+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0424 started at 13:53:51 on 07-Sep-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0424 in C2/c CELL 0.71073 25.0178 8.8338 16.5583 90.000 97.264 90.000 ZERR 4.00 0.0010 0.0002 0.0006 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N NI I UNIT 160 112 32 4 8 V = 3630.05 F(000) = 1832.0 Mu = 2.28 mm-1 Cell Wt = 3732.86 Rho = 1.708 MERG 2 OMIT -3.00 55.00 EXTI 0.00026 FMAP 2 PLAN 5 SIZE 0.02 0.06 0.20 ACTA BOND $H WGHT 0.05100 28.74790 L.S. 6 TEMP -153.00 FVAR 0.22931 C1 1 0.861104 0.528552 0.362614 11.00000 0.01937 0.01993 = 0.01915 -0.00167 0.00615 -0.00129 C2 1 0.871890 0.392237 0.407496 11.00000 0.02526 0.02646 = 0.02506 -0.00348 0.00080 0.00010 C3 1 0.809530 0.470803 0.488429 11.00000 0.02517 0.02285 = 0.02394 -0.00211 -0.00037 0.00271 C4 1 0.883271 0.573986 0.287076 11.00000 0.02475 0.03515 = 0.02233 0.00613 0.00309 -0.00029 C5 1 0.886124 0.472367 0.221213 11.00000 0.02621 0.02843 = 0.03195 -0.00169 0.00164 0.00375 AFIX 43 H5 2 0.873734 0.371190 0.224609 11.00000 -1.20000 AFIX 0 C6 1 0.906461 0.519746 0.153801 11.00000 0.03464 0.04890 = 0.03066 -0.00299 0.00160 0.00684 AFIX 43 H6 2 0.907870 0.451408 0.109821 11.00000 -1.20000 AFIX 0 C7 1 0.925640 0.668828 0.147523 11.00000 0.03875 0.05392 = 0.03396 0.00951 0.01044 0.00051 AFIX 43 H7 2 0.940306 0.700988 0.100184 11.00000 -1.20000 AFIX 0 C8 1 0.922702 0.765357 0.210527 11.00000 0.03789 0.03985 = 0.03665 0.00527 0.01160 -0.01178 AFIX 43 H8 2 0.935616 0.865956 0.206939 11.00000 -1.20000 AFIX 0 C9 1 0.901303 0.720716 0.280038 11.00000 0.04013 0.03253 = 0.03122 -0.00088 0.00888 -0.00098 AFIX 43 H9 2 0.899033 0.791056 0.322869 11.00000 -1.20000 AFIX 0 C10 1 0.913020 0.277979 0.396470 11.00000 0.03530 0.03140 = 0.02442 -0.00233 0.00153 0.00691 C11 1 0.906845 0.131730 0.426291 11.00000 0.02920 0.02261 = 0.02362 -0.00345 0.00217 0.00531 AFIX 43 H11 2 0.875043 0.106554 0.449188 11.00000 -1.20000 AFIX 0 C12 1 0.945809 0.024715 0.422982 11.00000 0.05702 0.03926 = 0.03962 -0.00526 0.00550 0.01785 AFIX 43 H12 2 0.940684 -0.074285 0.443054 11.00000 -1.20000 AFIX 0 C13 1 0.992650 0.058912 0.390725 11.00000 0.05163 0.06144 = 0.05080 -0.00032 0.01618 0.03296 AFIX 43 H13 2 1.019715 -0.015911 0.388636 11.00000 -1.20000 AFIX 0 C14 1 0.999812 0.205014 0.361145 11.00000 0.04229 0.07025 = 0.04184 0.01318 0.01390 0.01598 AFIX 43 H14 2 1.031780 0.228617 0.338314 11.00000 -1.20000 AFIX 0 C15 1 0.961302 0.314602 0.364665 11.00000 0.03119 0.06519 = 0.02870 0.00231 0.01329 -0.00205 AFIX 43 H15 2 0.967010 0.414220 0.345906 11.00000 -1.20000 AFIX 0 C16 1 0.779762 0.443121 0.559876 11.00000 0.01763 0.01717 = 0.01859 -0.00251 0.00161 0.00254 C17 1 0.782759 0.308999 0.601974 11.00000 0.02720 0.01890 = 0.02853 -0.00206 -0.00075 0.00254 AFIX 43 H17 2 0.803510 0.227017 0.585652 11.00000 -1.20000 AFIX 0 C18 1 0.755138 0.295756 0.668187 11.00000 0.03675 0.02074 = 0.02998 0.00812 -0.00219 -0.00502 AFIX 43 H18 2 0.756518 0.204401 0.698651 11.00000 -1.20000 AFIX 0 C19 1 0.725235 0.417755 0.689834 11.00000 0.03342 0.03981 = 0.02118 0.00381 0.00969 -0.00867 AFIX 43 H19 2 0.705995 0.411579 0.735649 11.00000 -1.20000 AFIX 0 C20 1 0.723748 0.549988 0.643396 11.00000 0.02418 0.02443 = 0.02247 -0.00415 0.01099 0.00066 AFIX 43 H20 2 0.703055 0.633368 0.658179 11.00000 -1.20000 AFIX 0 N1 3 0.801557 0.604710 0.450315 11.00000 0.02499 0.02709 = 0.02570 -0.00388 0.00614 0.00264 N2 3 0.825941 0.629289 0.385579 11.00000 0.02760 0.02886 = 0.02640 -0.00332 0.00947 -0.00136 N3 3 0.843685 0.364671 0.469563 11.00000 0.02613 0.02447 = 0.02559 -0.00061 0.00689 0.00287 N4 3 0.750601 0.563015 0.578599 11.00000 0.01889 0.01566 = 0.01643 0.00179 0.00401 0.00241 I1 5 0.663050 0.618214 0.405454 11.00000 0.02821 0.02145 = 0.02466 0.00196 0.00337 0.00015 NI1 4 0.750000 0.750000 0.500000 10.50000 0.01982 0.01384 = 0.01526 0.00174 0.00742 0.00397 HKLF 4 Covalent radii and connectivity table for 2005slh0424 in C2/c C 0.770 H 0.320 N 0.700 NI 1.250 I 1.330 C1 - N2 C2 C4 C2 - N3 C1 C10 C3 - N3 N1 C16 C4 - C9 C5 C1 C5 - C6 C4 C6 - C5 C7 C7 - C8 C6 C8 - C7 C9 C9 - C4 C8 C10 - C11 C15 C2 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C15 C13 C15 - C14 C10 C16 - N4 C17 C3 C17 - C16 C18 C18 - C17 C19 C19 - C18 C20 C20 - N4 C19 N1 - N2 C3 Ni1 N2 - N1 C1 N3 - C3 C2 N4 - C20 C16 Ni1 I1 - Ni1 Ni1 - N1_$1 N1 N4 N4_$1 I1_$1 I1 Operators for generating equivalent atoms: $1 -x+3/2, -y+3/2, -z+1 21294 Reflections read, of which 700 rejected -32 =< h =< 32, -10 =< k =< 11, -21 =< l =< 18, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 4173 Unique reflections, of which 0 suppressed R(int) = 0.0459 R(sigma) = 0.0381 Friedel opposites merged Maximum memory for data reduction = 2235 / 49927 Special position constraints for Ni1 x = 0.7500 y = 0.7500 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 2864 / 289870 wR2 = 0.1101 before cycle 1 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 0.004 OSF 2 0.00026 0.00012 -0.004 EXTI Mean shift/esd = 0.002 Maximum = 0.023 for U13 I1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C19 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2864 / 289870 wR2 = 0.1101 before cycle 2 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 -0.004 OSF 2 0.00026 0.00012 -0.003 EXTI Mean shift/esd = 0.001 Maximum = 0.008 for U13 I1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2864 / 289870 wR2 = 0.1101 before cycle 3 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 0.000 OSF 2 0.00026 0.00012 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x I1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2864 / 289870 wR2 = 0.1101 before cycle 4 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 0.000 OSF 2 0.00026 0.00012 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x I1 Max. shift = 0.000 A for N4 Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2864 / 289870 wR2 = 0.1101 before cycle 5 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 0.000 OSF 2 0.00026 0.00012 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x I1 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2864 / 289870 wR2 = 0.1101 before cycle 6 for 4173 data and 233 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22931 0.00054 0.000 OSF 2 0.00026 0.00012 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x I1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C13 Largest correlation matrix elements 0.649 EXTI / OSF 0.624 U11 I1 / OSF 0.627 U33 I1 / OSF 0.624 U22 I1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5 0.8737 0.3712 0.2246 43 0.950 0.000 C5 C6 C4 H6 0.9079 0.4514 0.1098 43 0.950 0.000 C6 C5 C7 H7 0.9403 0.7010 0.1002 43 0.950 0.000 C7 C8 C6 H8 0.9356 0.8660 0.2069 43 0.950 0.000 C8 C7 C9 H9 0.8990 0.7911 0.3229 43 0.950 0.000 C9 C4 C8 H11 0.8750 0.1066 0.4492 43 0.950 0.000 C11 C12 C10 H12 0.9407 -0.0743 0.4431 43 0.950 0.000 C12 C11 C13 H13 1.0197 -0.0159 0.3886 43 0.950 0.000 C13 C12 C14 H14 1.0318 0.2286 0.3383 43 0.950 0.000 C14 C15 C13 H15 0.9670 0.4142 0.3459 43 0.950 0.000 C15 C14 C10 H17 0.8035 0.2270 0.5857 43 0.950 0.000 C17 C16 C18 H18 0.7565 0.2044 0.6987 43 0.950 0.000 C18 C17 C19 H19 0.7060 0.4116 0.7356 43 0.950 0.000 C19 C18 C20 H20 0.7031 0.6334 0.6582 43 0.950 0.000 C20 N4 C19 2005slh0424 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86110 0.52855 0.36261 1.00000 0.01937 0.01993 0.01915 -0.00167 0.00615 -0.00129 0.01916 0.00709 0.00016 0.00045 0.00024 0.00000 0.00182 0.00193 0.00188 0.00151 0.00150 0.00148 0.00078 C2 0.87189 0.39224 0.40750 1.00000 0.02526 0.02646 0.02506 -0.00348 0.00080 0.00010 0.02580 0.00779 0.00018 0.00049 0.00028 0.00000 0.00212 0.00229 0.00221 0.00169 0.00174 0.00167 0.00091 C3 0.80953 0.47080 0.48843 1.00000 0.02517 0.02285 0.02394 -0.00211 -0.00037 0.00271 0.02428 0.00760 0.00017 0.00048 0.00026 0.00000 0.00205 0.00209 0.00207 0.00164 0.00166 0.00161 0.00086 C4 0.88327 0.57399 0.28708 1.00000 0.02475 0.03515 0.02233 0.00613 0.00308 -0.00029 0.02740 0.00848 0.00018 0.00055 0.00027 0.00000 0.00211 0.00242 0.00212 0.00181 0.00172 0.00182 0.00092 C5 0.88612 0.47237 0.22121 1.00000 0.02621 0.02843 0.03195 -0.00169 0.00164 0.00375 0.02904 0.00838 0.00018 0.00054 0.00028 0.00000 0.00215 0.00233 0.00237 0.00186 0.00183 0.00177 0.00095 H5 0.87373 0.37119 0.22461 1.00000 0.03485 0.00000 0.00000 C6 0.90646 0.51975 0.15380 1.00000 0.03463 0.04889 0.03066 -0.00299 0.00159 0.00684 0.03828 0.00969 0.00020 0.00065 0.00031 0.00000 0.00255 0.00315 0.00251 0.00223 0.00205 0.00226 0.00115 H6 0.90787 0.45141 0.10982 1.00000 0.04594 0.00000 0.00000 C7 0.92564 0.66883 0.14752 1.00000 0.03875 0.05392 0.03396 0.00951 0.01044 0.00051 0.04171 0.01062 0.00022 0.00068 0.00033 0.00000 0.00278 0.00333 0.00275 0.00243 0.00224 0.00248 0.00122 H7 0.94031 0.70099 0.10018 1.00000 0.05005 0.00000 0.00000 C8 0.92270 0.76536 0.21053 1.00000 0.03789 0.03985 0.03664 0.00527 0.01160 -0.01178 0.03754 0.00955 0.00021 0.00062 0.00032 0.00000 0.00267 0.00284 0.00272 0.00216 0.00221 0.00217 0.00115 H8 0.93562 0.86596 0.20694 1.00000 0.04504 0.00000 0.00000 C9 0.90130 0.72072 0.28004 1.00000 0.04013 0.03252 0.03122 -0.00087 0.00888 -0.00098 0.03425 0.00927 0.00020 0.00057 0.00031 0.00000 0.00267 0.00255 0.00248 0.00198 0.00210 0.00206 0.00106 H9 0.89903 0.79106 0.32287 1.00000 0.04110 0.00000 0.00000 C10 0.91302 0.27798 0.39647 1.00000 0.03530 0.03140 0.02442 -0.00233 0.00153 0.00691 0.03057 0.00861 0.00019 0.00054 0.00028 0.00000 0.00248 0.00244 0.00224 0.00183 0.00191 0.00193 0.00099 C11 0.90685 0.13173 0.42629 1.00000 0.02920 0.02260 0.02362 -0.00345 0.00217 0.00531 0.02524 0.00784 0.00018 0.00047 0.00027 0.00000 0.00221 0.00216 0.00214 0.00163 0.00175 0.00167 0.00089 H11 0.87504 0.10655 0.44919 1.00000 0.03029 0.00000 0.00000 C12 0.94581 0.02472 0.42298 1.00000 0.05702 0.03926 0.03962 -0.00526 0.00550 0.01784 0.04535 0.01077 0.00024 0.00067 0.00034 0.00000 0.00346 0.00302 0.00293 0.00235 0.00257 0.00257 0.00134 H12 0.94068 -0.07428 0.44305 1.00000 0.05442 0.00000 0.00000 C13 0.99265 0.05891 0.39073 1.00000 0.05163 0.06143 0.05080 -0.00032 0.01618 0.03296 0.05379 0.01311 0.00026 0.00078 0.00038 0.00000 0.00351 0.00393 0.00349 0.00297 0.00283 0.00307 0.00161 H13 1.01971 -0.01591 0.38863 1.00000 0.06454 0.00000 0.00000 C14 0.99981 0.20501 0.36115 1.00000 0.04229 0.07025 0.04184 0.01319 0.01390 0.01598 0.05073 0.01256 0.00024 0.00078 0.00036 0.00000 0.00307 0.00421 0.00315 0.00291 0.00252 0.00286 0.00150 H14 1.03178 0.22862 0.33832 1.00000 0.06087 0.00000 0.00000 C15 0.96130 0.31460 0.36467 1.00000 0.03118 0.06518 0.02870 0.00231 0.01329 -0.00205 0.04088 0.01014 0.00020 0.00073 0.00030 0.00000 0.00253 0.00367 0.00253 0.00241 0.00208 0.00243 0.00124 H15 0.96701 0.41422 0.34591 1.00000 0.04905 0.00000 0.00000 C16 0.77976 0.44312 0.55988 1.00000 0.01763 0.01717 0.01859 -0.00251 0.00161 0.00254 0.01785 0.00690 0.00015 0.00044 0.00024 0.00000 0.00178 0.00188 0.00187 0.00146 0.00148 0.00140 0.00076 C17 0.78276 0.30900 0.60197 1.00000 0.02720 0.01890 0.02853 -0.00206 -0.00075 0.00254 0.02524 0.00768 0.00018 0.00048 0.00027 0.00000 0.00211 0.00205 0.00224 0.00166 0.00176 0.00162 0.00088 H17 0.80351 0.22702 0.58565 1.00000 0.03029 0.00000 0.00000 C18 0.75514 0.29576 0.66819 1.00000 0.03675 0.02074 0.02997 0.00812 -0.00219 -0.00502 0.02970 0.00822 0.00019 0.00051 0.00028 0.00000 0.00246 0.00217 0.00235 0.00177 0.00194 0.00180 0.00098 H18 0.75652 0.20440 0.69865 1.00000 0.03564 0.00000 0.00000 C19 0.72523 0.41776 0.68983 1.00000 0.03341 0.03981 0.02117 0.00381 0.00969 -0.00867 0.03093 0.00853 0.00019 0.00057 0.00028 0.00000 0.00242 0.00261 0.00217 0.00189 0.00186 0.00201 0.00100 H19 0.70600 0.41158 0.73565 1.00000 0.03712 0.00000 0.00000 C20 0.72375 0.54999 0.64340 1.00000 0.02418 0.02443 0.02247 -0.00415 0.01099 0.00066 0.02300 0.00762 0.00017 0.00049 0.00025 0.00000 0.00202 0.00216 0.00204 0.00163 0.00165 0.00159 0.00085 H20 0.70306 0.63337 0.65818 1.00000 0.02760 0.00000 0.00000 N1 0.80156 0.60471 0.45032 1.00000 0.02499 0.02709 0.02570 -0.00388 0.00613 0.00263 0.02567 0.00675 0.00015 0.00041 0.00023 0.00000 0.00182 0.00197 0.00191 0.00145 0.00150 0.00143 0.00078 N2 0.82594 0.62929 0.38558 1.00000 0.02760 0.02886 0.02640 -0.00333 0.00947 -0.00136 0.02710 0.00689 0.00015 0.00042 0.00024 0.00000 0.00189 0.00201 0.00194 0.00149 0.00156 0.00148 0.00080 N3 0.84369 0.36467 0.46956 1.00000 0.02613 0.02447 0.02559 -0.00061 0.00690 0.00287 0.02508 0.00677 0.00015 0.00041 0.00023 0.00000 0.00184 0.00188 0.00189 0.00143 0.00151 0.00142 0.00077 N4 0.75060 0.56301 0.57860 1.00000 0.01888 0.01566 0.01643 0.00179 0.00401 0.00240 0.01684 0.00595 0.00013 0.00037 0.00019 0.00000 0.00156 0.00156 0.00156 0.00124 0.00125 0.00123 0.00064 I1 0.66305 0.61821 0.40545 1.00000 0.02821 0.02145 0.02466 0.00196 0.00337 0.00015 0.02477 0.00049 0.00001 0.00003 0.00002 0.00000 0.00018 0.00018 0.00018 0.00010 0.00011 0.00010 0.00013 Ni1 0.75000 0.75000 0.50000 0.50000 0.01982 0.01384 0.01526 0.00174 0.00742 0.00397 0.01586 0.00000 0.00000 0.00000 0.00000 0.00000 0.00034 0.00034 0.00034 0.00025 0.00027 0.00025 0.00017 Final Structure Factor Calculation for 2005slh0424 in C2/c Total number of l.s. parameters = 233 Maximum vector length = 511 Memory required = 2631 / 24017 wR2 = 0.1101 before cycle 7 for 4173 data and 0 / 233 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0510 * P )^2 + 28.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0416 for 3603 Fo > 4sig(Fo) and 0.0508 for all 4173 data wR2 = 0.1101, GooF = S = 1.042, Restrained GooF = 1.042 for all data Occupancy sum of asymmetric unit = 25.50 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0236 0.0189 0.0150 C1 0.0302 0.0256 0.0216 C2 0.0304 0.0214 0.0210 C3 0.0377 0.0247 0.0198 C4 0.0347 0.0290 0.0234 C5 0.0527 0.0325 0.0297 C6 0.0579 0.0406 0.0267 C7 0.0507 0.0414 0.0205 C8 0.0416 0.0324 0.0288 C9 0.0416 0.0264 0.0236 C10 0.0334 0.0243 0.0180 C11 0.0691 0.0411 0.0259 C12 0.0901 0.0518 0.0195 C13 0.0820 0.0381 0.0320 C14 0.0654 0.0385 0.0187 C15 0.0220 0.0175 0.0141 C16 0.0336 0.0241 0.0180 C17 0.0451 0.0282 0.0158 C18 0.0459 0.0318 0.0151 C19 0.0313 0.0249 0.0128 C20 0.0304 0.0276 0.0190 N1 0.0342 0.0274 0.0197 N2 0.0297 0.0255 0.0201 N3 0.0211 0.0153 0.0141 N4 0.0282 0.0256 0.0205 I1 0.0242 0.0127 0.0107 Ni1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.051 0.076 0.104 0.129 0.164 0.204 0.260 0.353 1.000 Number in group 433. 411. 413. 423. 405. 417. 423. 411. 417. 420. GooF 0.962 1.071 1.038 1.234 1.022 0.964 1.044 1.001 1.061 0.999 K 1.583 1.025 0.954 0.988 0.972 0.999 0.997 1.018 1.015 1.007 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 429. 407. 430. 403. 416. 421. 418. 414. 417. 418. GooF 0.953 0.956 0.900 0.944 0.888 0.885 0.965 1.019 0.970 1.690 K 0.974 1.007 1.011 1.015 1.017 1.028 1.022 1.021 1.005 0.995 R1 0.113 0.091 0.074 0.062 0.051 0.043 0.040 0.034 0.030 0.039 Recommended weighting scheme: WGHT 0.0511 28.7436 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 0 2 13572.30 25136.61 6.64 0.371 6.48 -5 1 1 3725.67 1768.30 6.20 0.099 4.30 4 0 2 14039.51 20530.44 5.20 0.336 4.67 3 1 1 29068.04 21230.08 5.00 0.341 5.51 -6 4 1 3178.83 1673.58 4.99 0.096 1.95 -5 3 3 744.16 1844.22 4.86 0.101 2.36 -12 0 4 3136.97 5538.74 4.83 0.174 1.95 0 2 5 2347.65 1227.51 4.63 0.082 2.64 9 1 5 8020.19 5510.03 4.48 0.174 1.94 6 2 4 11255.43 8071.14 4.44 0.210 2.33 -10 0 6 3151.00 1646.34 4.34 0.095 1.97 -7 9 5 4177.58 7013.64 4.19 0.196 0.92 -3 3 5 12020.67 8834.03 4.12 0.220 2.17 -9 1 5 1854.76 3187.95 4.01 0.132 2.19 10 2 2 253.02 10.41 3.69 0.008 2.04 -2 4 3 7192.19 5201.91 3.69 0.169 2.04 7 3 3 21287.38 27033.60 3.64 0.385 2.04 0 2 0 262.40 855.43 3.57 0.069 4.42 5 1 3 150469.27 124126.86 3.54 0.825 3.23 1 1 4 7183.49 5303.59 3.50 0.171 3.62 -14 2 2 704.70 253.50 3.42 0.037 1.65 -8 4 1 715.05 294.80 3.37 0.040 1.80 -4 4 2 880.90 1637.06 3.37 0.095 2.04 -2 8 15 -360.03 1515.20 3.36 0.091 0.78 10 2 5 3039.47 4421.96 3.36 0.156 1.72 5 5 6 324.31 70.04 3.35 0.020 1.40 8 2 5 12438.31 15822.31 3.32 0.295 1.92 -20 4 3 433.35 20.88 3.27 0.011 1.08 -1 1 6 4733.65 6428.72 3.22 0.188 2.63 20 0 0 3541.81 2228.12 3.20 0.111 1.24 -18 4 5 1350.73 662.15 3.17 0.060 1.14 2 2 7 14534.28 18550.96 3.17 0.319 2.01 9 3 1 2784.93 1888.82 3.14 0.102 1.98 10 2 4 17472.00 14178.33 3.11 0.279 1.83 9 3 2 628.94 268.15 3.10 0.038 1.91 2 2 2 8934.25 7020.15 3.01 0.196 3.65 9 1 4 4641.18 6171.30 3.00 0.184 2.10 -19 7 13 249.14 1066.78 2.96 0.077 0.77 -30 2 7 161.12 775.27 2.94 0.065 0.80 1 1 5 7282.46 9266.26 2.89 0.226 3.01 8 2 4 15802.07 12942.43 2.89 0.267 2.07 -3 11 4 -329.96 557.18 2.89 0.055 0.79 -6 4 11 1143.88 1926.68 2.86 0.103 1.22 20 4 9 440.11 993.26 2.83 0.074 0.89 -4 2 9 712.19 332.70 2.82 0.043 1.68 -14 2 20 -19.32 412.28 2.81 0.048 0.77 -3 1 9 7905.20 9959.29 2.81 0.234 1.79 -7 1 6 7206.60 5641.07 2.80 0.176 2.24 2 4 0 11392.41 14082.63 2.79 0.278 2.17 -6 4 3 12983.64 10604.99 2.77 0.241 1.87 Bond lengths and angles C1 - Distance Angles N2 1.3398 (0.0053) C2 1.4228 (0.0059) 120.12 (0.37) C4 1.4861 (0.0058) 112.82 (0.37) 127.00 (0.38) C1 - N2 C2 C2 - Distance Angles N3 1.3404 (0.0059) C1 1.4228 (0.0059) 118.08 (0.38) C10 1.4691 (0.0062) 114.54 (0.39) 127.31 (0.41) C2 - N3 C1 C3 - Distance Angles N3 1.3320 (0.0054) N1 1.3437 (0.0057) 124.82 (0.41) C16 1.4956 (0.0058) 117.96 (0.37) 117.15 (0.36) C3 - N3 N1 C4 - Distance Angles C9 1.3822 (0.0068) C5 1.4213 (0.0066) 118.62 (0.42) C1 1.4861 (0.0058) 119.00 (0.42) 122.38 (0.42) C4 - C9 C5 C5 - Distance Angles C6 1.3504 (0.0071) C4 1.4213 (0.0066) 119.95 (0.46) H5 0.9500 120.03 120.03 C5 - C6 C4 C6 - Distance Angles C5 1.3504 (0.0070) C7 1.4100 (0.0082) 121.18 (0.49) H6 0.9500 119.41 119.41 C6 - C5 C7 C7 - Distance Angles C8 1.3566 (0.0079) C6 1.4100 (0.0082) 118.58 (0.48) H7 0.9500 120.71 120.71 C7 - C8 C6 C8 - Distance Angles C7 1.3566 (0.0079) C9 1.3866 (0.0069) 121.58 (0.50) H8 0.9500 119.21 119.21 C8 - C7 C9 C9 - Distance Angles C4 1.3822 (0.0068) C8 1.3866 (0.0069) 120.07 (0.47) H9 0.9500 119.96 119.96 C9 - C4 C8 C10 - Distance Angles C11 1.3986 (0.0065) C15 1.4149 (0.0068) 118.70 (0.46) C2 1.4691 (0.0062) 118.71 (0.43) 122.24 (0.46) C10 - C11 C15 C11 - Distance Angles C12 1.3640 (0.0066) C10 1.3986 (0.0065) 120.97 (0.48) H11 0.9500 119.51 119.51 C11 - C12 C10 C12 - Distance Angles C11 1.3640 (0.0066) C13 1.3813 (0.0089) 120.63 (0.56) H12 0.9500 119.68 119.68 C12 - C11 C13 C13 - Distance Angles C12 1.3813 (0.0089) C14 1.4000 (0.0097) 119.29 (0.52) H13 0.9500 120.35 120.35 C13 - C12 C14 C14 - Distance Angles C15 1.3722 (0.0081) C13 1.4000 (0.0097) 120.93 (0.55) H14 0.9500 119.54 119.54 C14 - C15 C13 C15 - Distance Angles C14 1.3722 (0.0081) C10 1.4149 (0.0068) 119.44 (0.55) H15 0.9500 120.28 120.28 C15 - C14 C10 C16 - Distance Angles N4 1.3443 (0.0049) C17 1.3719 (0.0060) 124.03 (0.38) C3 1.4956 (0.0058) 113.12 (0.34) 122.85 (0.37) C16 - N4 C17 C17 - Distance Angles C16 1.3719 (0.0060) C18 1.3729 (0.0067) 118.60 (0.40) H17 0.9500 120.70 120.70 C17 - C16 C18 C18 - Distance Angles C17 1.3729 (0.0067) C19 1.3847 (0.0071) 118.90 (0.40) H18 0.9500 120.55 120.55 C18 - C17 C19 C19 - Distance Angles C18 1.3847 (0.0070) C20 1.3964 (0.0064) 119.09 (0.41) H19 0.9500 120.46 120.46 C19 - C18 C20 C20 - Distance Angles N4 1.3409 (0.0051) C19 1.3964 (0.0064) 122.09 (0.39) H20 0.9500 118.96 118.96 C20 - N4 C19 N1 - Distance Angles N2 1.3167 (0.0053) C3 1.3437 (0.0057) 118.10 (0.36) Ni1 2.0630 (0.0036) 126.83 (0.29) 115.06 (0.29) N1 - N2 C3 N2 - Distance Angles N1 1.3167 (0.0053) C1 1.3398 (0.0053) 120.66 (0.37) N2 - N1 N3 - Distance Angles C3 1.3320 (0.0054) C2 1.3404 (0.0059) 117.87 (0.38) N3 - C3 N4 - Distance Angles C20 1.3409 (0.0051) C16 1.3443 (0.0049) 117.28 (0.34) Ni1 2.1018 (0.0032) 126.71 (0.27) 115.97 (0.26) N4 - C20 C16 I1 - Distance Angles Ni1 2.7707 (0.0003) I1 - Ni1 - Distance Angles N1_$1 2.0630 (0.0036) N1 2.0630 (0.0036) 180.00 (0.19) N4 2.1018 (0.0032) 101.41 (0.14) 78.59 (0.14) N4_$1 2.1018 (0.0032) 78.59 (0.14) 101.41 (0.14) 180.00 (0.00) I1_$1 2.7707 (0.0003) 89.95 (0.10) 90.05 (0.10) 92.10 (0.09) 87.90 (0.09) I1 2.7707 (0.0003) 90.05 (0.10) 89.95 (0.10) 87.90 (0.09) 92.10 (0.09) 180.00 (0.01) Ni1 - N1_$1 N1 N4 N4_$1 I1_$1 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -1 -2 1.389 1 2 R1 = 0.0502 for 4173 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.51 at 0.1561 0.7713 0.1969 [ 1.39 A from H9 ] Deepest hole -0.91 at 0.3675 0.6119 0.1006 [ 0.76 A from I1 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 3017 / 20979 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8439 0.7713 0.3031 1.00000 0.05 1.51 1.39 H9 1.60 C9 1.64 H20 1.95 N2 Q2 1 0.8337 0.5598 0.4280 1.00000 0.05 1.47 0.93 N2 1.01 N1 1.38 C1 1.46 C3 Q3 1 0.6888 0.7136 0.6372 1.00000 0.05 1.36 0.85 H20 1.47 N2 1.69 C20 2.20 N1 Q4 1 0.8043 0.6963 0.4161 1.00000 0.05 1.33 0.98 N2 1.00 N1 1.94 H20 2.12 NI1 Q5 1 0.9023 0.3953 0.3798 1.00000 0.05 1.32 0.94 C2 1.10 C10 1.57 C1 1.69 C15 Shortest distances between peaks (including symmetry equivalents) 3 4 1.22 1 3 1.37 2 4 1.41 2 3 2.31 1 4 2.32 2 5 2.46 1 2 2.82 Time profile in seconds ----------------------- 0.06: 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 0.00: 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 0.01: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.85: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.53: Structure factors and derivatives 5.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.47: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.10: Fourier summations 0.11: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0424 finished at 13:54:03 Total CPU time: 11.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++