+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 14:54:10 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S93 in Pbca CELL 0.71073 12.1886 9.5923 31.3227 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0001 0.0005 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N FE I UNIT 136 216 16 8 8 V = 3662.15 F(000) = 1776.0 Mu = 2.51 mm-1 Cell Wt = 3537.25 Rho = 1.604 MERG 2 SHEL 7 0.84 HFIX 137 -1.50 C12 C13 C16 C14 C17 H17A HFIX 23 -1.20 C15 C11 HFIX 43 -1.20 C5 C8 C6 C10 C3 C4 C9 C7 FMAP 2 PLAN 10 SIZE 0.20 0.30 0.40 ACTA BOND $H WGHT 0.01410 4.91200 L.S. 12 TEMP -153.00 FVAR 0.18431 I1 5 0.912033 0.637725 0.671339 11.00000 0.02418 0.02356 = 0.02938 -0.00459 0.00090 0.00063 FE1 4 0.920127 0.216413 0.558016 11.00000 0.01832 0.01959 = 0.01952 -0.00067 -0.00083 0.00137 N1 3 0.944131 0.184569 0.698364 11.00000 0.02047 0.02339 = 0.01982 0.00191 -0.00037 0.00029 N2 3 1.218553 0.323433 0.632207 11.00000 0.02341 0.03741 = 0.03015 0.00127 -0.00426 -0.00505 C15 1 1.122798 0.358626 0.605474 11.00000 0.02442 0.02782 = 0.02858 -0.00021 -0.00041 -0.00018 C5 1 0.936916 0.045193 0.596017 11.00000 0.02015 0.01804 = 0.02468 0.00030 -0.00503 0.00107 C8 1 0.893265 0.408227 0.531948 11.00000 0.02995 0.02311 = 0.03180 0.00638 -0.00113 0.00128 C6 1 0.756847 0.257247 0.551640 11.00000 0.01738 0.03990 = 0.03258 0.01055 -0.00326 0.00362 C12 1 0.934149 0.030051 0.702344 11.00000 0.04519 0.02256 = 0.02913 0.00650 0.00050 0.00270 C10 1 0.800815 0.210513 0.512466 11.00000 0.02989 0.02871 = 0.02723 0.00246 -0.01167 0.00051 C13 1 0.871155 0.252889 0.730554 11.00000 0.02426 0.03993 = 0.02224 -0.00339 0.00389 -0.00115 C16 1 1.307181 0.268877 0.606495 11.00000 0.02071 0.05769 = 0.03953 0.00394 0.00181 -0.00701 C11 1 0.908045 0.232114 0.654134 11.00000 0.02126 0.02323 = 0.01842 0.00012 -0.00065 0.00086 C2 1 1.058692 0.229956 0.594180 11.00000 0.01803 0.02145 = 0.02060 0.00179 -0.00101 0.00057 C14 1 1.059729 0.229569 0.706393 11.00000 0.02320 0.04910 = 0.02004 -0.00123 -0.00077 -0.00141 C1 1 0.969948 0.169718 0.617753 11.00000 0.01684 0.01871 = 0.01651 -0.00183 -0.00176 0.00196 C3 1 1.077026 0.142812 0.557933 11.00000 0.02097 0.02846 = 0.02061 0.00145 0.00125 0.00435 C4 1 1.002652 0.030076 0.559325 11.00000 0.02842 0.02317 = 0.02211 -0.00780 -0.00551 0.00870 C9 1 0.885107 0.303701 0.500137 11.00000 0.03019 0.03154 = 0.02573 0.00615 -0.00193 0.00241 C17 1 1.258743 0.443465 0.655961 11.00000 0.04113 0.04505 = 0.03827 -0.00195 -0.00776 -0.02120 C7 1 0.813797 0.379436 0.563812 11.00000 0.02670 0.02624 = 0.03149 0.00392 0.00045 0.01109 HKLF 4 Covalent radii and connectivity table for S93 in Pbca C 0.770 H 0.320 N 0.700 FE 1.240 I 1.330 I1 - no bonds found Fe1 - C1 C2 C10 C6 C3 C5 C7 C8 C9 C4 N1 - C12 C14 C13 C11 N2 - C16 C17 C15 C15 - N2 C2 C5 - C4 C1 Fe1 C8 - C9 C7 Fe1 C6 - C10 C7 Fe1 C12 - N1 C10 - C6 C9 Fe1 C13 - N1 C16 - N2 C11 - C1 N1 C2 - C3 C1 C15 Fe1 C14 - N1 C1 - C2 C5 C11 Fe1 C3 - C4 C2 Fe1 C4 - C5 C3 Fe1 C9 - C10 C8 Fe1 C17 - N2 C7 - C6 C8 Fe1 h k l Fo^2 Sigma Why rejected 7 6 0 17.58 2.93 observed but should be systematically absent 10 0 5 5.76 1.44 observed but should be systematically absent 6 0 7 7.15 1.43 observed but should be systematically absent 6 0 1 10.16 1.45 observed but should be systematically absent 2 0 7 7.22 1.44 observed but should be systematically absent 6 0 1 7.32 1.46 observed but should be systematically absent 0 1 6 8.71 1.45 observed but should be systematically absent 11 1 0 20.30 2.90 observed but should be systematically absent 0 3 7 14.30 1.43 observed but should be systematically absent 0 3 13 8.62 1.44 observed but should be systematically absent 0 3 15 5.76 1.44 observed but should be systematically absent 0 5 13 5.77 1.44 observed but should be systematically absent 0 5 15 7.19 1.44 observed but should be systematically absent 0 5 16 7.20 1.44 observed but should be systematically absent 1 7 0 8.61 1.44 observed but should be systematically absent 16759 Reflections read, of which 3160 rejected -14 =< h =< 13, -11 =< k =< 11, -37 =< l =< 37, Max. 2-theta = 50.05 15 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 1 2 638.02 5.71 17 36.25 1 Inconsistent equivalents 3191 Unique reflections, of which 0 suppressed R(int) = 0.0417 R(sigma) = 0.0315 Friedel opposites merged Maximum memory for data reduction = 2608 / 32205 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. Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C12 The center of the range is eclipsed (cis) to C14 and rotation is clockwise looking down N1 to C12 43 48 61 80 87 70 34 1 -10 6 42 75 86 73 52 34 21 18 32 61 79 70 49 40 After local symmetry averaging: 18 24 45 72 84 71 45 25 Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C13 The center of the range is eclipsed (cis) to C12 and rotation is clockwise looking down N1 to C13 32 38 56 78 90 76 50 33 31 42 70 92 87 58 24 5 7 21 43 61 65 56 42 34 After local symmetry averaging: 23 34 56 77 81 63 39 24 Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C16 The center of the range is eclipsed (cis) to C17 and rotation is clockwise looking down N2 to C16 11 20 39 62 69 52 17 -5 2 19 26 39 58 59 41 19 4 9 36 66 78 60 28 10 After local symmetry averaging: 6 16 34 56 68 57 29 8 Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C14 The center of the range is eclipsed (cis) to C12 and rotation is clockwise looking down N1 to C14 -18 9 44 65 68 53 28 10 10 20 38 57 59 34 4 -3 5 18 41 66 72 56 21 -13 After local symmetry averaging: 0 16 41 63 67 48 18 -2 Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C17 The center of the range is eclipsed (cis) to C16 and rotation is clockwise looking down N2 to C17 30 38 59 81 92 84 69 57 51 52 59 72 87 91 75 47 24 27 42 50 53 50 46 37 After local symmetry averaging: 35 39 53 68 77 75 63 47 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0614 before cycle 1 for 3191 data and 195 / 195 parameters GooF = S = 1.160; Restrained GooF = 1.160 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18442 0.00020 0.549 OSF Mean shift/su = 0.282 Maximum = 2.583 for z C17 Max. shift = 0.031 A for H17A Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0608 before cycle 2 for 3191 data and 195 / 195 parameters GooF = S = 1.149; Restrained GooF = 1.149 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.152 OSF Mean shift/su = 0.108 Maximum = 1.085 for z C17 Max. shift = 0.021 A for H17A Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 3 for 3191 data and 195 / 195 parameters GooF = S = 1.148; Restrained GooF = 1.148 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.014 OSF Mean shift/su = 0.010 Maximum = -0.272 for tors H17A Max. shift = 0.007 A for H17A Max. dU = 0.000 for C17 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 4 for 3191 data and 195 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.003 OSF Mean shift/su = 0.003 Maximum = -0.095 for tors H17A Max. shift = 0.003 A for H17A Max. dU = 0.000 for C17 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0608 before cycle 5 for 3191 data and 195 / 195 parameters GooF = S = 1.148; Restrained GooF = 1.148 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 -0.001 OSF Mean shift/su = 0.001 Maximum = -0.033 for tors H17A Max. shift = 0.001 A for H17A Max. dU = 0.000 for C17 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0608 before cycle 6 for 3191 data and 195 / 195 parameters GooF = S = 1.148; Restrained GooF = 1.148 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.001 OSF Mean shift/su = 0.000 Maximum = -0.012 for tors H17A Max. shift = 0.000 A for H17A Max. dU = 0.000 for C17 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0608 before cycle 7 for 3191 data and 195 / 195 parameters GooF = S = 1.148; Restrained GooF = 1.148 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.004 for tors H17A Max. shift = 0.000 A for H17B Max. dU = 0.000 for C11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 8 for 3191 data and 195 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H17A Max. shift = 0.000 A for H17A Max. dU = 0.000 for C13 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0608 before cycle 9 for 3191 data and 195 / 195 parameters GooF = S = 1.148; Restrained GooF = 1.148 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z I1 Max. shift = 0.000 A for H17B Max. dU = 0.000 for N1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 10 for 3191 data and 195 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z I1 Max. shift = 0.000 A for H17A Max. dU = 0.000 for N1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 11 for 3191 data and 195 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z I1 Max. shift = 0.000 A for H13B Max. dU = 0.000 for C16 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3217 / 242807 wR2 = 0.0607 before cycle 12 for 3191 data and 195 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18445 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z I1 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C17 Largest correlation matrix elements 0.552 U11 I1 / OSF 0.515 U22 I1 / OSF Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H15A 1.1478 0.4051 0.5790 23 0.990 0.000 C15 N2 C2 H15B 1.0747 0.4242 0.6211 23 0.990 0.000 C15 N2 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.8802 -0.0166 0.6049 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.9429 0.4843 0.5319 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.6989 0.2143 0.5672 43 0.950 0.000 C6 C10 C7 H12A 0.9821 -0.0151 0.6813 137 0.980 0.000 C12 N1 H12A H12B 0.8582 0.0020 0.6974 137 0.980 0.000 C12 N1 H12A H12C 0.9566 0.0015 0.7312 137 0.980 0.000 C12 N1 H12A ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.7780 0.1299 0.4972 43 0.950 0.000 C10 C6 C9 H13A 0.7953 0.2212 0.7264 137 0.980 0.000 C13 N1 H13A H13B 0.8745 0.3543 0.7272 137 0.980 0.000 C13 N1 H13A H13C 0.8954 0.2277 0.7594 137 0.980 0.000 C13 N1 H13A H16A 1.3306 0.3393 0.5860 137 0.980 0.000 C16 N2 H16A H16B 1.2823 0.1852 0.5915 137 0.980 0.000 C16 N2 H16A H16C 1.3691 0.2445 0.6253 137 0.980 0.000 C16 N2 H16A H11A 0.8295 0.2097 0.6507 23 0.990 0.000 C11 C1 N1 H11B 0.9157 0.3348 0.6527 23 0.990 0.000 C11 C1 N1 H14A 1.0834 0.1950 0.7344 137 0.980 0.000 C14 N1 H14A H14B 1.0637 0.3314 0.7060 137 0.980 0.000 C14 N1 H14A H14C 1.1075 0.1912 0.6842 137 0.980 0.000 C14 N1 H14A ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 1.1306 0.1583 0.5364 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.9979 -0.0433 0.5390 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.9286 0.2970 0.4750 43 0.950 0.000 C9 C10 C8 H17A 1.3121 0.4124 0.6777 137 0.980 0.000 C17 N2 H17A H17B 1.1967 0.4888 0.6709 137 0.980 0.000 C17 N2 H17A H17C 1.2933 0.5102 0.6369 137 0.980 0.000 C17 N2 H17A ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.8015 0.4327 0.5889 43 0.950 0.000 C7 C6 C8 S93 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq I1 0.91204 0.63773 0.67134 1.00000 0.02422 0.02362 0.02943 -0.00462 0.00088 0.00067 0.02576 0.00036 0.00002 0.00002 0.00001 0.00000 0.00012 0.00013 0.00013 0.00009 0.00009 0.00009 0.00008 Fe1 0.92011 0.21641 0.55802 1.00000 0.01836 0.01963 0.01959 -0.00075 -0.00080 0.00140 0.01919 0.00075 0.00003 0.00005 0.00001 0.00000 0.00022 0.00025 0.00024 0.00019 0.00019 0.00018 0.00012 N1 0.94412 0.18455 0.69834 1.00000 0.02064 0.02310 0.01947 0.00165 0.00007 0.00017 0.02107 0.00449 0.00020 0.00027 0.00009 0.00000 0.00131 0.00145 0.00148 0.00116 0.00111 0.00111 0.00059 N2 1.21854 0.32335 0.63219 1.00000 0.02328 0.03759 0.03052 0.00077 -0.00496 -0.00522 0.03046 0.00471 0.00021 0.00030 0.00009 0.00000 0.00141 0.00174 0.00173 0.00138 0.00127 0.00125 0.00069 C15 1.12267 0.35851 0.60550 1.00000 0.02503 0.02800 0.02854 -0.00001 0.00091 0.00021 0.02719 0.00567 0.00026 0.00034 0.00011 0.00000 0.00163 0.00188 0.00197 0.00150 0.00147 0.00146 0.00076 H15A 1.14776 0.40510 0.57904 1.00000 0.03263 0.00000 0.00000 H15B 1.07467 0.42423 0.62115 1.00000 0.03263 0.00000 0.00000 C5 0.93678 0.04511 0.59604 1.00000 0.02118 0.01775 0.02483 0.00015 -0.00601 0.00131 0.02126 0.00529 0.00024 0.00032 0.00011 0.00000 0.00150 0.00161 0.00177 0.00138 0.00141 0.00128 0.00068 H5 0.88020 -0.01661 0.60486 1.00000 0.02551 0.00000 0.00000 C8 0.89311 0.40811 0.53193 1.00000 0.03029 0.02318 0.03193 0.00633 -0.00172 0.00086 0.02846 0.00614 0.00027 0.00035 0.00012 0.00000 0.00176 0.00181 0.00201 0.00152 0.00155 0.00145 0.00079 H8 0.94290 0.48430 0.53187 1.00000 0.03416 0.00000 0.00000 C6 0.75675 0.25715 0.55172 1.00000 0.01805 0.03893 0.03247 0.01059 -0.00372 0.00387 0.02982 0.00599 0.00025 0.00036 0.00011 0.00000 0.00154 0.00208 0.00200 0.00167 0.00153 0.00150 0.00080 H6 0.69888 0.21427 0.56722 1.00000 0.03578 0.00000 0.00000 C12 0.93441 0.02996 0.70240 1.00000 0.04587 0.02152 0.03008 0.00629 0.00010 0.00207 0.03249 0.00620 0.00029 0.00034 0.00012 0.00000 0.00205 0.00183 0.00205 0.00151 0.00170 0.00161 0.00083 H12A 0.98210 -0.01507 0.68132 1.00000 0.04874 0.00000 0.00000 H12B 0.85817 0.00199 0.69737 1.00000 0.04874 0.00000 0.00000 H12C 0.95659 0.00148 0.73118 1.00000 0.04874 0.00000 0.00000 C10 0.80090 0.21013 0.51252 1.00000 0.02942 0.03090 0.02636 0.00296 -0.01125 0.00131 0.02889 0.00591 0.00026 0.00036 0.00011 0.00000 0.00173 0.00202 0.00194 0.00157 0.00153 0.00149 0.00079 H10 0.77800 0.12986 0.49715 1.00000 0.03467 0.00000 0.00000 C13 0.87099 0.25282 0.73064 1.00000 0.02559 0.03897 0.02203 -0.00335 0.00488 -0.00006 0.02886 0.00591 0.00025 0.00037 0.00011 0.00000 0.00165 0.00205 0.00184 0.00157 0.00148 0.00157 0.00078 H13A 0.79532 0.22116 0.72642 1.00000 0.04329 0.00000 0.00000 H13B 0.87446 0.35426 0.72717 1.00000 0.04329 0.00000 0.00000 H13C 0.89538 0.22767 0.75944 1.00000 0.04329 0.00000 0.00000 C16 1.30726 0.26868 0.60668 1.00000 0.02031 0.05821 0.04147 0.00355 0.00207 -0.00627 0.04000 0.00668 0.00026 0.00043 0.00013 0.00000 0.00167 0.00266 0.00247 0.00200 0.00164 0.00170 0.00098 H16A 1.33065 0.33926 0.58597 1.00000 0.05999 0.00000 0.00000 H16B 1.28231 0.18519 0.59148 1.00000 0.05999 0.00000 0.00000 H16C 1.36907 0.24445 0.62526 1.00000 0.05999 0.00000 0.00000 C11 0.90823 0.23215 0.65423 1.00000 0.02130 0.02472 0.01796 0.00072 -0.00101 0.00200 0.02133 0.00547 0.00023 0.00034 0.00010 0.00000 0.00153 0.00179 0.00163 0.00137 0.00134 0.00136 0.00069 H11A 0.82948 0.20970 0.65068 1.00000 0.02559 0.00000 0.00000 H11B 0.91569 0.33480 0.65272 1.00000 0.02559 0.00000 0.00000 C2 1.05862 0.22995 0.59414 1.00000 0.01783 0.02149 0.02067 0.00116 -0.00112 0.00053 0.02000 0.00527 0.00023 0.00032 0.00010 0.00000 0.00145 0.00167 0.00170 0.00137 0.00133 0.00127 0.00067 C14 1.05961 0.22940 0.70645 1.00000 0.02208 0.04826 0.02142 -0.00145 -0.00062 -0.00261 0.03059 0.00582 0.00024 0.00040 0.00011 0.00000 0.00160 0.00234 0.00188 0.00165 0.00142 0.00157 0.00082 H14A 1.08336 0.19498 0.73443 1.00000 0.04588 0.00000 0.00000 H14B 1.06370 0.33143 0.70604 1.00000 0.04588 0.00000 0.00000 H14C 1.10754 0.19123 0.68422 1.00000 0.04588 0.00000 0.00000 C1 0.96999 0.16975 0.61775 1.00000 0.01708 0.01831 0.01662 -0.00191 -0.00204 0.00183 0.01733 0.00509 0.00023 0.00030 0.00010 0.00000 0.00144 0.00160 0.00169 0.00130 0.00126 0.00124 0.00065 C3 1.07702 0.14287 0.55794 1.00000 0.02035 0.02841 0.02122 0.00106 0.00066 0.00458 0.02332 0.00546 0.00024 0.00033 0.00011 0.00000 0.00155 0.00186 0.00174 0.00143 0.00134 0.00140 0.00072 H3 1.13056 0.15828 0.53641 1.00000 0.02799 0.00000 0.00000 C4 1.00271 0.03001 0.55931 1.00000 0.02806 0.02279 0.02180 -0.00743 -0.00467 0.00886 0.02422 0.00549 0.00025 0.00033 0.00011 0.00000 0.00169 0.00178 0.00177 0.00142 0.00142 0.00143 0.00073 H4 0.99793 -0.04335 0.53901 1.00000 0.02906 0.00000 0.00000 C9 0.88518 0.30344 0.50014 1.00000 0.03123 0.03171 0.02521 0.00702 -0.00219 0.00234 0.02938 0.00594 0.00027 0.00035 0.00011 0.00000 0.00180 0.00196 0.00195 0.00157 0.00150 0.00151 0.00080 H9 0.92860 0.29702 0.47502 1.00000 0.03526 0.00000 0.00000 C17 1.25847 0.44365 0.65644 1.00000 0.03682 0.04306 0.04557 0.00045 -0.00863 -0.01862 0.04182 0.00603 0.00030 0.00040 0.00013 0.00000 0.00202 0.00232 0.00248 0.00192 0.00191 0.00185 0.00098 H17A 1.31214 0.41244 0.67769 1.00000 0.06273 0.00000 0.00000 H17B 1.19672 0.48883 0.67093 1.00000 0.06273 0.00000 0.00000 H17C 1.29328 0.51016 0.63693 1.00000 0.06273 0.00000 0.00000 C7 0.81402 0.37938 0.56378 1.00000 0.02692 0.02654 0.03126 0.00368 0.00073 0.01159 0.02824 0.00616 0.00025 0.00034 0.00012 0.00000 0.00173 0.00191 0.00204 0.00157 0.00154 0.00146 0.00080 H7 0.80152 0.43274 0.58886 1.00000 0.03389 0.00000 0.00000 Final Structure Factor Calculation for S93 in Pbca Total number of l.s. parameters = 195 Maximum vector length = 511 Memory required = 3022 / 24017 wR2 = 0.0607 before cycle 13 for 3191 data and 0 / 195 parameters GooF = S = 1.147; Restrained GooF = 1.147 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0141 * P )^2 + 4.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0291 for 2800 Fo > 4sig(Fo) and 0.0363 for all 3191 data wR2 = 0.0607, GooF = S = 1.147, Restrained GooF = 1.147 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0320 0.0245 0.0208 I1 0.0212 0.0189 0.0174 Fe1 0.0237 0.0206 0.0188 N1 0.0399 0.0318 0.0197 N2 0.0288 0.0280 0.0248 C15 0.0293 0.0185 0.0160 C5 0.0355 0.0303 0.0196 C8 0.0468 0.0276 0.0151 C6 0.0461 0.0333 0.0181 C12 0.0394 0.0314 0.0159 C10 0.0397 0.0287 0.0183 C13 0.0598 0.0412 0.0190 C16 0.0257 0.0209 0.0174 C11 0.0223 0.0204 0.0173 C2 0.0486 0.0224 0.0208 C14 0.0213 0.0160 0.0148 C1 0.0306 0.0211 0.0183 C3 0.0387 0.0199 0.0140 C4 0.0363 0.0319 0.0199 C9 0.0612 0.0448 0.0195 C17 0.0395 0.0303 0.0149 C7 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.026 0.040 0.056 0.075 0.096 0.127 0.168 0.236 1.000 Number in group 329. 322. 321. 306. 320. 322. 313. 319. 324. 315. GooF 1.502 1.335 1.141 1.042 0.972 1.061 1.104 1.044 1.087 1.064 K 4.636 1.352 1.111 1.045 1.003 0.993 0.984 0.996 1.007 0.991 Resolution(A) 0.84 0.87 0.90 0.94 0.99 1.05 1.14 1.25 1.43 1.81 inf Number in group 328. 315. 319. 324. 317. 316. 323. 312. 320. 317. GooF 1.028 0.981 1.036 1.022 1.118 0.953 1.115 1.226 1.292 1.571 K 1.014 1.012 1.024 1.014 1.010 1.004 1.000 0.993 0.994 0.988 R1 0.074 0.065 0.056 0.045 0.045 0.035 0.029 0.028 0.021 0.021 Recommended weighting scheme: WGHT 0.0148 5.8680 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 8 7 0 557.39 4.83 4.36 0.004 1.02 5 7 2 192.66 3.37 4.30 0.003 1.19 2 2 0 3140.34 2546.49 3.92 0.095 3.77 4 9 1 257.15 3.88 3.89 0.004 1.01 7 6 2 181.22 29.74 3.84 0.010 1.17 5 5 11 172.09 48.17 3.83 0.013 1.33 7 1 2 305.45 143.89 3.74 0.023 1.70 5 4 3 123.05 24.72 3.66 0.009 1.69 5 0 8 5401.27 4612.88 3.65 0.128 2.07 2 4 5 84.74 3.29 3.64 0.003 2.10 2 0 10 145.02 22.99 3.63 0.009 2.79 3 3 15 319.67 98.32 3.58 0.019 1.61 3 0 2 242793.77 271181.13 3.51 0.982 3.93 9 7 1 205.20 30.16 3.49 0.010 0.96 7 4 5 85.22 1.17 3.47 0.002 1.37 4 0 16 224.90 79.50 3.46 0.017 1.65 1 2 2 3895.03 3333.74 3.44 0.109 4.29 0 2 0 194590.47 222193.98 3.34 0.889 4.80 12 4 5 175.34 2.66 3.29 0.003 0.93 2 1 5 15397.56 14043.21 3.28 0.223 3.98 2 0 0 100389.50 117623.72 3.24 0.647 6.09 7 3 4 199.07 92.54 3.24 0.018 1.50 2 0 4 398.50 249.43 3.21 0.030 4.81 3 1 24 386.21 67.26 3.16 0.015 1.23 1 1 5 20678.65 19021.90 3.14 0.260 4.82 8 9 7 528.45 125.52 3.13 0.021 0.86 7 7 10 235.80 10.47 3.12 0.006 1.02 0 4 0 4790.61 5584.68 3.07 0.141 2.40 0 4 13 331.42 167.58 3.04 0.024 1.70 8 5 5 132.81 19.51 3.02 0.008 1.17 3 3 16 160.18 48.87 3.02 0.013 1.54 3 2 22 1307.14 1687.98 2.98 0.077 1.29 0 4 10 186.24 75.35 2.94 0.016 1.90 2 7 0 1677.75 1318.03 2.90 0.068 1.34 2 2 10 1612.25 1941.23 2.89 0.083 2.41 4 2 2 134.55 54.20 2.89 0.014 2.54 3 2 8 9115.13 8295.96 2.86 0.172 2.43 8 3 2 260.43 40.77 2.79 0.012 1.37 0 10 13 1576.31 995.58 2.78 0.059 0.89 1 7 8 114.79 9.16 2.75 0.006 1.29 1 1 6 30357.78 28357.35 2.75 0.318 4.29 1 2 14 100.44 12.96 2.74 0.007 2.00 9 2 23 13015.29 11736.81 2.73 0.204 0.94 3 4 5 1910.52 1610.63 2.71 0.076 1.96 12 3 5 846.16 620.66 2.71 0.047 0.96 3 3 13 645.10 468.63 2.69 0.041 1.74 3 1 14 2037.49 1668.18 2.68 0.077 1.92 7 2 1 4631.23 5173.84 2.64 0.136 1.63 4 4 17 206.94 104.00 2.63 0.019 1.32 12 1 0 213.52 88.58 2.61 0.018 1.01 Bond lengths and angles Fe1 - Distance Angles C1 2.0175 (0.0031) C2 2.0363 (0.0030) 41.34 (0.12) C10 2.0362 (0.0032) 149.04 (0.13) 169.21 (0.14) C6 2.0387 (0.0031) 115.25 (0.13) 148.35 (0.13) 40.62 (0.13) C3 2.0385 (0.0030) 69.01 (0.12) 40.97 (0.12) 131.17 (0.14) 169.27 (0.14) C5 2.0395 (0.0032) 41.39 (0.12) 69.17 (0.12) 117.13 (0.13) 107.96 (0.13) 68.19 (0.12) C7 2.0367 (0.0031) 106.23 (0.13) 115.36 (0.14) 68.38 (0.14) 40.66 (0.13) 149.47 (0.13) 129.05 (0.13) C8 2.0389 (0.0034) 128.34 (0.14) 107.40 (0.13) 68.34 (0.14) 68.33 (0.13) 117.58 (0.13) 167.61 (0.14) 40.61 (0.13) C9 2.0410 (0.0034) 167.80 (0.13) 129.82 (0.13) 40.66 (0.13) 68.40 (0.13) 109.64 (0.14) 150.35 (0.14) 68.42 (0.14) C4 2.0524 (0.0030) 68.95 (0.12) 68.78 (0.12) 109.75 (0.13) 130.39 (0.14) 40.39 (0.12) 40.34 (0.12) 168.06 (0.13) Fe1 - C1 C2 C10 C6 C3 C5 C7 N1 - Distance Angles C12 1.4931 (0.0041) C14 1.4936 (0.0038) 110.26 (0.26) C13 1.4988 (0.0040) 109.23 (0.25) 108.65 (0.25) C11 1.5197 (0.0039) 110.67 (0.25) 109.84 (0.24) 108.13 (0.24) N1 - C12 C14 C13 N2 - Distance Angles C16 1.4432 (0.0044) C17 1.4648 (0.0045) 108.93 (0.28) C15 1.4758 (0.0041) 111.26 (0.29) 112.14 (0.28) N2 - C16 C17 C15 - Distance Angles N2 1.4758 (0.0041) C2 1.5023 (0.0044) 110.98 (0.27) H15A 0.9900 109.44 109.44 H15B 0.9900 109.44 109.44 108.04 C15 - N2 C2 H15A C5 - Distance Angles C4 1.4109 (0.0044) C1 1.4338 (0.0043) 108.16 (0.27) Fe1 2.0395 (0.0032) 70.32 (0.18) 68.49 (0.17) H5 0.9500 125.92 125.92 126.84 C5 - C4 C1 Fe1 C8 - Distance Angles C9 1.4175 (0.0050) C7 1.4142 (0.0047) 108.13 (0.31) Fe1 2.0389 (0.0033) 69.75 (0.19) 69.61 (0.19) H8 0.9500 125.94 125.94 126.27 C8 - C9 C7 Fe1 C6 - Distance Angles C10 1.4144 (0.0048) C7 1.4159 (0.0048) 107.94 (0.30) Fe1 2.0387 (0.0030) 69.59 (0.18) 69.59 (0.18) H6 0.9500 126.03 126.03 126.35 C6 - C10 C7 Fe1 C12 - Distance Angles N1 1.4931 (0.0041) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - N1 H12A H12B C10 - Distance Angles C6 1.4144 (0.0048) C9 1.4166 (0.0047) 108.19 (0.31) Fe1 2.0362 (0.0032) 69.79 (0.19) 69.85 (0.19) H10 0.9500 125.90 125.90 126.04 C10 - C6 C9 Fe1 C13 - Distance Angles N1 1.4988 (0.0040) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - N1 H13A H13B C16 - Distance Angles N2 1.4432 (0.0044) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - N2 H16A H16B C11 - Distance Angles C1 1.4933 (0.0042) N1 1.5197 (0.0039) 115.48 (0.24) H11A 0.9900 108.41 108.41 H11B 0.9900 108.41 108.41 107.46 C11 - C1 N1 H11A C2 - Distance Angles C3 1.4262 (0.0044) C1 1.4309 (0.0042) 107.06 (0.27) C15 1.5023 (0.0044) 125.96 (0.28) 126.96 (0.29) Fe1 2.0363 (0.0029) 69.60 (0.17) 68.63 (0.17) 127.93 (0.22) C2 - C3 C1 C15 C14 - Distance Angles N1 1.4936 (0.0038) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - N1 H14A H14B C1 - Distance Angles C2 1.4309 (0.0042) C5 1.4338 (0.0043) 107.72 (0.28) C11 1.4933 (0.0042) 127.90 (0.28) 123.70 (0.27) Fe1 2.0175 (0.0031) 70.04 (0.18) 70.13 (0.18) 117.95 (0.20) C1 - C2 C5 C11 C3 - Distance Angles C4 1.4122 (0.0044) C2 1.4262 (0.0044) 108.90 (0.27) Fe1 2.0385 (0.0029) 70.33 (0.17) 69.43 (0.17) H3 0.9500 125.55 125.55 126.27 C3 - C4 C2 Fe1 C4 - Distance Angles C5 1.4109 (0.0044) C3 1.4122 (0.0044) 108.14 (0.28) Fe1 2.0524 (0.0030) 69.34 (0.17) 69.28 (0.17) H4 0.9500 125.93 125.93 127.02 C4 - C5 C3 Fe1 C9 - Distance Angles C10 1.4166 (0.0047) C8 1.4175 (0.0050) 107.73 (0.32) Fe1 2.0410 (0.0034) 69.49 (0.19) 69.59 (0.20) H9 0.9500 126.14 126.14 126.36 C9 - C10 C8 Fe1 C17 - Distance Angles N2 1.4648 (0.0045) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - N2 H17A H17B C7 - Distance Angles C6 1.4159 (0.0048) C8 1.4142 (0.0048) 108.02 (0.32) Fe1 2.0367 (0.0031) 69.75 (0.18) 69.78 (0.18) H7 0.9500 125.99 125.99 126.06 C7 - C6 C8 Fe1 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 24 -2 2.500 1 2 R1 = 0.0353 for 3191 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.61 at 0.7625 0.0431 0.3083 [ 0.86 A from H17A ] Deepest hole -0.42 at 0.5841 0.1231 0.6228 [ 1.53 A from I1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3730 / 30359 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2625 0.4569 0.6917 1.00000 0.05 0.61 0.86 H17A 1.08 H17B 1.11 C17 1.83 H17C Q2 1 0.9791 0.6655 0.6524 1.00000 0.05 0.32 1.04 I1 2.17 H16C 2.77 H15B 3.13 C16 Q3 1 1.3569 0.3919 0.6470 1.00000 0.05 0.31 1.12 H17A 1.33 C17 1.41 H17C 1.58 H16C Q4 1 1.2812 0.3734 0.6118 1.00000 0.05 0.29 1.06 H16A 1.07 C16 1.11 N2 1.54 H17C Q5 1 1.1848 0.5261 0.7283 1.00000 0.05 0.28 1.84 H17B 2.15 H12C 2.20 H13C 2.36 H13A Q6 1 0.7662 0.3455 0.5451 1.00000 0.05 0.28 0.88 C6 0.89 C7 1.65 H6 1.66 H7 Q7 1 1.2474 0.4800 0.7166 1.00000 0.05 0.27 1.56 H17B 1.59 H17A 1.92 C17 2.57 H17C Q8 1 0.8038 0.0032 0.6871 1.00000 0.05 0.27 0.74 H12B 1.68 C12 2.19 H12A 2.31 H11A Q9 1 1.2592 0.5466 0.6423 1.00000 0.05 0.26 0.57 H17C 1.08 C17 1.30 H17B 1.82 H17A Q10 1 0.8588 0.3912 0.5102 1.00000 0.05 0.25 0.81 C8 0.95 C9 1.52 H8 1.66 H9 Shortest distances between peaks (including symmetry equivalents) 1 7 0.83 5 7 0.95 3 4 1.45 1 5 1.63 6 10 1.63 1 9 1.77 3 9 1.91 1 3 1.92 4 9 1.93 7 9 2.42 1 4 2.64 5 8 2.66 3 7 2.69 5 9 2.85 2 3 2.96 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.83: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.31: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.81: Structure factors and derivatives 2.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 14:54:16 Total CPU time: 6.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++