00190 0.00173 0.00144 0.00131 0.00136 0.00074 C8 0.25809 0.64878 0.87513 1.00000 0.02601 0.05710 0.04658 0.02139 0.01009 0.00628 0.04313 0.00658 0.00025 0.00021 0.00014 0.00000 0.00158 0.00226 0.00189 0.00165 0.00141 0.00153 0.00085 H8 0.22462 0.63167 0.90732 1.00000 0.05175 0.00000 0.00000 C9 0.20123 0.68086 0.82973 1.00000 0.02138 0.03751 0.04894 0.01106 0.00780 0.00635 0.03587 0.00594 0.00025 0.00018 0.00013 0.00000 0.00143 0.00186 0.00183 0.00144 0.00132 0.00133 0.00074 H9 0.12383 0.68838 0.82648 1.00000 0.04304 0.00000 0.00000 C10 0.28295 0.70007 0.78920 1.00000 0.02548 0.02567 0.03875 0.00162 0.00125 0.00196 0.02996 0.00528 0.00023 0.00017 0.00012 0.00000 0.00150 0.00161 0.00160 0.00124 0.00124 0.00123 0.00066 C11 0.26490 0.73090 0.73267 1.00000 0.02880 0.02073 0.03619 -0.00109 -0.00367 -0.00133 0.02862 0.00500 0.00024 0.00016 0.00012 0.00000 0.00150 0.00150 0.00159 0.00118 0.00130 0.00122 0.00064 C12 0.11549 0.79076 0.67339 1.00000 0.02982 0.03139 0.03267 0.00055 -0.00596 -0.00457 0.03137 0.00513 0.00025 0.00017 0.00012 0.00000 0.00156 0.00173 0.00158 0.00126 0.00128 0.00132 0.00068 C13 0.17684 0.79764 0.62535 1.00000 0.03696 0.05956 0.04003 0.00499 -0.00156 0.00234 0.04554 0.00627 0.00029 0.00022 0.00013 0.00000 0.00180 0.00243 0.00183 0.00164 0.00148 0.00169 0.00087 H13 0.25083 0.78082 0.62327 1.00000 0.05465 0.00000 0.00000 C14 0.12201 0.83105 0.58030 1.00000 0.05145 0.08237 0.03795 0.01687 0.00207 -0.00484 0.05724 0.00720 0.00032 0.00025 0.00015 0.00000 0.00224 0.00311 0.00189 0.00187 0.00167 0.00210 0.00107 H14 0.15973 0.83728 0.54712 1.00000 0.06869 0.00000 0.00000 C15 0.01307 0.85469 0.58463 1.00000 0.04643 0.06186 0.04602 0.01824 -0.01091 -0.00193 0.05157 0.00667 0.00031 0.00022 0.00014 0.00000 0.00206 0.00255 0.00205 0.00177 0.00167 0.00187 0.00095 H15 -0.02313 0.87749 0.55462 1.00000 0.06188 0.00000 0.00000 C16 -0.04316 0.84462 0.63376 1.00000 0.03286 0.03751 0.04521 0.00651 -0.01224 -0.00275 0.03867 0.00558 0.00026 0.00019 0.00013 0.00000 0.00165 0.00189 0.00181 0.00146 0.00142 0.00146 0.00076 C17 -0.16320 0.86917 0.64061 1.00000 0.04112 0.04813 0.05833 0.01152 -0.01473 0.00402 0.04936 0.00662 0.00029 0.00022 0.00015 0.00000 0.00192 0.00233 0.00215 0.00171 0.00164 0.00170 0.00090 H17A -0.21296 0.82862 0.63131 1.00000 0.07405 0.00000 0.00000 H17B -0.17876 0.91070 0.61652 1.00000 0.07405 0.00000 0.00000 H17C -0.17460 0.88386 0.67837 1.00000 0.07405 0.00000 0.00000 C18 0.45788 0.61191 0.90301 1.00000 0.02276 0.05432 0.04814 0.01397 0.00393 0.00379 0.04170 0.00641 0.00026 0.00021 0.00014 0.00000 0.00148 0.00218 0.00193 0.00167 0.00141 0.00150 0.00082 C19 0.66194 0.58687 0.91810 1.00000 0.02453 0.04098 0.04580 0.01112 0.00308 0.00107 0.03707 0.00597 0.00026 0.00018 0.00013 0.00000 0.00150 0.00195 0.00179 0.00147 0.00134 0.00136 0.00075 C20 0.65305 0.53994 0.96287 1.00000 0.02892 0.04143 0.04035 0.00828 0.00134 -0.00096 0.03689 0.00555 0.00025 0.00018 0.00012 0.00000 0.00157 0.00197 0.00171 0.00144 0.00134 0.00141 0.00075 H20 0.58285 0.52609 0.97605 1.00000 0.04427 0.00000 0.00000 C21 0.75067 0.51396 0.98771 1.00000 0.03194 0.06524 0.06353 0.03260 -0.00476 0.00162 0.05363 0.00713 0.00028 0.00023 0.00016 0.00000 0.00177 0.00270 0.00233 0.00197 0.00160 0.00174 0.00103 H21 0.74768 0.48258 1.01837 1.00000 0.06436 0.00000 0.00000 C22 0.85193 0.53494 0.96667 1.00000 0.02702 0.11994 0.13957 0.08632 -0.01364 0.00376 0.09568 0.01016 0.00033 0.00031 0.00023 0.00000 0.00193 0.00471 0.00444 0.00392 0.00235 0.00236 0.00208 H22 0.91882 0.51799 0.98291 1.00000 0.11481 0.00000 0.00000 C23 0.85443 0.58216 0.92046 1.00000 0.02334 0.10436 0.11480 0.07232 0.00416 0.00324 0.08080 0.00980 0.00031 0.00029 0.00022 0.00000 0.00183 0.00388 0.00369 0.00313 0.00211 0.00202 0.00167 C24 0.96328 0.60621 0.89471 1.00000 0.02018 0.18260 0.20368 0.13409 0.01196 0.00624 0.13537 0.01416 0.00034 0.00041 0.00031 0.00000 0.00199 0.00644 0.00668 0.00575 0.00295 0.00284 0.00315 H24A 0.95006 0.61796 0.85632 1.00000 0.20306 0.00000 0.00000 H24B 1.01735 0.56647 0.89770 1.00000 0.20306 0.00000 0.00000 H24C 0.99187 0.64955 0.91367 1.00000 0.20306 0.00000 0.00000 O01 1.01691 0.29081 0.93260 0.50000 0.10617 0.03381 0.10305 -0.01704 0.02256 -0.00969 0.08078 0.01645 0.00091 0.00041 0.00042 0.00000 0.00634 0.00345 0.00554 0.00372 0.00478 0.00373 0.00241 O01' 0.90356 0.32870 0.92314 0.50000 0.09266 0.08254 0.13375 -0.03641 -0.03402 0.00920 0.10338 0.01308 0.00072 0.00047 0.00041 0.00000 0.00568 0.00553 0.00705 0.00504 0.00498 0.00450 0.00256 C01 0.99921 0.34563 0.87382 0.80000 0.05944 0.10927 0.24331 -0.10150 0.04415 -0.02284 0.13688 0.01722 0.00074 0.00060 0.00068 0.00000 0.00439 0.00818 0.01529 0.01070 0.00673 0.00479 0.00628 C01' 1.02775 0.36858 0.90655 0.20000 0.13146 0.09040 0.15354 0.07853 0.12941 0.09825 0.12373 0.11427 0.00371 0.00199 0.00204 0.00000 0.02792 0.01937 0.03196 0.02304 0.02805 0.02053 0.01766 C02 0.95684 0.38510 0.82858 0.40000 0.04415 0.06565 0.08864 0.03509 -0.00599 -0.04015 0.06623 0.01986 0.00091 0.00067 0.00051 0.00000 0.00565 0.00723 0.00776 0.00637 0.00555 0.00535 0.00329 C02' 0.94850 0.43013 0.88057 0.60000 0.01019 0.01710 0.06182 -0.01009 0.00234 -0.00172 0.02968 0.00820 0.00035 0.00026 0.00022 0.00000 0.00198 0.00236 0.00326 0.00217 0.00208 0.00175 0.00111 C03 1.01890 0.32153 0.93609 0.50000 0.28995 0.64433 0.40552 -0.38631 -0.01532 0.16897 0.44683 0.09970 0.00477 0.00468 0.00289 0.00000 0.05011 0.07741 0.05572 0.05487 0.04263 0.05076 0.03973 C03' 0.94160 0.30293 0.97033 0.50000 0.13304 0.09816 0.12743 0.02237 -0.02037 0.01250 0.11979 0.03286 0.00180 0.00093 0.00085 0.00000 0.01396 0.01082 0.01390 0.00977 0.01164 0.01008 0.00526 C04 0.82881 0.27840 0.99671 1.00000 0.42037 0.18762 0.16247 -0.04859 -0.10115 0.06842 0.25799 0.02334 0.00156 0.00076 0.00053 0.00000 0.02665 0.01479 0.00914 0.00949 0.01497 0.01527 0.00848 Final Structure Factor Calculation for 00SRC072 in C2/c Total number of l.s. parameters = 363 Maximum vector length = 511 Memory required = 3894 / 24017 wR2 = 0.1872 before cycle 5 for 5830 data and 0 / 363 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.3863 0.1000 ISOR U23 C03 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. 0. 0. 30. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.111 0.000 GooF = S = 1.121; Restrained GooF = 1.121 for 30 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0623 for 3597 Fo > 4sig(Fo) and 0.1144 for all 5830 data wR2 = 0.1872, GooF = S = 1.121, Restrained GooF = 1.121 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0709 0.0268 0.0223 Fe1 0.0431 0.0365 0.0241 O1 0.1187 0.0281 0.0219 O2 0.0361 0.0326 0.0249 N1 0.0406 0.0323 0.0241 N2 0.0642 0.0259 0.0228 N3 0.1316 0.0328 0.0240 N4 0.1242 0.0584 0.0286 C1 0.1422 0.0545 0.0296 C2 0.1592 0.0542 0.0246 C3 0.1557 0.0588 0.0267 C4 0.1440 0.0540 0.0294 C5 0.0372 0.0300 0.0201 C6 0.0562 0.0287 0.0232 C7 0.0760 0.0314 0.0219 C8 0.0580 0.0310 0.0187 C9 0.0390 0.0273 0.0236 C10 0.0382 0.0274 0.0203 C11 0.0395 0.0313 0.0233 C12 0.0609 0.0407 0.0350 C13 0.0886 0.0514 0.0318 C14 0.0763 0.0490 0.0294 C15 0.0562 0.0350 0.0248 C16 0.0708 0.0496 0.0277 C17 0.0661 0.0369 0.0221 C18 0.0550 0.0321 0.0242 C19 0.0492 0.0330 0.0285 C20 0.0972 0.0368 0.0270 C21 0.2172 0.0496 0.0202 C22 may be split into 0.8514 0.5425 0.9730 and 0.8524 0.5274 0.9603 0.1821 0.0371 0.0232 C23 0.3279 0.0588 0.0194 C24 may be split into 0.9645 0.6160 0.9026 and 0.9621 0.5964 0.8868 0.1288 0.0840 0.0296 O01 0.1704 0.0795 0.0603 O01' 0.3062 0.0547 0.0497 C01 may be split into 1.0036 0.3391 0.8828 and 0.9948 0.3522 0.8648 0.3313 0.0387 0.0012 C01' may be split into 1.0423 0.3755 0.9136 and 1.0132 0.3617 0.8995 0.1264 0.0629 0.0093 C02 0.0640 0.0152 0.0098 C02' 0.9650 0.2957 0.0798 C03 may be split into 1.0260 0.3397 0.9265 and 1.0118 0.3033 0.9456 0.1540 0.1279 0.0775 C03' 0.4827 0.1752 0.1161 C04 may be split into 0.8497 0.2825 0.9927 and 0.8080 0.2743 1.0007 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.028 0.037 0.049 0.063 0.086 0.127 1.000 Number in group 639. 561. 584. 576. 562. 618. 546. 595. 568. 581. GooF 0.915 0.975 1.031 1.109 1.255 1.357 1.239 1.168 1.071 1.015 K 4.949 1.196 0.923 1.025 1.032 1.028 1.014 1.005 1.006 1.019 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 607. 569. 585. 578. 580. 583. 577. 585. 579. 587. GooF 0.915 0.884 0.886 0.972 1.049 1.138 1.111 1.059 1.201 1.735 K 1.054 0.993 1.035 1.021 1.019 1.020 1.028 1.029 1.028 1.009 R1 0.400 0.279 0.217 0.158 0.116 0.093 0.078 0.059 0.053 0.056 Recommended weighting scheme: WGHT 0.1008 4.2773 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) 2 4 2 838.65 369.44 5.88 0.038 3.42 -2 2 5 372.05 768.57 5.37 0.054 3.48 -4 0 2 646.14 1217.73 4.99 0.068 2.89 4 2 7 272.62 60.43 4.85 0.015 2.16 1 3 1 9014.77 5384.83 4.73 0.143 5.20 2 8 6 253.50 20.22 4.67 0.009 1.85 2 4 9 527.74 192.63 4.63 0.027 2.13 -3 3 3 1895.56 3257.81 4.40 0.111 3.06 1 1 3 647.41 1103.40 4.30 0.065 6.20 -4 0 4 1198.31 2031.74 4.29 0.088 2.68 0 12 14 160.36 423.22 4.21 0.040 1.13 -3 5 1 834.58 522.21 4.18 0.045 2.64 4 6 1 660.89 387.51 4.00 0.038 2.09 -2 2 3 8753.20 14055.65 3.93 0.231 4.24 -3 9 18 206.23 89.37 3.92 0.018 1.07 4 0 20 103.12 370.99 3.91 0.038 1.11 -2 6 5 423.88 221.99 3.89 0.029 2.34 -6 2 5 266.79 464.80 3.88 0.042 1.80 -1 3 11 894.02 579.14 3.88 0.047 2.03 -5 1 2 1381.14 913.26 3.84 0.059 2.32 5 5 5 386.77 185.00 3.83 0.027 1.82 2 8 8 1169.64 693.90 3.78 0.051 1.72 2 6 22 931.04 534.70 3.77 0.045 1.01 -5 5 1 491.00 798.13 3.69 0.055 1.97 0 2 5 11138.28 7566.20 3.67 0.170 4.25 1 3 0 20017.21 31169.91 3.63 0.345 5.33 2 0 0 52385.25 81422.29 3.62 0.557 5.93 4 4 6 467.64 755.42 3.56 0.054 2.09 2 14 19 947.55 519.09 3.54 0.044 0.89 -1 11 16 2227.88 1480.39 3.52 0.075 1.10 7 3 8 846.53 493.56 3.49 0.043 1.42 0 12 13 129.22 317.93 3.49 0.035 1.16 -4 4 4 3985.06 6012.01 3.46 0.151 2.30 2 4 24 560.60 291.26 3.45 0.033 0.96 -7 1 2 787.82 511.21 3.44 0.044 1.67 5 5 6 283.18 101.20 3.40 0.020 1.76 -4 0 6 158.31 76.70 3.40 0.017 2.41 3 7 8 793.62 1223.99 3.39 0.068 1.74 -3 7 6 784.37 1227.21 3.39 0.068 1.90 4 4 1 1095.99 1651.99 3.38 0.079 2.46 8 8 14 41.95 297.86 3.37 0.034 1.00 -5 3 16 400.33 689.83 3.34 0.051 1.25 -5 1 4 6517.80 4588.08 3.34 0.132 2.20 2 2 4 889.45 605.84 3.33 0.048 3.80 9 13 18 1286.48 4.82 3.32 0.004 0.77 -1 5 8 825.20 552.53 3.32 0.046 2.27 3 3 25 244.46 514.50 3.30 0.044 0.92 -1 9 13 458.87 781.62 3.28 0.055 1.35 3 3 8 1406.32 968.29 3.27 0.061 2.21 -6 2 6 706.47 458.32 3.25 0.042 1.75 Bond lengths and angles Fe1 - Distance Angles C9 2.0276 (0.0031) C6 2.0281 (0.0030) 69.44 (0.12) C10 2.0291 (0.0031) 41.28 (0.11) 41.25 (0.12) C8 2.0361 (0.0037) 40.31 (0.13) 68.98 (0.13) 68.60 (0.13) C4 2.0374 (0.0041) 125.25 (0.17) 154.61 (0.16) 162.93 (0.16) 107.69 (0.20) C1 2.0384 (0.0044) 118.82 (0.16) 126.29 (0.17) 107.07 (0.16) 153.09 (0.16) 68.25 (0.22) C3 2.0403 (0.0041) 164.35 (0.18) 119.63 (0.15) 153.68 (0.16) 127.95 (0.19) 41.42 (0.19) 67.65 (0.21) C5 2.0403 (0.0042) 106.65 (0.17) 163.66 (0.17) 125.57 (0.16) 118.97 (0.18) 40.38 (0.19) 40.57 (0.19) 68.25 (0.18) C7 2.0425 (0.0035) 68.81 (0.13) 40.99 (0.12) 68.97 (0.13) 40.97 (0.12) 119.92 (0.18) 164.45 (0.17) 108.82 (0.18) C2 2.0442 (0.0043) 153.50 (0.19) 107.71 (0.16) 119.10 (0.18) 165.18 (0.17) 68.74 (0.22) 40.40 (0.17) 40.06 (0.20) Fe1 - C9 C6 C10 C8 C4 C1 C3 O1 - Distance Angles C11 1.2181 (0.0033) O1 - O2 - Distance Angles C18 1.2154 (0.0038) O2 - N1 - Distance Angles C11 1.3729 (0.0036) C12 1.4151 (0.0038) 127.46 (0.24) N1 - C11 N2 - Distance Angles C12 1.3394 (0.0039) C16 1.3466 (0.0040) 118.46 (0.26) N2 - C12 N3 - Distance Angles C18 1.3736 (0.0038) C19 1.4046 (0.0040) 126.66 (0.25) N3 - C18 N4 - Distance Angles C23 1.3257 (0.0048) C19 1.3331 (0.0039) 118.47 (0.30) N4 - C23 C1 - Distance Angles C2 1.4098 (0.0060) C5 1.4140 (0.0066) 108.57 (0.46) Fe1 2.0384 (0.0044) 70.02 (0.26) 69.79 (0.27) C1 - C2 C5 C2 - Distance Angles C3 1.3990 (0.0070) C1 1.4098 (0.0059) 107.86 (0.45) Fe1 2.0442 (0.0043) 69.82 (0.28) 69.58 (0.24) C2 - C3 C1 C3 - Distance Angles C2 1.3990 (0.0070) C4 1.4419 (0.0067) 108.39 (0.44) Fe1 2.0403 (0.0041) 70.12 (0.24) 69.18 (0.24) C3 - C2 C4 C4 - Distance Angles C5 1.4075 (0.0066) C3 1.4419 (0.0068) 106.91 (0.48) Fe1 2.0374 (0.0041) 69.92 (0.24) 69.40 (0.22) C4 - C5 C3 C5 - Distance Angles C4 1.4075 (0.0066) C1 1.4140 (0.0067) 108.26 (0.40) Fe1 2.0403 (0.0042) 69.70 (0.24) 69.64 (0.23) C5 - C4 C1 C6 - Distance Angles C7 1.4253 (0.0041) C10 1.4293 (0.0041) 107.71 (0.23) Fe1 2.0281 (0.0029) 70.05 (0.18) 69.41 (0.17) C6 - C7 C10 C7 - Distance Angles C6 1.4253 (0.0041) C8 1.4273 (0.0039) 107.56 (0.26) C18 1.4804 (0.0045) 130.60 (0.26) 121.73 (0.27) Fe1 2.0425 (0.0034) 68.96 (0.18) 69.28 (0.20) 123.99 (0.25) C7 - C6 C8 C18 C8 - Distance Angles C9 1.4001 (0.0045) C7 1.4273 (0.0039) 108.86 (0.26) Fe1 2.0361 (0.0037) 69.52 (0.19) 69.76 (0.20) C8 - C9 C7 C9 - Distance Angles C8 1.4001 (0.0046) C10 1.4300 (0.0039) 108.08 (0.26) Fe1 2.0276 (0.0031) 70.17 (0.20) 69.42 (0.17) C9 - C8 C10 C10 - Distance Angles C9 1.4300 (0.0039) C6 1.4293 (0.0041) 107.78 (0.26) C11 1.4837 (0.0042) 128.96 (0.27) 123.04 (0.24) Fe1 2.0291 (0.0031) 69.30 (0.17) 69.33 (0.17) 122.70 (0.21) C10 - C9 C6 C11 C11 - Distance Angles O1 1.2181 (0.0033) N1 1.3729 (0.0036) 124.74 (0.26) C10 1.4837 (0.0042) 121.08 (0.26) 114.18 (0.24) C11 - O1 N1 C12 - Distance Angles N2 1.3394 (0.0039) C13 1.3841 (0.0043) 123.81 (0.29) N1 1.4151 (0.0038) 112.32 (0.25) 123.85 (0.28) C12 - N2 C13 C13 - Distance Angles C12 1.3841 (0.0043) C14 1.3925 (0.0050) 116.52 (0.33) C13 - C12 C14 - Distance Angles C15 1.3655 (0.0053) C13 1.3925 (0.0050) 120.26 (0.33) C14 - C15 C15 - Distance Angles C14 1.3655 (0.0053) C16 1.3816 (0.0048) 119.75 (0.32) C15 - C14 C16 - Distance Angles N2 1.3466 (0.0040) C15 1.3816 (0.0048) 121.10 (0.30) C17 1.5019 (0.0046) 117.01 (0.29) 121.89 (0.30) C16 - N2 C15 C17 - Distance Angles C16 1.5019 (0.0046) C17 - C18 - Distance Angles O2 1.2154 (0.0038) N3 1.3736 (0.0038) 123.18 (0.30) C7 1.4804 (0.0045) 120.81 (0.27) 116.00 (0.27) C18 - O2 N3 C19 - Distance Angles N4 1.3331 (0.0039) C20 1.3739 (0.0043) 123.39 (0.30) N3 1.4046 (0.0040) 112.50 (0.27) 124.09 (0.27) C19 - N4 C20 C20 - Distance Angles C19 1.3739 (0.0043) C21 1.3761 (0.0045) 118.31 (0.29) C20 - C19 C21 - Distance Angles C22 1.3645 (0.0052) C20 1.3761 (0.0045) 118.98 (0.33) C21 - C22 C22 - Distance Angles C21 1.3645 (0.0052) C23 1.3998 (0.0056) 119.54 (0.36) C22 - C21 C23 - Distance Angles N4 1.3257 (0.0048) C22 1.3998 (0.0056) 121.31 (0.33) C24 1.5052 (0.0051) 116.60 (0.36) 122.09 (0.38) C23 - N4 C22 C24 - Distance Angles C23 1.5052 (0.0051) C24 - O01 - Distance Angles C03' 1.3040 (0.0248) O01' 1.5200 (0.0141) 54.26 (0.83) C01' 1.5344 (0.0286) 101.41 (1.35) 67.24 (1.66) C01 1.7348 (0.0196) 113.66 (1.02) 61.95 (0.59) 32.99 (2.32) O01 - C03' O01' C01' O01' - Distance Angles C03' 1.3021 (0.0176) C03 1.4041 (0.0550) 56.69 (3.51) O01 1.5200 (0.0141) 54.38 (1.12) 21.50 (3.21) C01 1.6852 (0.0162) 116.97 (1.27) 60.57 (3.42) 65.30 (0.69) C01' 1.6911 (0.0424) 93.79 (2.02) 40.71 (4.07) 56.79 (1.09) 32.60 (1.89) O01' - C03' C03 O01 C01 C01 - Distance Angles C01' 0.9478 (0.0617) C02 1.3874 (0.0174) 123.64 (2.18) O01' 1.6852 (0.0162) 74.04 (2.24) 114.06 (0.86) C02' 1.6377 (0.0112) 69.09 (1.80) 58.57 (0.80) 80.98 (0.56) O01 1.7348 (0.0196) 61.81 (2.12) 165.63 (0.84) 52.75 (0.64) 118.78 (0.85) C03 1.5767 (0.0789) 43.92 (3.60) 159.21 (2.17) 50.86 (2.15) 101.95 (2.38) 18.59 (2.60) C01 - C01' C02 O01' C02' O01 C01' - Distance Angles C01 0.9478 (0.0613) C03 1.1097 (0.1038) 99.75 (5.66) C02' 1.5723 (0.0330) 76.64 (3.23) 136.56 (4.18) O01 1.5344 (0.0284) 85.20 (3.32) 15.88 (2.69) 138.26 (3.32) O01' 1.6911 (0.0420) 73.35 (3.45) 55.61 (3.66) 82.71 (2.03) 55.97 (1.28) C01' - C01 C03 C02' O01 C02 - Distance Angles C01 1.3874 (0.0174) C02' 1.4957 (0.0141) 69.11 (0.69) C02 - C01 C02' - Distance Angles C02 1.4957 (0.0141) C01' 1.5723 (0.0330) 84.77 (1.95) C01 1.6377 (0.0113) 52.32 (0.63) 34.27 (2.17) C02' - C02 C01' C03 - Distance Angles C03' 1.2881 (0.0757) O01' 1.4041 (0.0545) 57.65 (2.61) C01' 1.1097 (0.1037) 133.17 (5.21) 83.68 (5.07) C01 1.5767 (0.0789) 125.88 (4.42) 68.57 (3.27) 36.33 (3.81) C03 - C03' O01' C01' C03' - Distance Angles C03 1.2881 (0.0765) O01' 1.3021 (0.0176) 65.65 (3.18) O01 1.3040 (0.0248) 24.81 (3.15) 71.36 (1.26) C04 1.5544 (0.0211) 164.22 (3.39) 99.78 (1.49) 147.45 (1.66) C03' - C03 O01' O01 C04 - Distance Angles C03' 1.5544 (0.0211) C04 - FMAP and GRID set by program FMAP 2 2 22 GRID -1.316 24 -2 1.316 1 2 R1 = 0.1121 for 5830 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.68 at 0.4334 0.0850 0.3558 [ 0.68 A from C02' ] Deepest hole -0.63 at 0.2137 0.1054 0.6622 [ 0.85 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4262 / 41657 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9334 0.4150 0.8558 1.00000 0.05 0.68 0.68 C02' 0.90 C02 1.53 C01 1.84 C01' Q2 1 0.9763 0.4047 0.8835 1.00000 0.05 0.66 0.57 C02' 1.04 C01' 1.12 C01 1.39 C02 Q3 1 0.9431 0.4191 0.8974 1.00000 0.05 0.52 0.46 C02' 1.37 C01' 1.58 C01 1.78 C02 Q4 1 0.8712 0.2775 0.8595 1.00000 0.05 0.50 1.82 O01' 1.97 C01 2.10 H17A 2.16 C6 Q5 1 0.9754 0.3686 0.8302 1.00000 0.05 0.48 0.37 C02 1.16 C01 1.68 C02' 1.93 C01' Q6 1 1.0732 0.3717 0.9314 1.00000 0.05 0.43 0.80 C01' 1.11 C03 1.60 O01 1.70 C01 Q7 1 0.9644 0.6370 0.9297 1.00000 0.05 0.43 0.56 H24C 1.01 C24 1.61 H24B 1.65 C23 Q8 1 0.9525 0.5883 0.8862 1.00000 0.05 0.41 0.40 C24 0.90 H24A 0.90 H24B 1.36 H24C Q9 1 0.9791 0.3247 0.8739 1.00000 0.05 0.35 0.44 C01 1.25 C01' 1.50 O01' 1.56 C02 Q10 1 0.8533 0.5885 0.9565 1.00000 0.05 0.35 0.88 C23 0.99 C22 1.61 H22 1.83 N4 Shortest distances between peaks (including symmetry equivalents) 2 3 0.58 1 2 0.85 1 3 1.01 1 5 1.15 5 9 1.31 7 8 1.37 2 5 1.44 2 9 1.45 4 9 1.57 7 10 1.71 2 6 1.72 1 9 1.76 3 9 1.83 3 5 1.90 3 6 1.93 6 9 1.96 8 10 2.08 4 5 2.17 1 6 2.56 1 4 2.57 2 4 2.66 5 6 2.69 3 4 2.82 6 10 2.91 Time profile in seconds ----------------------- 0.19: 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 0.02: Analyse other restraints etc. 3.80: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.31: Structure factors and derivatives 5.77: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.78: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.13: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:05:22 Total CPU time: 14.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++