+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0421 started at 10:50:30 on 08-Sep-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0421 in P-1 CELL 0.71073 9.2767 10.4672 15.0969 79.283 84.701 65.476 ZERR 1.00 0.0011 0.0024 0.0013 0.013 0.008 0.016 LATT 1 SFAC C H N O P S NI UNIT 56 48 8 4 2 4 1 V = 1310.23 F(000) = 594.0 Mu = 0.65 mm-1 Cell Wt = 1145.91 Rho = 1.452 MERG 2 OMIT -3.00 55.00 OMIT 0 0 3 OMIT 6 6 3 EXTI 0.00570 FMAP 2 PLAN 5 SIZE 0.02 0.04 0.12 ACTA BOND $H WGHT 0.03400 1.14550 L.S. 6 TEMP -153.00 FVAR 0.64580 C1 1 0.649498 0.975102 0.572057 11.00000 0.02877 0.01959 = 0.03672 -0.00133 -0.00497 -0.01098 AFIX 137 H1A 2 0.640482 0.992441 0.506326 11.00000 -1.50000 H1B 2 0.708349 1.025794 0.588888 11.00000 -1.50000 H1C 2 0.543352 1.009356 0.599820 11.00000 -1.50000 AFIX 0 C2 1 0.799202 0.566299 0.681950 11.00000 0.02096 0.01868 = 0.02084 -0.00609 -0.00205 -0.01084 C3 1 0.784763 0.519809 0.773863 11.00000 0.02354 0.02383 = 0.02172 -0.00771 0.00340 -0.00954 AFIX 43 H3 2 0.690171 0.568609 0.805650 11.00000 -1.20000 AFIX 0 C4 1 0.905800 0.404109 0.819147 11.00000 0.03310 0.02643 = 0.02098 -0.00345 -0.00206 -0.01117 AFIX 43 H4 2 0.893741 0.373260 0.881581 11.00000 -1.20000 AFIX 0 C5 1 1.045838 0.332249 0.773591 11.00000 0.02580 0.01801 = 0.03433 -0.00694 -0.00850 -0.00637 C6 1 1.065042 0.379231 0.682886 11.00000 0.02185 0.02498 = 0.03232 -0.01307 0.00164 -0.00924 AFIX 43 H6 2 1.161713 0.332729 0.652061 11.00000 -1.20000 AFIX 0 C7 1 0.941393 0.495105 0.637467 11.00000 0.02410 0.02625 = 0.02342 -0.00881 0.00276 -0.01372 AFIX 43 H7 2 0.953899 0.526324 0.575143 11.00000 -1.20000 AFIX 0 C8 1 1.306217 0.144446 0.781718 11.00000 0.03387 0.02998 = 0.06264 -0.00987 -0.01047 0.00187 AFIX 137 H8A 2 1.289864 0.108618 0.729652 11.00000 -1.50000 H8B 2 1.375086 0.064628 0.824779 11.00000 -1.50000 H8C 2 1.356096 0.211326 0.761566 11.00000 -1.50000 AFIX 0 C9 1 0.717191 0.452485 0.237330 11.00000 0.01749 0.02078 = 0.01766 -0.00597 0.00105 -0.01028 C10 1 0.852631 0.321469 0.258219 11.00000 0.02146 0.02224 = 0.02098 -0.00449 -0.00102 -0.01189 C11 1 0.785749 0.331772 0.406438 11.00000 0.01911 0.02048 = 0.02049 -0.00671 0.00172 -0.01080 C12 1 0.672296 0.536038 0.145602 11.00000 0.02573 0.02034 = 0.02028 -0.00592 -0.00018 -0.00964 C13 1 0.785434 0.552455 0.081284 11.00000 0.02697 0.02657 = 0.02449 -0.00774 0.00376 -0.01193 AFIX 43 H13 2 0.894686 0.508341 0.095681 11.00000 -1.20000 AFIX 0 C14 1 0.738169 0.632876 -0.003194 11.00000 0.03906 0.02862 = 0.02744 -0.00865 0.00761 -0.01331 AFIX 43 H14 2 0.815189 0.644310 -0.046186 11.00000 -1.20000 AFIX 0 C15 1 0.578612 0.696877 -0.025312 11.00000 0.04921 0.02851 = 0.01942 -0.00292 -0.00257 -0.00971 AFIX 43 H15 2 0.546766 0.750373 -0.083596 11.00000 -1.20000 AFIX 0 C16 1 0.467009 0.682171 0.037890 11.00000 0.02889 0.03557 = 0.02316 -0.00650 -0.00649 -0.00490 AFIX 43 H16 2 0.357888 0.726965 0.023204 11.00000 -1.20000 AFIX 0 C17 1 0.512760 0.602334 0.122966 11.00000 0.02738 0.03138 = 0.02356 -0.00880 0.00098 -0.01075 AFIX 43 H17 2 0.434729 0.592956 0.165906 11.00000 -1.20000 AFIX 0 C18 1 0.956895 0.235897 0.191209 11.00000 0.02300 0.02055 = 0.02075 -0.00384 0.00090 -0.00901 C19 1 1.119213 0.165078 0.206415 11.00000 0.02445 0.02460 = 0.02106 -0.00488 0.00088 -0.00907 AFIX 43 H19 2 1.162274 0.173561 0.258630 11.00000 -1.20000 AFIX 0 C20 1 1.218102 0.081984 0.145100 11.00000 0.02541 0.02881 = 0.03525 -0.00514 0.00541 -0.00673 AFIX 43 H20 2 1.328604 0.033513 0.155762 11.00000 -1.20000 AFIX 0 C21 1 1.156573 0.069509 0.068757 11.00000 0.04073 0.02768 = 0.02933 -0.01107 0.00987 -0.00769 AFIX 43 H21 2 1.224711 0.014153 0.026438 11.00000 -1.20000 AFIX 0 C22 1 0.994455 0.138411 0.054263 11.00000 0.04374 0.02907 = 0.02589 -0.01020 -0.00503 -0.00816 AFIX 43 H22 2 0.951858 0.128827 0.002243 11.00000 -1.20000 AFIX 0 C23 1 0.894580 0.220778 0.114841 11.00000 0.03121 0.02825 = 0.02709 -0.00667 -0.00749 -0.00987 AFIX 43 H23 2 0.783824 0.267014 0.104600 11.00000 -1.20000 AFIX 0 C24 1 0.273210 0.719276 0.350908 11.00000 0.02250 0.02206 = 0.01843 -0.00465 0.00056 -0.01058 AFIX 43 H24 2 0.355065 0.678562 0.308943 11.00000 -1.20000 AFIX 0 C25 1 0.133306 0.830503 0.318399 11.00000 0.02969 0.02191 = 0.01902 -0.00018 -0.00517 -0.01310 AFIX 43 H25 2 0.120866 0.864500 0.255486 11.00000 -1.20000 AFIX 0 C26 1 0.012218 0.891463 0.378168 11.00000 0.02318 0.01914 = 0.02795 -0.00202 -0.00636 -0.00695 AFIX 43 H26 2 -0.084522 0.967297 0.357307 11.00000 -1.20000 AFIX 0 C27 1 0.036300 0.838372 0.469887 11.00000 0.02121 0.02295 = 0.02428 -0.00798 0.00097 -0.00884 AFIX 43 H27 2 -0.044058 0.877388 0.512993 11.00000 -1.20000 AFIX 0 C28 1 0.179030 0.728040 0.497033 11.00000 0.02201 0.01864 = 0.01686 -0.00462 -0.00103 -0.01121 N1 3 0.648135 0.444899 0.388387 11.00000 0.02179 0.02068 = 0.01926 -0.00463 0.00086 -0.01152 N2 3 0.618611 0.509443 0.302992 11.00000 0.02346 0.02379 = 0.01761 -0.00472 -0.00063 -0.01159 N3 3 0.889301 0.266356 0.344556 11.00000 0.02124 0.02203 = 0.02006 -0.00610 0.00071 -0.01024 N4 3 0.297785 0.666847 0.438953 11.00000 0.01952 0.01786 = 0.01776 -0.00541 -0.00039 -0.00942 O1 4 0.732423 0.824472 0.603184 11.00000 0.02220 0.01996 = 0.02898 -0.00443 -0.00272 -0.01229 O2 4 1.156273 0.215860 0.824415 11.00000 0.03401 0.02609 = 0.04224 -0.00545 -0.01064 -0.00069 P1 5 0.641420 0.719385 0.621682 11.00000 0.01925 0.01887 = 0.01963 -0.00541 -0.00006 -0.00999 S1 6 0.615104 0.678325 0.500113 11.00000 0.02505 0.02295 = 0.01778 -0.00421 -0.00090 -0.01377 S2 6 0.450497 0.794816 0.697981 11.00000 0.02038 0.02442 = 0.02707 -0.00998 0.00336 -0.00930 NI1 7 0.500000 0.500000 0.500000 10.50000 0.01606 0.01712 = 0.01351 -0.00365 0.00011 -0.00652 HKLF 4 Covalent radii and connectivity table for 2005slh0421 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 NI 1.250 C1 - O1 C2 - C3 C7 P1 C3 - C4 C2 C4 - C3 C5 C5 - O2 C6 C4 C6 - C5 C7 C7 - C6 C2 C8 - O2 C9 - N2 C10 C12 C10 - N3 C9 C18 C11 - N3 N1 C28_$1 C12 - C17 C13 C9 C13 - C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - C16 C12 C18 - C19 C23 C10 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C23 C21 C23 - C22 C18 C24 - N4 C25 C25 - C26 C24 C26 - C25 C27 C27 - C28 C26 C28 - N4 C27 C11_$1 N1 - N2 C11 Ni1 N2 - C9 N1 N3 - C10 C11 N4 - C24 C28 Ni1 O1 - C1 P1 O2 - C5 C8 P1 - O1 C2 S2 S1 S1 - P1 Ni1 S2 - P1 Ni1 - N1 N1_$1 N4 N4_$1 S1 S1_$1 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+1 26223 Reflections read, of which 16 rejected -12 =< h =< 12, -13 =< k =< 13, -19 =< l =< 19, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 -2 8 0.83 0.28 4 2.22 1 Inconsistent equivalents 5955 Unique reflections, of which 0 suppressed R(int) = 0.0588 R(sigma) = 0.0535 Friedel opposites merged Maximum memory for data reduction = 3255 / 60399 Special position constraints for Ni1 x = 0.5000 y = 0.5000 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 = 4192 / 436289 wR2 = 0.0992 before cycle 1 for 5955 data and 343 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64562 0.00105 -0.169 OSF 2 0.00563 0.00115 -0.062 EXTI Mean shift/esd = 0.023 Maximum = -0.169 for OSF Max. shift = 0.001 A for H1C Max. dU = 0.000 for C28 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4192 / 436289 wR2 = 0.0992 before cycle 2 for 5955 data and 343 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64554 0.00105 -0.080 OSF 2 0.00560 0.00115 -0.028 EXTI Mean shift/esd = 0.008 Maximum = -0.080 for OSF Max. shift = 0.000 A for H1C Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4192 / 436289 wR2 = 0.0991 before cycle 3 for 5955 data and 343 / 343 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64554 0.00105 0.000 OSF 2 0.00559 0.00115 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U13 C5 Max. shift = 0.000 A for H1C Max. dU = 0.000 for C17 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4192 / 436289 wR2 = 0.0991 before cycle 4 for 5955 data and 343 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64554 0.00105 0.000 OSF 2 0.00559 0.00115 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for z S1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4192 / 436289 wR2 = 0.0991 before cycle 5 for 5955 data and 343 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64554 0.00105 0.001 OSF 2 0.00560 0.00115 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H8C Max. dU = 0.000 for C18 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4192 / 436289 wR2 = 0.0991 before cycle 6 for 5955 data and 343 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64554 0.00105 0.000 OSF 2 0.00560 0.00115 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for z S1 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C5 Largest correlation matrix elements -0.592 U12 S1 / U22 S1 -0.564 U12 O1 / U22 O1 -0.556 U12 C7 / U11 C7 0.582 EXTI / OSF -0.564 U12 C11 / U22 C11 -0.552 U12 P1 / U11 P1 -0.573 U12 S1 / U11 S1 -0.562 U12 N1 / U22 N1 -0.552 U12 C28 / U11 C28 -0.569 U12 C10 / U22 C10 -0.561 U12 O1 / U11 O1 -0.551 U12 C24 / U22 C24 -0.569 U12 C7 / U22 C7 -0.560 U12 C25 / U22 C25 -0.550 U12 S2 / U22 S2 -0.568 U12 C28 / U22 C28 -0.560 U12 Ni1 / U22 Ni1 -0.550 U12 C25 / U11 C25 -0.567 U12 P1 / U22 P1 -0.559 U12 C2 / U22 C2 -0.549 U12 N1 / U11 N1 -0.564 U12 C9 / U22 C9 -0.558 U12 C10 / U11 C10 -0.549 U12 C9 / U11 C9 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.6405 0.9925 0.5063 137 0.980 0.000 C1 O1 H1A H1B 0.7083 1.0258 0.5889 137 0.980 0.000 C1 O1 H1A H1C 0.5433 1.0094 0.5998 137 0.980 0.000 C1 O1 H1A H3 0.6902 0.5686 0.8056 43 0.950 0.000 C3 C4 C2 H4 0.8937 0.3733 0.8816 43 0.950 0.000 C4 C3 C5 H6 1.1617 0.3327 0.6521 43 0.950 0.000 C6 C5 C7 H7 0.9539 0.5263 0.5751 43 0.950 0.000 C7 C6 C2 H8A 1.2898 0.1086 0.7297 137 0.980 0.000 C8 O2 H8A H8B 1.3751 0.0646 0.8248 137 0.980 0.000 C8 O2 H8A H8C 1.3561 0.2113 0.7616 137 0.980 0.000 C8 O2 H8A H13 0.8947 0.5084 0.0957 43 0.950 0.000 C13 C14 C12 H14 0.8152 0.6443 -0.0462 43 0.950 0.000 C14 C13 C15 H15 0.5468 0.7504 -0.0836 43 0.950 0.000 C15 C16 C14 H16 0.3579 0.7270 0.0232 43 0.950 0.000 C16 C15 C17 H17 0.4347 0.5929 0.1659 43 0.950 0.000 C17 C16 C12 H19 1.1623 0.1736 0.2586 43 0.950 0.000 C19 C20 C18 H20 1.3286 0.0335 0.1558 43 0.950 0.000 C20 C21 C19 H21 1.2247 0.0142 0.0264 43 0.950 0.000 C21 C20 C22 H22 0.9519 0.1288 0.0022 43 0.950 0.000 C22 C23 C21 H23 0.7838 0.2670 0.1046 43 0.950 0.000 C23 C22 C18 H24 0.3551 0.6786 0.3089 43 0.950 0.000 C24 N4 C25 H25 0.1209 0.8645 0.2555 43 0.950 0.000 C25 C26 C24 H26 -0.0845 0.9673 0.3573 43 0.950 0.000 C26 C25 C27 H27 -0.0441 0.8774 0.5130 43 0.950 0.000 C27 C28 C26 2005slh0421 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.64949 0.97511 0.57205 1.00000 0.02875 0.01955 0.03667 -0.00128 -0.00501 -0.01097 0.02809 0.00360 0.00030 0.00025 0.00017 0.00000 0.00132 0.00122 0.00137 0.00102 0.00108 0.00106 0.00054 H1A 0.64055 0.99246 0.50631 1.00000 0.04213 0.00000 0.00000 H1B 0.70829 1.02581 0.58893 1.00000 0.04213 0.00000 0.00000 H1C 0.54331 1.00935 0.59977 1.00000 0.04213 0.00000 0.00000 C2 0.79919 0.56631 0.68195 1.00000 0.02094 0.01864 0.02077 -0.00606 -0.00206 -0.01085 0.01865 0.00298 0.00026 0.00023 0.00014 0.00000 0.00112 0.00111 0.00107 0.00088 0.00089 0.00094 0.00045 C3 0.78475 0.51982 0.77386 1.00000 0.02353 0.02380 0.02166 -0.00772 0.00339 -0.00955 0.02272 0.00327 0.00028 0.00025 0.00015 0.00000 0.00119 0.00121 0.00113 0.00094 0.00094 0.00101 0.00049 H3 0.69016 0.56862 0.80565 1.00000 0.02726 0.00000 0.00000 C4 0.90579 0.40412 0.81914 1.00000 0.03307 0.02635 0.02094 -0.00342 -0.00211 -0.01113 0.02706 0.00349 0.00030 0.00026 0.00016 0.00000 0.00137 0.00130 0.00115 0.00097 0.00101 0.00112 0.00053 H4 0.89374 0.37327 0.88157 1.00000 0.03247 0.00000 0.00000 C5 1.04582 0.33227 0.77359 1.00000 0.02579 0.01795 0.03428 -0.00690 -0.00850 -0.00635 0.02594 0.00331 0.00029 0.00025 0.00017 0.00000 0.00125 0.00116 0.00133 0.00100 0.00104 0.00100 0.00052 C6 1.06504 0.37924 0.68288 1.00000 0.02180 0.02494 0.03229 -0.01304 0.00162 -0.00923 0.02540 0.00329 0.00028 0.00025 0.00016 0.00000 0.00120 0.00125 0.00130 0.00103 0.00101 0.00103 0.00052 H6 1.16171 0.33274 0.65206 1.00000 0.03048 0.00000 0.00000 C7 0.94139 0.49510 0.63747 1.00000 0.02410 0.02621 0.02336 -0.00878 0.00274 -0.01373 0.02292 0.00320 0.00027 0.00025 0.00016 0.00000 0.00120 0.00125 0.00114 0.00096 0.00095 0.00104 0.00049 H7 0.95388 0.52632 0.57514 1.00000 0.02751 0.00000 0.00000 C8 1.30621 0.14445 0.78173 1.00000 0.03383 0.02998 0.06266 -0.00991 -0.01047 0.00189 0.04620 0.00467 0.00035 0.00031 0.00023 0.00000 0.00159 0.00155 0.00201 0.00142 0.00143 0.00129 0.00075 H8A 1.28985 0.10865 0.72965 1.00000 0.06929 0.00000 0.00000 H8B 1.37506 0.06461 0.82479 1.00000 0.06929 0.00000 0.00000 H8C 1.35611 0.21131 0.76160 1.00000 0.06929 0.00000 0.00000 C9 0.71719 0.45249 0.23733 1.00000 0.01744 0.02072 0.01761 -0.00593 0.00106 -0.01026 0.01744 0.00299 0.00025 0.00023 0.00014 0.00000 0.00107 0.00113 0.00103 0.00086 0.00085 0.00093 0.00044 C10 0.85264 0.32147 0.25821 1.00000 0.02143 0.02217 0.02095 -0.00451 -0.00099 -0.01185 0.02032 0.00311 0.00027 0.00024 0.00015 0.00000 0.00115 0.00117 0.00109 0.00090 0.00090 0.00098 0.00047 C11 0.78575 0.33177 0.40644 1.00000 0.01908 0.02037 0.02050 -0.00670 0.00172 -0.01076 0.01872 0.00303 0.00026 0.00023 0.00014 0.00000 0.00110 0.00113 0.00108 0.00089 0.00088 0.00095 0.00045 C12 0.67230 0.53603 0.14560 1.00000 0.02571 0.02030 0.02025 -0.00592 -0.00016 -0.00963 0.02164 0.00322 0.00028 0.00024 0.00015 0.00000 0.00122 0.00115 0.00110 0.00090 0.00093 0.00099 0.00048 C13 0.78542 0.55246 0.08129 1.00000 0.02691 0.02655 0.02445 -0.00774 0.00376 -0.01190 0.02540 0.00346 0.00030 0.00026 0.00015 0.00000 0.00126 0.00128 0.00118 0.00099 0.00099 0.00107 0.00051 H13 0.89467 0.50836 0.09569 1.00000 0.03049 0.00000 0.00000 C14 0.73818 0.63288 -0.00320 1.00000 0.03893 0.02859 0.02742 -0.00863 0.00761 -0.01328 0.03179 0.00384 0.00033 0.00027 0.00017 0.00000 0.00152 0.00137 0.00128 0.00106 0.00112 0.00121 0.00058 H14 0.81520 0.64431 -0.04618 1.00000 0.03815 0.00000 0.00000 C15 0.57862 0.69687 -0.02531 1.00000 0.04914 0.02852 0.01941 -0.00295 -0.00253 -0.00969 0.03443 0.00396 0.00035 0.00028 0.00017 0.00000 0.00170 0.00139 0.00119 0.00103 0.00115 0.00127 0.00062 H15 0.54678 0.75037 -0.08360 1.00000 0.04131 0.00000 0.00000 C16 0.46700 0.68217 0.03788 1.00000 0.02889 0.03554 0.02310 -0.00647 -0.00651 -0.00492 0.03129 0.00372 0.00031 0.00028 0.00016 0.00000 0.00135 0.00147 0.00122 0.00107 0.00104 0.00116 0.00058 H16 0.35788 0.72696 0.02320 1.00000 0.03755 0.00000 0.00000 C17 0.51277 0.60233 0.12297 1.00000 0.02734 0.03131 0.02352 -0.00879 0.00097 -0.01071 0.02729 0.00347 0.00030 0.00027 0.00016 0.00000 0.00128 0.00135 0.00118 0.00102 0.00099 0.00110 0.00053 H17 0.43475 0.59295 0.16591 1.00000 0.03275 0.00000 0.00000 C18 0.95689 0.23590 0.19122 1.00000 0.02297 0.02053 0.02069 -0.00384 0.00092 -0.00899 0.02137 0.00326 0.00027 0.00024 0.00015 0.00000 0.00117 0.00116 0.00111 0.00090 0.00092 0.00097 0.00047 C19 1.11921 0.16507 0.20642 1.00000 0.02438 0.02457 0.02099 -0.00486 0.00088 -0.00904 0.02355 0.00346 0.00028 0.00025 0.00015 0.00000 0.00123 0.00123 0.00111 0.00094 0.00094 0.00103 0.00049 H19 1.16227 0.17355 0.25864 1.00000 0.02826 0.00000 0.00000 C20 1.21810 0.08197 0.14510 1.00000 0.02537 0.02880 0.03520 -0.00513 0.00541 -0.00672 0.03166 0.00398 0.00031 0.00028 0.00017 0.00000 0.00131 0.00137 0.00140 0.00110 0.00109 0.00111 0.00058 H20 1.32860 0.03350 0.15577 1.00000 0.03800 0.00000 0.00000 C21 1.15657 0.06951 0.06876 1.00000 0.04071 0.02765 0.02929 -0.01105 0.00986 -0.00770 0.03447 0.00409 0.00033 0.00028 0.00017 0.00000 0.00158 0.00138 0.00134 0.00109 0.00117 0.00122 0.00062 H21 1.22471 0.01416 0.02644 1.00000 0.04137 0.00000 0.00000 C22 0.99445 0.13842 0.05427 1.00000 0.04371 0.02904 0.02589 -0.01020 -0.00503 -0.00816 0.03402 0.00389 0.00034 0.00028 0.00017 0.00000 0.00162 0.00139 0.00129 0.00107 0.00115 0.00124 0.00061 H22 0.95186 0.12883 0.00225 1.00000 0.04082 0.00000 0.00000 C23 0.89458 0.22078 0.11484 1.00000 0.03116 0.02824 0.02703 -0.00666 -0.00748 -0.00987 0.02878 0.00349 0.00031 0.00027 0.00016 0.00000 0.00135 0.00133 0.00125 0.00103 0.00105 0.00112 0.00054 H23 0.78383 0.26703 0.10459 1.00000 0.03453 0.00000 0.00000 C24 0.27321 0.71927 0.35091 1.00000 0.02247 0.02200 0.01837 -0.00465 0.00056 -0.01055 0.02031 0.00314 0.00027 0.00024 0.00015 0.00000 0.00115 0.00117 0.00106 0.00089 0.00089 0.00098 0.00046 H24 0.35507 0.67856 0.30894 1.00000 0.02437 0.00000 0.00000 C25 0.13330 0.83051 0.31840 1.00000 0.02964 0.02187 0.01897 -0.00016 -0.00515 -0.01309 0.02272 0.00324 0.00028 0.00024 0.00015 0.00000 0.00128 0.00118 0.00109 0.00091 0.00095 0.00104 0.00049 H25 0.12085 0.86452 0.25549 1.00000 0.02727 0.00000 0.00000 C26 0.01222 0.89146 0.37818 1.00000 0.02313 0.01910 0.02790 -0.00200 -0.00637 -0.00691 0.02380 0.00328 0.00028 0.00025 0.00016 0.00000 0.00120 0.00115 0.00122 0.00095 0.00098 0.00098 0.00050 H26 -0.08452 0.96730 0.35732 1.00000 0.02856 0.00000 0.00000 C27 0.03629 0.83837 0.46988 1.00000 0.02114 0.02289 0.02426 -0.00796 0.00098 -0.00882 0.02232 0.00323 0.00027 0.00025 0.00015 0.00000 0.00115 0.00119 0.00115 0.00094 0.00093 0.00098 0.00048 H27 -0.04407 0.87739 0.51298 1.00000 0.02679 0.00000 0.00000 C28 0.17904 0.72803 0.49704 1.00000 0.02193 0.01858 0.01684 -0.00463 -0.00102 -0.01119 0.01782 0.00298 0.00026 0.00023 0.00014 0.00000 0.00113 0.00110 0.00103 0.00085 0.00087 0.00095 0.00044 N1 0.64812 0.44490 0.38838 1.00000 0.02175 0.02061 0.01923 -0.00462 0.00088 -0.01149 0.01944 0.00260 0.00022 0.00020 0.00012 0.00000 0.00098 0.00097 0.00092 0.00075 0.00076 0.00083 0.00039 N2 0.61860 0.50944 0.30299 1.00000 0.02347 0.02374 0.01758 -0.00472 -0.00062 -0.01160 0.02071 0.00261 0.00023 0.00020 0.00012 0.00000 0.00100 0.00102 0.00091 0.00077 0.00076 0.00085 0.00040 N3 0.88931 0.26636 0.34455 1.00000 0.02123 0.02200 0.02000 -0.00609 0.00072 -0.01024 0.02028 0.00261 0.00022 0.00020 0.00012 0.00000 0.00097 0.00100 0.00093 0.00077 0.00076 0.00083 0.00040 N4 0.29778 0.66684 0.43895 1.00000 0.01950 0.01782 0.01770 -0.00539 -0.00042 -0.00941 0.01736 0.00247 0.00021 0.00019 0.00012 0.00000 0.00094 0.00092 0.00088 0.00072 0.00073 0.00078 0.00038 O1 0.73241 0.82447 0.60318 1.00000 0.02217 0.01989 0.02895 -0.00441 -0.00273 -0.01228 0.02218 0.00215 0.00018 0.00016 0.00011 0.00000 0.00083 0.00082 0.00085 0.00066 0.00067 0.00069 0.00035 O2 1.15629 0.21586 0.82442 1.00000 0.03399 0.02605 0.04218 -0.00544 -0.01064 -0.00068 0.03731 0.00272 0.00022 0.00019 0.00013 0.00000 0.00104 0.00097 0.00108 0.00082 0.00085 0.00083 0.00045 P1 0.64142 0.71938 0.62168 1.00000 0.01922 0.01883 0.01960 -0.00539 -0.00007 -0.00998 0.01816 0.00079 0.00007 0.00006 0.00004 0.00000 0.00029 0.00030 0.00028 0.00022 0.00022 0.00024 0.00014 S1 0.61510 0.67832 0.50011 1.00000 0.02502 0.02291 0.01774 -0.00421 -0.00090 -0.01375 0.02037 0.00077 0.00007 0.00006 0.00004 0.00000 0.00030 0.00030 0.00027 0.00022 0.00022 0.00025 0.00014 S2 0.45050 0.79482 0.69798 1.00000 0.02034 0.02438 0.02705 -0.00997 0.00337 -0.00928 0.02331 0.00083 0.00007 0.00006 0.00004 0.00000 0.00029 0.00031 0.00030 0.00024 0.00023 0.00025 0.00014 Ni1 0.50000 0.50000 0.50000 0.50000 0.01603 0.01708 0.01349 -0.00364 0.00010 -0.00651 0.01547 0.00000 0.00000 0.00000 0.00000 0.00000 0.00021 0.00021 0.00019 0.00015 0.00015 0.00016 0.00011 Final Structure Factor Calculation for 2005slh0421 in P-1 Total number of l.s. parameters = 343 Maximum vector length = 511 Memory required = 3849 / 26061 wR2 = 0.0991 before cycle 7 for 5955 data and 0 / 343 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0416 for 4790 Fo > 4sig(Fo) and 0.0573 for all 5955 data wR2 = 0.0991, GooF = S = 1.038, Restrained GooF = 1.038 for all data Occupancy sum of asymmetric unit = 37.50 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0390 0.0269 0.0184 C1 0.0226 0.0220 0.0114 C2 0.0270 0.0238 0.0173 C3 0.0341 0.0264 0.0207 C4 0.0405 0.0208 0.0165 C5 0.0367 0.0218 0.0177 C6 0.0304 0.0207 0.0177 C7 0.0686 0.0488 0.0212 C8 0.0225 0.0162 0.0136 C9 0.0239 0.0214 0.0156 C10 0.0242 0.0178 0.0142 C11 0.0258 0.0225 0.0166 C12 0.0306 0.0250 0.0207 C13 0.0441 0.0292 0.0220 C14 0.0553 0.0287 0.0192 C15 0.0471 0.0277 0.0190 C16 0.0334 0.0277 0.0207 C17 0.0237 0.0204 0.0200 C18 0.0261 0.0243 0.0202 C19 0.0420 0.0313 0.0217 C20 0.0520 0.0333 0.0181 C21 0.0521 0.0303 0.0197 C22 0.0387 0.0277 0.0199 C23 0.0235 0.0198 0.0175 C24 0.0318 0.0193 0.0171 C25 0.0319 0.0214 0.0181 C26 0.0272 0.0212 0.0186 C27 0.0228 0.0183 0.0124 C28 0.0236 0.0187 0.0159 N1 0.0250 0.0208 0.0162 N2 0.0239 0.0199 0.0170 N3 0.0205 0.0189 0.0128 N4 0.0296 0.0235 0.0134 O1 0.0545 0.0369 0.0206 O2 0.0216 0.0191 0.0138 P1 0.0270 0.0190 0.0151 S1 0.0310 0.0210 0.0180 S2 0.0174 0.0161 0.0129 Ni1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.030 0.046 0.063 0.081 0.102 0.126 0.162 0.217 1.000 Number in group 630. 577. 600. 594. 603. 586. 587. 596. 586. 596. GooF 1.000 0.950 1.033 1.080 1.095 1.096 1.117 0.979 1.020 0.993 K 1.816 0.982 0.976 0.956 0.965 0.975 0.995 1.009 1.025 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.66 inf Number in group 618. 574. 605. 593. 592. 602. 581. 601. 595. 594. GooF 1.003 0.963 0.997 0.987 0.990 0.984 0.980 0.943 1.051 1.402 K 0.968 1.004 1.007 1.007 1.026 1.026 1.024 1.016 1.003 0.997 R1 0.135 0.116 0.096 0.077 0.060 0.048 0.040 0.032 0.029 0.030 Recommended weighting scheme: WGHT 0.0334 1.1545 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 2 1 95.19 42.41 5.48 0.043 4.70 -4 0 3 413.33 276.24 5.39 0.109 1.93 -3 0 6 179.89 76.17 5.17 0.057 1.84 -2 2 4 455.05 318.67 4.97 0.117 2.24 3 -3 6 97.57 36.15 4.92 0.039 1.38 -3 3 3 27.50 0.95 4.91 0.006 1.71 -3 -6 6 26.41 0.60 4.56 0.005 1.29 0 -3 3 46.38 5.33 4.45 0.015 2.47 6 3 0 25.41 2.52 4.44 0.010 1.54 7 11 9 78.87 160.10 4.31 0.083 0.85 3 0 3 28.77 0.83 4.29 0.006 2.46 3 6 9 69.81 19.48 4.23 0.029 1.31 -3 2 6 54.39 98.98 4.01 0.065 1.64 4 5 4 104.35 59.80 3.98 0.051 1.76 2 0 0 36.70 12.23 3.98 0.023 4.22 -5 6 11 38.83 105.43 3.89 0.067 0.82 -11 -7 4 47.68 119.84 3.88 0.072 0.79 -10 -8 6 139.33 286.11 3.88 0.111 0.79 8 12 6 44.78 101.10 3.74 0.066 0.81 10 1 7 -2.90 42.41 3.67 0.043 0.82 0 0 9 1655.32 1965.15 3.64 0.291 1.65 -3 -3 6 382.91 283.74 3.61 0.110 1.70 5 -4 5 188.27 272.94 3.58 0.108 1.06 -11 -6 5 -41.54 57.77 3.46 0.050 0.78 -1 2 1 138.88 94.52 3.39 0.064 3.54 1 0 7 891.70 741.91 3.32 0.179 2.06 -1 -2 5 580.30 475.34 3.25 0.143 2.38 1 -1 7 727.40 867.40 3.15 0.193 1.91 2 2 10 95.79 59.19 3.12 0.050 1.47 -2 9 2 1136.97 922.08 3.12 0.199 0.94 7 -4 7 975.20 693.80 3.12 0.173 0.84 3 -6 2 78.80 126.30 3.09 0.074 1.14 -6 4 8 1285.77 1072.49 3.08 0.215 0.93 2 -3 9 253.50 189.28 3.08 0.090 1.24 -1 -1 3 785.50 929.86 3.07 0.200 3.96 3 1 7 -3.46 8.48 3.06 0.019 1.80 -3 -3 3 758.97 899.28 3.04 0.197 2.23 2 1 5 98.13 65.38 3.02 0.053 2.62 -4 -6 13 8.82 38.39 3.02 0.041 0.86 8 9 12 99.68 168.15 3.01 0.085 0.83 0 6 5 484.26 589.50 3.00 0.159 1.49 -2 -1 3 52.42 30.88 2.97 0.036 3.22 -2 -11 4 72.84 141.66 2.97 0.078 0.85 -3 -13 1 -5.14 44.57 2.95 0.044 0.77 5 3 15 51.27 15.77 2.91 0.026 0.91 -6 -1 4 13.13 1.03 2.90 0.007 1.36 10 8 1 -4.66 9.38 2.89 0.020 0.88 7 -2 3 327.83 419.87 2.88 0.134 1.04 2 1 3 3086.84 3529.25 2.87 0.390 3.55 0 -3 13 150.18 202.52 2.87 0.093 1.02 Bond lengths and angles C1 - Distance Angles O1 1.4433 (0.0028) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles C3 1.3959 (0.0031) C7 1.3974 (0.0031) 118.31 (0.21) P1 1.8150 (0.0023) 121.40 (0.17) 120.25 (0.17) C2 - C3 C7 C3 - Distance Angles C4 1.3783 (0.0034) C2 1.3959 (0.0031) 120.93 (0.21) H3 0.9500 119.54 119.54 C3 - C4 C2 C4 - Distance Angles C3 1.3783 (0.0034) C5 1.3937 (0.0035) 120.19 (0.22) H4 0.9500 119.91 119.91 C4 - C3 C5 C5 - Distance Angles O2 1.3728 (0.0030) C6 1.3878 (0.0034) 124.71 (0.22) C4 1.3937 (0.0035) 115.33 (0.22) 119.96 (0.22) C5 - O2 C6 C6 - Distance Angles C5 1.3878 (0.0034) C7 1.3921 (0.0035) 119.41 (0.22) H6 0.9500 120.30 120.30 C6 - C5 C7 C7 - Distance Angles C6 1.3921 (0.0035) C2 1.3974 (0.0031) 121.16 (0.21) H7 0.9500 119.42 119.42 C7 - C6 C2 C8 - Distance Angles O2 1.4348 (0.0034) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O2 H8A H8B C9 - Distance Angles N2 1.3320 (0.0028) C10 1.4286 (0.0032) 120.02 (0.20) C12 1.4864 (0.0031) 114.44 (0.20) 125.54 (0.19) C9 - N2 C10 C10 - Distance Angles N3 1.3368 (0.0029) C9 1.4286 (0.0032) 119.14 (0.20) C18 1.4825 (0.0031) 115.55 (0.20) 125.28 (0.20) C10 - N3 C9 C11 - Distance Angles N3 1.3381 (0.0028) N1 1.3401 (0.0030) 125.16 (0.20) C28_$1 1.4836 (0.0030) 118.17 (0.20) 116.61 (0.19) C11 - N3 N1 C12 - Distance Angles C17 1.3932 (0.0034) C13 1.4047 (0.0032) 118.77 (0.22) C9 1.4864 (0.0031) 119.10 (0.20) 122.12 (0.21) C12 - C17 C13 C13 - Distance Angles C14 1.3874 (0.0035) C12 1.4047 (0.0032) 120.24 (0.24) H13 0.9500 119.88 119.88 C13 - C14 C12 C14 - Distance Angles C13 1.3874 (0.0035) C15 1.3914 (0.0039) 120.37 (0.24) H14 0.9500 119.81 119.81 C14 - C13 C15 C15 - Distance Angles C16 1.3789 (0.0037) C14 1.3914 (0.0039) 119.60 (0.23) H15 0.9500 120.20 120.20 C15 - C16 C14 C16 - Distance Angles C15 1.3789 (0.0037) C17 1.3913 (0.0034) 120.58 (0.25) H16 0.9500 119.71 119.71 C16 - C15 C17 C17 - Distance Angles C16 1.3913 (0.0034) C12 1.3932 (0.0034) 120.43 (0.23) H17 0.9500 119.79 119.79 C17 - C16 C12 C18 - Distance Angles C19 1.3941 (0.0033) C23 1.3984 (0.0033) 119.47 (0.22) C10 1.4825 (0.0031) 119.31 (0.20) 121.17 (0.21) C18 - C19 C23 C19 - Distance Angles C20 1.3911 (0.0034) C18 1.3941 (0.0033) 119.98 (0.23) H19 0.9500 120.01 120.01 C19 - C20 C18 C20 - Distance Angles C21 1.3822 (0.0038) C19 1.3911 (0.0034) 120.40 (0.25) H20 0.9500 119.80 119.80 C20 - C21 C19 C21 - Distance Angles C20 1.3822 (0.0038) C22 1.3898 (0.0040) 119.62 (0.24) H21 0.9500 120.19 120.19 C21 - C20 C22 C22 - Distance Angles C23 1.3826 (0.0036) C21 1.3898 (0.0040) 120.62 (0.25) H22 0.9500 119.69 119.69 C22 - C23 C21 C23 - Distance Angles C22 1.3826 (0.0036) C18 1.3984 (0.0033) 119.88 (0.24) H23 0.9500 120.06 120.06 C23 - C22 C18 C24 - Distance Angles N4 1.3419 (0.0028) C25 1.3899 (0.0033) 122.90 (0.21) H24 0.9500 118.55 118.55 C24 - N4 C25 C25 - Distance Angles C26 1.3838 (0.0033) C24 1.3899 (0.0033) 119.64 (0.21) H25 0.9500 120.18 120.18 C25 - C26 C24 C26 - Distance Angles C25 1.3838 (0.0033) C27 1.3940 (0.0032) 118.09 (0.22) H26 0.9500 120.96 120.96 C26 - C25 C27 C27 - Distance Angles C28 1.3821 (0.0033) C26 1.3940 (0.0032) 118.88 (0.21) H27 0.9500 120.56 120.56 C27 - C28 C26 C28 - Distance Angles N4 1.3555 (0.0028) C27 1.3821 (0.0032) 123.46 (0.20) C11_$1 1.4836 (0.0030) 114.68 (0.19) 121.85 (0.20) C28 - N4 C27 N1 - Distance Angles N2 1.3345 (0.0025) C11 1.3401 (0.0030) 118.35 (0.18) Ni1 2.0823 (0.0018) 126.75 (0.15) 114.90 (0.14) N1 - N2 C11 N2 - Distance Angles C9 1.3320 (0.0028) N1 1.3345 (0.0025) 119.81 (0.19) N2 - C9 N3 - Distance Angles C10 1.3368 (0.0029) C11 1.3381 (0.0028) 116.64 (0.20) N3 - C10 N4 - Distance Angles C24 1.3419 (0.0028) C28 1.3555 (0.0028) 117.03 (0.19) Ni1 2.1022 (0.0019) 128.15 (0.15) 114.83 (0.14) N4 - C24 C28 O1 - Distance Angles C1 1.4433 (0.0028) P1 1.6166 (0.0016) 121.60 (0.14) O1 - C1 O2 - Distance Angles C5 1.3728 (0.0030) C8 1.4348 (0.0034) 117.09 (0.21) O2 - C5 P1 - Distance Angles O1 1.6166 (0.0016) C2 1.8150 (0.0024) 97.28 (0.09) S2 1.9717 (0.0009) 111.15 (0.07) 112.24 (0.08) S1 2.0189 (0.0008) 106.34 (0.06) 109.64 (0.08) 118.06 (0.04) P1 - O1 C2 S2 S1 - Distance Angles P1 2.0189 (0.0008) Ni1 2.5061 (0.0007) 116.58 (0.03) S1 - P1 S2 - Distance Angles P1 1.9717 (0.0009) S2 - Ni1 - Distance Angles N1 2.0823 (0.0018) N1_$1 2.0823 (0.0018) 180.00 N4 2.1022 (0.0019) 101.33 (0.07) 78.67 (0.07) N4_$1 2.1022 (0.0019) 78.67 (0.07) 101.33 (0.07) 180.00 (0.09) S1 2.5061 (0.0007) 85.10 (0.05) 94.90 (0.05) 88.20 (0.05) 91.80 (0.05) S1_$1 2.5061 (0.0007) 94.90 (0.05) 85.10 (0.05) 91.80 (0.05) 88.20 (0.05) 180.00 Ni1 - N1 N1_$1 N4 N4_$1 S1 FMAP and GRID set by program FMAP 2 3 41 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0550 for 5955 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.4539 0.6603 0.2249 [ 1.30 A from H17 ] Deepest hole -0.38 at 0.4253 0.5762 0.4711 [ 0.88 A from NI1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3621 / 27637 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4539 0.6603 0.2249 1.00000 0.05 0.51 1.30 H17 1.49 H24 1.72 C17 1.96 N2 Q2 1 0.6126 0.7381 -0.0925 1.00000 0.05 0.46 0.58 H15 1.10 C15 1.75 C14 1.85 H14 Q3 1 0.9825 0.2839 0.2399 1.00000 0.05 0.41 1.06 C18 1.13 C10 1.49 C19 1.60 H19 Q4 1 0.4363 0.6255 0.3079 1.00000 0.05 0.40 0.73 H24 1.58 C24 1.63 N2 2.23 H17 Q5 1 0.5437 0.5261 0.3610 1.00000 0.05 0.40 1.04 N1 1.06 N2 1.92 H24 2.09 NI1 Shortest distances between peaks (including symmetry equivalents) 1 4 1.25 4 5 1.30 1 5 2.27 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 0.01: 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. 2.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.02: Generate idealized H-atoms 3.81: Structure factors and derivatives 12.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.89: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.24: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.06: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0421 finished at 10:50:50 Total CPU time: 20.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++