+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0009p-1 started at 15:22:25 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0009p-1 in P-1 CELL 0.71073 8.3059 10.8568 15.6687 71.627 77.606 81.799 ZERR 2.00 0.0004 0.0008 0.0011 0.003 0.004 0.004 LATT 1 SFAC C H N O UNIT 40 96 4 16 V = 1305.36 F(000) = 492.0 Mu = 0.09 mm-1 Cell Wt = 889.21 Rho = 1.131 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 O1WA H1WA O1WA H2WA O1WB H1WB O1WB H2WB O2W H21W O2W H22W DANG 1.35 0.02 H1WA H2WA H1WB H2WB H21W H22W HTAB O2 O1A HTAB N25 O3 HTAB N25 O4B HTAB O2W O1A EQIV_$1 -x+1, -y+1, -z HTAB O2 O1WB_$1 HTAB O2 O1WA_$1 HTAB N25 O2_$1 HTAB N25 O1WA_$1 EQIV_$2 -x+1, -y, -z HTAB O3 O1B_$2 HTAB N35 O1A_$2 HTAB O2W O1B_$2 EQIV_$3 -x+2, -y, -z HTAB N35 O4A_$3 EQIV_$4 x+1, y, z HTAB N35 O2W_$4 EQIV_$5 x-1, y, z HTAB O2W O4A_$5 EQIV_$6 -x+2, -y+1, -z MPLA C1 O1A O1B MPLA C4 O4A O4B FMAP 2 PLAN 10 SIZE 0.02 0.08 0.10 ACTA BOND $H WGHT 0.05840 4.97040 L.S. 4 TEMP -153.00 FVAR 0.69917 0.79865 MOLE 1 C1 1 0.514726 0.140045 -0.094591 11.00000 0.02288 0.02214 = 0.02606 -0.00763 -0.00734 -0.00299 C2 1 0.611920 0.241505 -0.083421 11.00000 0.02106 0.02065 = 0.03104 -0.01065 -0.00461 -0.00294 AFIX 13 H2 2 0.702394 0.263528 -0.138015 11.00000 -1.20000 AFIX 0 C3 1 0.692731 0.188643 0.001486 11.00000 0.02103 0.02342 = 0.03953 -0.01580 -0.00528 0.00116 AFIX 13 H3 2 0.761793 0.106206 -0.001399 11.00000 -1.20000 AFIX 0 C4 1 0.804493 0.288985 0.000847 11.00000 0.03004 0.02309 = 0.04157 -0.01308 -0.01669 0.00170 O1A 4 0.361023 0.163759 -0.086842 11.00000 0.02248 0.03469 = 0.04152 -0.01753 -0.01013 -0.00305 O1B 4 0.595502 0.039679 -0.110023 11.00000 0.02495 0.02231 = 0.03724 -0.01170 -0.00370 -0.00260 O2 4 0.512794 0.357760 -0.080448 11.00000 0.02267 0.02205 = 0.05270 -0.01038 -0.01229 -0.00151 AFIX 147 H2O 2 0.413031 0.345813 -0.075366 11.00000 -1.50000 AFIX 0 O3 4 0.574700 0.162864 0.083226 11.00000 0.03380 0.02374 = 0.03500 -0.01066 -0.00663 -0.00901 AFIX 147 H3O 2 0.530163 0.094728 0.090226 11.00000 -1.50000 AFIX 0 O4A 4 0.933671 0.301946 -0.060252 11.00000 0.02285 0.04442 = 0.07159 -0.03502 0.00236 -0.00982 O4B 4 0.760683 0.352707 0.056231 11.00000 0.05325 0.03966 = 0.05204 -0.02952 -0.00439 -0.01348 MOLE 2 C21 1 0.475955 0.177619 0.422018 11.00000 0.11767 0.04521 = 0.03411 -0.00488 0.00969 -0.01836 AFIX 137 H21A 2 0.354883 0.189682 0.432765 11.00000 -1.50000 H21B 2 0.514699 0.158213 0.480056 11.00000 -1.50000 H21C 2 0.512770 0.105158 0.395905 11.00000 -1.50000 AFIX 0 C22 1 0.547017 0.302223 0.355395 11.00000 0.07071 0.03306 = 0.03518 -0.01322 0.00325 -0.00712 C23 1 0.519840 0.327959 0.256875 11.00000 0.03770 0.02859 = 0.03667 -0.01134 0.00796 -0.00896 AFIX 23 H23A 2 0.589801 0.259580 0.233487 11.00000 -1.20000 H23B 2 0.567385 0.411441 0.220827 11.00000 -1.20000 AFIX 0 C24 1 0.348702 0.335321 0.230667 11.00000 0.03882 0.02067 = 0.05841 -0.01338 0.00971 -0.00808 C26 1 0.735294 0.286835 0.348635 11.00000 0.07967 0.05854 = 0.04456 -0.01418 -0.01961 -0.00269 AFIX 137 H26A 2 0.781451 0.212301 0.326073 11.00000 -1.50000 H26B 2 0.761983 0.272294 0.409197 11.00000 -1.50000 H26C 2 0.782805 0.366071 0.306314 11.00000 -1.50000 AFIX 0 C27 1 0.479382 0.416670 0.394290 11.00000 0.09932 0.04982 = 0.04931 -0.02482 0.00247 -0.00588 AFIX 137 H27A 2 0.517556 0.497910 0.349920 11.00000 -1.50000 H27B 2 0.519244 0.402989 0.451353 11.00000 -1.50000 H27C 2 0.358220 0.422088 0.406400 11.00000 -1.50000 AFIX 0 C28 1 0.220878 0.436253 0.259967 11.00000 0.04383 0.03856 = 0.09069 -0.03037 0.01923 -0.00514 AFIX 137 H28A 2 0.125932 0.447711 0.229555 11.00000 -1.50000 H28B 2 0.270270 0.519376 0.242830 11.00000 -1.50000 H28C 2 0.184096 0.406685 0.326388 11.00000 -1.50000 AFIX 0 C29 1 0.276768 0.203372 0.257494 11.00000 0.05269 0.03713 = 0.07339 -0.01760 0.01616 -0.02236 AFIX 137 H29A 2 0.242375 0.172590 0.324047 11.00000 -1.50000 H29B 2 0.360975 0.140365 0.237449 11.00000 -1.50000 H29C 2 0.180897 0.212676 0.228162 11.00000 -1.50000 AFIX 0 N25 3 0.386454 0.381074 0.127782 11.00000 0.02676 0.02440 = 0.05744 -0.01507 -0.00808 -0.00167 AFIX 137 H25A 2 0.463653 0.323828 0.106968 11.00000 -1.50000 H25B 2 0.426083 0.461096 0.108700 11.00000 -1.50000 H25C 2 0.292447 0.385953 0.105489 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 1.263429 -0.213937 0.362976 11.00000 0.03894 0.05955 = 0.03960 -0.01166 -0.01766 -0.00300 AFIX 137 H31A 2 1.306487 -0.133763 0.319466 11.00000 -1.50000 H31B 2 1.309326 -0.287984 0.339814 11.00000 -1.50000 H31C 2 1.295336 -0.227304 0.422142 11.00000 -1.50000 AFIX 0 C32 1 1.073533 -0.202565 0.374770 11.00000 0.03280 0.03018 = 0.02562 -0.00744 -0.00424 -0.00354 C33 1 1.039162 -0.177990 0.277135 11.00000 0.02586 0.02723 = 0.02929 -0.00992 -0.00993 -0.00002 AFIX 23 H33A 2 1.087436 -0.095382 0.239565 11.00000 -1.20000 H33B 2 1.106010 -0.247507 0.253718 11.00000 -1.20000 AFIX 0 C34 1 0.866795 -0.169345 0.253572 11.00000 0.02500 0.02604 = 0.03155 -0.00900 -0.00118 -0.00269 C36 1 1.009333 -0.328158 0.441651 11.00000 0.05855 0.03597 = 0.03546 -0.00267 -0.00970 -0.00842 AFIX 137 H36A 2 1.053662 -0.347784 0.498047 11.00000 -1.50000 H36B 2 1.044667 -0.399534 0.414319 11.00000 -1.50000 H36C 2 0.888263 -0.318163 0.455725 11.00000 -1.50000 AFIX 0 C37 1 1.007239 -0.088830 0.413500 11.00000 0.05986 0.03856 = 0.04465 -0.02126 -0.01555 -0.00349 AFIX 137 H37A 2 0.886277 -0.086001 0.428912 11.00000 -1.50000 H37B 2 1.040538 -0.007147 0.367793 11.00000 -1.50000 H37C 2 1.052351 -0.100339 0.468653 11.00000 -1.50000 AFIX 0 C38 1 0.790774 -0.299061 0.283956 11.00000 0.04427 0.04346 = 0.05045 -0.00214 -0.01474 -0.01787 AFIX 137 H38A 2 0.690892 -0.288703 0.257727 11.00000 -1.50000 H38B 2 0.761831 -0.328390 0.350827 11.00000 -1.50000 H38C 2 0.870587 -0.363720 0.262904 11.00000 -1.50000 AFIX 0 C39 1 0.742668 -0.064578 0.281350 11.00000 0.03217 0.06310 = 0.04377 -0.02129 -0.00359 0.01026 AFIX 137 H39A 2 0.644921 -0.054797 0.253429 11.00000 -1.50000 H39B 2 0.793661 0.018343 0.260393 11.00000 -1.50000 H39C 2 0.709749 -0.090033 0.348057 11.00000 -1.50000 AFIX 0 N35 3 0.898446 -0.127114 0.149834 11.00000 0.02359 0.03205 = 0.03273 -0.01307 -0.00929 -0.00160 AFIX 137 H35A 2 0.969498 -0.187739 0.129150 11.00000 -1.50000 H35B 2 0.943558 -0.049077 0.128246 11.00000 -1.50000 H35C 2 0.801264 -0.119197 0.129893 11.00000 -1.50000 AFIX 0 MOLE 4 PART 1 O1WA 4 0.821720 0.601389 0.004653 21.00000 0.03471 0.03483 = 0.11885 -0.03071 -0.02778 0.00194 PART 2 O1WB 4 0.799074 0.547188 0.121149 -21.00000 0.02598 0.01457 = 0.04881 -0.01433 0.00178 0.00246 MOLE 5 PART 0 O2W 4 0.095534 0.085715 0.087443 11.00000 0.02663 0.03254 = 0.04959 -0.00654 -0.00663 0.00066 AFIX 2 H21W 2 0.098798 0.152854 0.042410 11.00000 -1.50000 H22W 2 0.189355 0.046370 0.084318 11.00000 -1.50000 AFIX 0 HKLF 4 ** Warning: no match for 8 atoms in DFIX ** Following atoms could not be matched for particular residues for DFIX: H1WA H2WA H1WB H2WB H1WA H2WA H1WB H2WB Covalent radii and connectivity table for 07skc0009p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - C22 C22 - C21 C26 C27 C23 C23 - C22 C24 C24 - N25 C28 C29 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - C32 C32 - C36 C37 C31 C33 C33 - C34 C32 C34 - N35 C38 C39 C33 C36 - C32 C37 - C32 C38 - C34 C39 - C34 N35 - C34 O1WA_a - no bonds found O1WB_b - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y+1, -z $2 -x+1, -y, -z $3 -x+2, -y, -z $4 x+1, y, z $5 x-1, y, z 19972 Reflections read, of which 107 rejected -10 =< h =< 10, -14 =< k =< 14, -20 =< l =< 20, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 -6 4 1.89 0.67 5 5.21 1 Inconsistent equivalents 5901 Unique reflections, of which 0 suppressed R(int) = 0.0859 R(sigma) = 0.1065 Friedel opposites merged Maximum memory for data reduction = 4063 / 59381 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 40.00 40.00 H 96.00 92.00 N 4.00 4.00 O 16.00 16.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 5012 / 376670 wR2 = 0.2818 before cycle 1 for 5901 data and 301 / 301 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.085; Restrained GooF = 1.085 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0584 * P )^2 + 4.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69918 0.00241 0.004 OSF 2 0.79867 0.00925 0.002 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.004 for OSF Max. shift = 0.000 A for H21W Max. dU = 0.000 for O1WB_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 5012 / 376670 wR2 = 0.2818 before cycle 2 for 5901 data and 301 / 301 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.085; Restrained GooF = 1.085 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0584 * P )^2 + 4.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69918 0.00241 0.001 OSF 2 0.79867 0.00925 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for x O1WA_a Max. shift = 0.000 A for H21W Max. dU = 0.000 for O1WB_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 5012 / 376670 wR2 = 0.2818 before cycle 3 for 5901 data and 301 / 301 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.085; Restrained GooF = 1.085 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0584 * P )^2 + 4.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69918 0.00241 0.001 OSF 2 0.79868 0.00925 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H21W Max. dU = 0.000 for O1WA_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 5012 / 376670 wR2 = 0.2818 before cycle 4 for 5901 data and 301 / 301 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.085; Restrained GooF = 1.085 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0584 * P )^2 + 4.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69918 0.00241 0.000 OSF 2 0.79868 0.00925 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H26A Max. dU = 0.000 for O1WB_b Largest correlation matrix elements 0.694 y H22W / x H22W -0.534 U23 O4A / U33 O4A -0.510 U23 O4B / U33 O4B 0.666 z H21W / y H21W -0.515 U23 O4A / U22 O4A Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7024 0.2635 -0.1380 13 1.000 0.000 C2 O2 C1 C3 H3 0.7618 0.1062 -0.0014 13 1.000 0.000 C3 O3 C4 C2 H2O 0.4130 0.3458 -0.0754 147 0.840 0.000 O2 C2 H2O H3O 0.5302 0.0947 0.0902 147 0.840 0.000 O3 C3 H3O H21A 0.3549 0.1897 0.4328 137 0.980 0.000 C21 C22 H21A H21B 0.5147 0.1582 0.4801 137 0.980 0.000 C21 C22 H21A H21C 0.5128 0.1052 0.3959 137 0.980 0.000 C21 C22 H21A H23A 0.5898 0.2596 0.2335 23 0.990 0.000 C23 C22 C24 H23B 0.5674 0.4114 0.2208 23 0.990 0.000 C23 C22 C24 H26A 0.7815 0.2123 0.3261 137 0.980 0.000 C26 C22 H26A H26B 0.7620 0.2723 0.4092 137 0.980 0.000 C26 C22 H26A H26C 0.7828 0.3661 0.3063 137 0.980 0.000 C26 C22 H26A H27A 0.5176 0.4979 0.3499 137 0.980 0.000 C27 C22 H27A H27B 0.5192 0.4030 0.4514 137 0.980 0.000 C27 C22 H27A H27C 0.3582 0.4221 0.4064 137 0.980 0.000 C27 C22 H27A H28A 0.1259 0.4477 0.2296 137 0.980 0.000 C28 C24 H28A H28B 0.2703 0.5194 0.2428 137 0.980 0.000 C28 C24 H28A H28C 0.1841 0.4067 0.3264 137 0.980 0.000 C28 C24 H28A H29A 0.2424 0.1726 0.3240 137 0.980 0.000 C29 C24 H29A H29B 0.3610 0.1404 0.2374 137 0.980 0.000 C29 C24 H29A H29C 0.1809 0.2127 0.2282 137 0.980 0.000 C29 C24 H29A H25A 0.4637 0.3238 0.1070 137 0.910 0.000 N25 C24 H25A H25B 0.4261 0.4611 0.1087 137 0.910 0.000 N25 C24 H25A H25C 0.2924 0.3859 0.1055 137 0.910 0.000 N25 C24 H25A H31A 1.3065 -0.1338 0.3195 137 0.980 0.000 C31 C32 H31A H31B 1.3093 -0.2880 0.3398 137 0.980 0.000 C31 C32 H31A H31C 1.2953 -0.2273 0.4221 137 0.980 0.000 C31 C32 H31A H33A 1.0874 -0.0954 0.2396 23 0.990 0.000 C33 C34 C32 H33B 1.1060 -0.2475 0.2537 23 0.990 0.000 C33 C34 C32 H36A 1.0537 -0.3478 0.4980 137 0.980 0.000 C36 C32 H36A H36B 1.0447 -0.3995 0.4143 137 0.980 0.000 C36 C32 H36A H36C 0.8883 -0.3182 0.4557 137 0.980 0.000 C36 C32 H36A H37A 0.8863 -0.0860 0.4289 137 0.980 0.000 C37 C32 H37A H37B 1.0405 -0.0071 0.3678 137 0.980 0.000 C37 C32 H37A H37C 1.0524 -0.1003 0.4687 137 0.980 0.000 C37 C32 H37A H38A 0.6909 -0.2887 0.2577 137 0.980 0.000 C38 C34 H38A H38B 0.7618 -0.3284 0.3508 137 0.980 0.000 C38 C34 H38A H38C 0.8706 -0.3637 0.2629 137 0.980 0.000 C38 C34 H38A H39A 0.6449 -0.0548 0.2534 137 0.980 0.000 C39 C34 H39A H39B 0.7937 0.0183 0.2604 137 0.980 0.000 C39 C34 H39A H39C 0.7097 -0.0900 0.3481 137 0.980 0.000 C39 C34 H39A H35A 0.9695 -0.1877 0.1291 137 0.910 0.000 N35 C34 H35A H35B 0.9436 -0.0491 0.1282 137 0.910 0.000 N35 C34 H35A H35C 0.8013 -0.1192 0.1299 137 0.910 0.000 N35 C34 H35A 07skc0009p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.51473 0.14005 -0.09459 1.00000 0.02288 0.02214 0.02606 -0.00763 -0.00734 -0.00299 0.02299 0.00599 0.00051 0.00042 0.00030 0.00000 0.00217 0.00223 0.00239 0.00184 0.00176 0.00170 0.00092 C2 0.61192 0.24150 -0.08342 1.00000 0.02106 0.02065 0.03104 -0.01065 -0.00461 -0.00294 0.02341 0.00589 0.00050 0.00040 0.00031 0.00000 0.00208 0.00220 0.00254 0.00192 0.00180 0.00168 0.00095 H2 0.70239 0.26353 -0.13801 1.00000 0.02809 0.00000 0.00000 C3 0.69273 0.18864 0.00149 1.00000 0.02103 0.02342 0.03953 -0.01580 -0.00528 0.00116 0.02677 0.00627 0.00051 0.00043 0.00032 0.00000 0.00212 0.00231 0.00281 0.00207 0.00193 0.00173 0.00101 H3 0.76179 0.10621 -0.00140 1.00000 0.03213 0.00000 0.00000 C4 0.80449 0.28898 0.00085 1.00000 0.03004 0.02309 0.04157 -0.01308 -0.01669 0.00170 0.02951 0.00646 0.00056 0.00044 0.00034 0.00000 0.00246 0.00236 0.00293 0.00214 0.00217 0.00186 0.00106 O1A 0.36102 0.16376 -0.08684 1.00000 0.02248 0.03469 0.04152 -0.01753 -0.01013 -0.00305 0.03063 0.00429 0.00036 0.00031 0.00023 0.00000 0.00159 0.00187 0.00202 0.00156 0.00137 0.00133 0.00076 O1B 0.59550 0.03968 -0.11002 1.00000 0.02495 0.02231 0.03724 -0.01170 -0.00370 -0.00260 0.02770 0.00435 0.00036 0.00029 0.00022 0.00000 0.00157 0.00162 0.00189 0.00141 0.00134 0.00125 0.00072 O2 0.51279 0.35776 -0.08045 1.00000 0.02267 0.02205 0.05271 -0.01038 -0.01229 -0.00151 0.03179 0.00448 0.00037 0.00029 0.00024 0.00000 0.00158 0.00165 0.00221 0.00153 0.00153 0.00126 0.00079 H2O 0.41303 0.34581 -0.07537 1.00000 0.04769 0.00000 0.00000 O3 0.57470 0.16286 0.08323 1.00000 0.03380 0.02375 0.03500 -0.01066 -0.00663 -0.00901 0.02962 0.00440 0.00038 0.00030 0.00022 0.00000 0.00175 0.00171 0.00188 0.00143 0.00142 0.00133 0.00074 H3O 0.53016 0.09473 0.09023 1.00000 0.04442 0.00000 0.00000 O4A 0.93367 0.30195 -0.06025 1.00000 0.02285 0.04442 0.07159 -0.03502 0.00236 -0.00981 0.04300 0.00486 0.00039 0.00035 0.00027 0.00000 0.00170 0.00217 0.00273 0.00199 0.00172 0.00150 0.00096 O4B 0.76068 0.35271 0.05623 1.00000 0.05325 0.03967 0.05204 -0.02952 -0.00439 -0.01348 0.04431 0.00487 0.00045 0.00035 0.00026 0.00000 0.00227 0.00212 0.00239 0.00189 0.00181 0.00173 0.00095 C21 0.47595 0.17762 0.42202 1.00000 0.11767 0.04522 0.03411 -0.00488 0.00969 -0.01836 0.06975 0.01097 0.00101 0.00062 0.00042 0.00000 0.00613 0.00377 0.00346 0.00290 0.00364 0.00379 0.00210 H21A 0.35488 0.18968 0.43276 1.00000 0.10463 0.00000 0.00000 H21B 0.51470 0.15821 0.48006 1.00000 0.10463 0.00000 0.00000 H21C 0.51277 0.10516 0.39591 1.00000 0.10463 0.00000 0.00000 C22 0.54702 0.30222 0.35540 1.00000 0.07071 0.03306 0.03517 -0.01322 0.00325 -0.00712 0.04728 0.00865 0.00077 0.00053 0.00037 0.00000 0.00402 0.00298 0.00317 0.00248 0.00276 0.00269 0.00145 C23 0.51984 0.32796 0.25688 1.00000 0.03770 0.02859 0.03667 -0.01134 0.00796 -0.00896 0.03557 0.00732 0.00060 0.00048 0.00034 0.00000 0.00269 0.00260 0.00293 0.00222 0.00220 0.00208 0.00117 H23A 0.58980 0.25958 0.23349 1.00000 0.04268 0.00000 0.00000 H23B 0.56738 0.41144 0.22083 1.00000 0.04268 0.00000 0.00000 C24 0.34870 0.33532 0.23067 1.00000 0.03882 0.02068 0.05841 -0.01338 0.00971 -0.00808 0.04122 0.00804 0.00063 0.00046 0.00040 0.00000 0.00282 0.00246 0.00367 0.00242 0.00249 0.00208 0.00133 C26 0.73529 0.28683 0.34864 1.00000 0.07967 0.05854 0.04456 -0.01419 -0.01962 -0.00269 0.06014 0.00939 0.00083 0.00066 0.00043 0.00000 0.00473 0.00414 0.00369 0.00313 0.00332 0.00343 0.00173 H26A 0.78145 0.21230 0.32607 1.00000 0.09021 0.00000 0.00000 H26B 0.76198 0.27229 0.40920 1.00000 0.09021 0.00000 0.00000 H26C 0.78280 0.36607 0.30631 1.00000 0.09021 0.00000 0.00000 C27 0.47938 0.41667 0.39429 1.00000 0.09931 0.04982 0.04931 -0.02482 0.00248 -0.00588 0.06623 0.01031 0.00095 0.00063 0.00045 0.00000 0.00544 0.00392 0.00396 0.00323 0.00365 0.00363 0.00194 H27A 0.51756 0.49791 0.34992 1.00000 0.09935 0.00000 0.00000 H27B 0.51925 0.40299 0.45135 1.00000 0.09935 0.00000 0.00000 H27C 0.35822 0.42209 0.40640 1.00000 0.09935 0.00000 0.00000 C28 0.22088 0.43625 0.25997 1.00000 0.04383 0.03857 0.09068 -0.03037 0.01923 -0.00514 0.05975 0.00986 0.00071 0.00056 0.00050 0.00000 0.00330 0.00332 0.00511 0.00338 0.00322 0.00258 0.00185 H28A 0.12593 0.44771 0.22956 1.00000 0.08962 0.00000 0.00000 H28B 0.27027 0.51938 0.24283 1.00000 0.08962 0.00000 0.00000 H28C 0.18410 0.40668 0.32639 1.00000 0.08962 0.00000 0.00000 C29 0.27677 0.20337 0.25749 1.00000 0.05269 0.03713 0.07339 -0.01760 0.01615 -0.02236 0.05649 0.00920 0.00075 0.00055 0.00047 0.00000 0.00352 0.00320 0.00448 0.00306 0.00312 0.00269 0.00171 H29A 0.24238 0.17259 0.32405 1.00000 0.08474 0.00000 0.00000 H29B 0.36097 0.14037 0.23745 1.00000 0.08474 0.00000 0.00000 H29C 0.18090 0.21268 0.22816 1.00000 0.08474 0.00000 0.00000 N25 0.38645 0.38107 0.12778 1.00000 0.02676 0.02441 0.05744 -0.01507 -0.00808 -0.00167 0.03545 0.00576 0.00047 0.00038 0.00030 0.00000 0.00204 0.00209 0.00296 0.00200 0.00191 0.00162 0.00101 H25A 0.46366 0.32383 0.10697 1.00000 0.05317 0.00000 0.00000 H25B 0.42608 0.46110 0.10870 1.00000 0.05317 0.00000 0.00000 H25C 0.29245 0.38595 0.10549 1.00000 0.05317 0.00000 0.00000 C31 1.26343 -0.21394 0.36298 1.00000 0.03894 0.05955 0.03959 -0.01166 -0.01766 -0.00300 0.04517 0.00785 0.00063 0.00059 0.00038 0.00000 0.00295 0.00374 0.00322 0.00277 0.00247 0.00260 0.00138 H31A 1.30649 -0.13376 0.31947 1.00000 0.06775 0.00000 0.00000 H31B 1.30933 -0.28798 0.33981 1.00000 0.06775 0.00000 0.00000 H31C 1.29534 -0.22731 0.42214 1.00000 0.06775 0.00000 0.00000 C32 1.07353 -0.20256 0.37477 1.00000 0.03280 0.03018 0.02562 -0.00744 -0.00424 -0.00354 0.02977 0.00681 0.00057 0.00046 0.00032 0.00000 0.00247 0.00253 0.00251 0.00202 0.00196 0.00196 0.00104 C33 1.03916 -0.17799 0.27713 1.00000 0.02587 0.02723 0.02929 -0.00991 -0.00993 -0.00002 0.02653 0.00620 0.00052 0.00045 0.00031 0.00000 0.00224 0.00239 0.00255 0.00199 0.00189 0.00181 0.00098 H33A 1.08744 -0.09538 0.23956 1.00000 0.03183 0.00000 0.00000 H33B 1.10601 -0.24751 0.25372 1.00000 0.03183 0.00000 0.00000 C34 0.86679 -0.16935 0.25357 1.00000 0.02501 0.02604 0.03155 -0.00900 -0.00118 -0.00269 0.02796 0.00661 0.00053 0.00044 0.00032 0.00000 0.00226 0.00240 0.00265 0.00202 0.00190 0.00182 0.00102 C36 1.00933 -0.32816 0.44165 1.00000 0.05855 0.03597 0.03546 -0.00267 -0.00970 -0.00842 0.04453 0.00819 0.00072 0.00052 0.00037 0.00000 0.00351 0.00298 0.00308 0.00242 0.00260 0.00254 0.00134 H36A 1.05366 -0.34778 0.49805 1.00000 0.06679 0.00000 0.00000 H36B 1.04467 -0.39953 0.41432 1.00000 0.06679 0.00000 0.00000 H36C 0.88826 -0.31816 0.45572 1.00000 0.06679 0.00000 0.00000 C37 1.00724 -0.08883 0.41350 1.00000 0.05986 0.03856 0.04465 -0.02126 -0.01555 -0.00349 0.04463 0.00761 0.00072 0.00053 0.00039 0.00000 0.00357 0.00309 0.00333 0.00264 0.00272 0.00261 0.00135 H37A 0.88628 -0.08600 0.42891 1.00000 0.06695 0.00000 0.00000 H37B 1.04054 -0.00715 0.36779 1.00000 0.06695 0.00000 0.00000 H37C 1.05235 -0.10034 0.46865 1.00000 0.06695 0.00000 0.00000 C38 0.79077 -0.29906 0.28396 1.00000 0.04426 0.04346 0.05045 -0.00214 -0.01473 -0.01787 0.04638 0.00782 0.00068 0.00055 0.00041 0.00000 0.00311 0.00324 0.00356 0.00269 0.00263 0.00251 0.00141 H38A 0.69089 -0.28870 0.25773 1.00000 0.06958 0.00000 0.00000 H38B 0.76183 -0.32839 0.35083 1.00000 0.06958 0.00000 0.00000 H38C 0.87059 -0.36372 0.26290 1.00000 0.06958 0.00000 0.00000 C39 0.74267 -0.06458 0.28135 1.00000 0.03216 0.06311 0.04377 -0.02129 -0.00359 0.01026 0.04700 0.00869 0.00063 0.00060 0.00039 0.00000 0.00277 0.00391 0.00335 0.00290 0.00241 0.00256 0.00144 H39A 0.64492 -0.05480 0.25343 1.00000 0.07050 0.00000 0.00000 H39B 0.79366 0.01834 0.26039 1.00000 0.07050 0.00000 0.00000 H39C 0.70975 -0.09003 0.34806 1.00000 0.07050 0.00000 0.00000 N35 0.89845 -0.12711 0.14983 1.00000 0.02359 0.03205 0.03273 -0.01307 -0.00929 -0.00159 0.02802 0.00521 0.00044 0.00038 0.00026 0.00000 0.00188 0.00216 0.00225 0.00178 0.00160 0.00157 0.00087 H35A 0.96950 -0.18774 0.12915 1.00000 0.04203 0.00000 0.00000 H35B 0.94356 -0.04908 0.12825 1.00000 0.04203 0.00000 0.00000 H35C 0.80126 -0.11920 0.12989 1.00000 0.04203 0.00000 0.00000 O1WA_a 0.82172 0.60139 0.00465 0.79868 0.03472 0.03484 0.11887 -0.03072 -0.02779 0.00195 0.05918 0.00696 0.00056 0.00046 0.00043 0.00925 0.00269 0.00282 0.00546 0.00304 0.00284 0.00204 0.00201 O1WB_b 0.79907 0.54719 0.12115 0.20132 0.02596 0.01456 0.04878 -0.01432 0.00179 0.00246 0.03035 0.02311 0.00180 0.00138 0.00116 0.00925 0.00849 0.00793 0.01182 0.00734 0.00708 0.00593 0.00528 O2W 0.09553 0.08571 0.08744 1.00000 0.02663 0.03254 0.04959 -0.00654 -0.00663 0.00066 0.03793 0.00541 0.00040 0.00034 0.00025 0.00000 0.00174 0.00201 0.00237 0.00167 0.00159 0.00145 0.00087 H21W 0.09880 0.15286 0.04241 1.00000 0.05689 0.08820 0.00619 0.00358 0.00280 0.00000 0.00000 H22W 0.18936 0.04637 0.08432 1.00000 0.05689 0.08569 0.00376 0.00451 0.00359 0.00000 0.00000 Final Structure Factor Calculation for 07skc0009p-1 in P-1 Total number of l.s. parameters = 301 Maximum vector length = 511 Memory required = 4711 / 22995 wR2 = 0.2818 before cycle 5 for 5901 data and 0 / 301 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.085; Restrained GooF = 1.085 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0584 * P )^2 + 4.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1202 for 3285 Fo > 4sig(Fo) and 0.2055 for all 5901 data wR2 = 0.2818, GooF = S = 1.085, Restrained GooF = 1.085 for all data Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 46.00 for hydrogen atoms Principal mean square atomic displacements U 0.0274 0.0231 0.0185 C1 0.0313 0.0217 0.0171 C2 0.0405 0.0223 0.0175 C3 0.0462 0.0222 0.0202 C4 0.0440 0.0300 0.0179 O1A 0.0380 0.0249 0.0202 O1B 0.0538 0.0220 0.0196 O2 0.0366 0.0350 0.0172 O3 0.0807 0.0290 0.0193 O4A 0.0664 0.0488 0.0178 O4B 0.1293 0.0512 0.0287 C21 0.0780 0.0345 0.0293 C22 0.0551 0.0279 0.0237 C23 0.0744 0.0311 0.0181 C24 0.0807 0.0593 0.0405 C26 0.1081 0.0559 0.0347 C27 0.1137 0.0387 0.0268 C28 0.0985 0.0481 0.0228 C29 0.0578 0.0264 0.0222 N25 0.0614 0.0481 0.0259 C31 0.0332 0.0305 0.0256 C32 0.0326 0.0260 0.0211 C33 0.0344 0.0257 0.0238 C34 0.0592 0.0447 0.0296 C36 0.0613 0.0470 0.0256 C37 0.0694 0.0418 0.0279 C38 0.0702 0.0451 0.0257 C39 0.0357 0.0285 0.0198 N35 0.1195 0.0304 0.0277 O1WA_a 0.0540 0.0270 0.0100 O1WB_b 0.0548 0.0336 0.0254 O2W 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 0.027 0.036 0.046 0.060 0.082 0.120 1.000 Number in group 673. 549. 622. 541. 620. 545. 593. 586. 578. 594. GooF 1.135 1.083 1.133 1.109 1.121 1.111 1.058 1.011 0.947 1.120 K 23.368 3.324 2.142 1.316 1.174 1.072 1.070 1.024 1.010 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 610. 583. 592. 580. 587. 590. 599. 580. 589. 591. GooF 1.186 1.151 1.160 1.121 1.027 0.978 0.983 0.920 0.913 1.334 K 1.451 1.323 1.267 1.142 1.114 1.046 0.990 0.994 1.026 1.018 R1 0.448 0.415 0.379 0.334 0.296 0.196 0.144 0.117 0.085 0.073 Recommended weighting scheme: WGHT 0.0584 4.9690 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) 1 1 2 463.28 212.97 5.21 0.110 6.02 1 1 0 532.67 971.11 5.11 0.236 6.62 -1 1 1 316.34 584.55 4.36 0.183 5.72 1 1 1 3832.36 5527.20 4.06 0.562 6.98 -1 1 0 217.31 401.34 3.76 0.152 6.12 -1 0 1 477.71 759.79 3.76 0.208 6.59 -5 -5 8 135.52 25.86 3.40 0.038 0.93 1 3 2 440.46 275.58 3.36 0.126 3.45 1 11 16 156.92 21.59 3.26 0.035 0.79 5 -9 3 67.32 5.74 3.18 0.018 0.86 -8 4 9 -22.17 44.11 3.18 0.050 0.78 2 2 4 50.03 4.65 3.18 0.016 3.01 6 3 17 60.31 0.01 3.16 0.001 0.83 -2 -4 2 198.46 104.85 3.09 0.077 1.96 -2 0 11 72.10 7.87 3.08 0.021 1.20 10 0 5 69.30 0.40 3.03 0.005 0.82 -6 3 3 199.69 335.55 3.02 0.139 1.17 1 2 1 45.91 116.60 2.98 0.082 4.82 8 -5 5 66.41 0.76 2.96 0.007 0.85 -3 10 5 46.65 0.18 2.93 0.003 0.95 8 3 14 58.22 0.54 2.93 0.006 0.84 2 1 14 103.78 34.39 2.87 0.044 1.09 -1 -5 13 154.83 43.65 2.87 0.050 0.87 2 9 16 118.26 14.94 2.85 0.029 0.87 5 5 4 54.65 14.68 2.80 0.029 1.41 2 2 0 748.08 1011.63 2.80 0.241 3.31 5 -6 12 84.22 14.75 2.79 0.029 0.80 3 -6 12 -25.13 32.88 2.77 0.043 0.86 1 0 17 71.50 7.49 2.77 0.021 0.87 1 3 19 60.55 1.33 2.77 0.009 0.82 2 -4 16 55.52 4.54 2.72 0.016 0.80 0 -8 4 213.04 353.16 2.71 0.142 1.11 10 4 11 40.25 0.11 2.70 0.002 0.78 4 8 19 88.16 3.20 2.70 0.014 0.78 0 12 11 87.14 16.17 2.69 0.030 0.84 -6 6 13 73.03 13.85 2.67 0.028 0.77 1 -10 2 89.38 26.72 2.67 0.039 0.96 2 -2 17 -24.15 29.12 2.67 0.041 0.82 8 -3 11 69.00 0.21 2.66 0.003 0.81 -2 -12 3 212.25 114.24 2.64 0.081 0.80 0 1 4 72.03 147.30 2.64 0.092 3.82 5 -10 3 45.32 0.02 2.64 0.001 0.81 4 7 14 178.56 76.66 2.63 0.066 0.99 1 1 5 3471.41 2809.67 2.63 0.401 3.09 9 1 7 54.09 0.90 2.63 0.007 0.90 1 5 7 4.47 44.40 2.62 0.050 1.79 5 -1 2 93.88 40.48 2.62 0.048 1.59 5 7 15 55.73 0.57 2.61 0.006 0.92 -1 5 6 682.83 499.45 2.61 0.169 1.74 1 -4 15 40.73 2.00 2.58 0.011 0.84 Bond lengths and angles C1 - Distance Angles O1A 1.2531 (0.0050) O1B 1.2585 (0.0051) 125.73 (0.40) C2 1.5270 (0.0057) 116.95 (0.37) 117.31 (0.36) C1 - O1A O1B C2 - Distance Angles O2 1.4132 (0.0050) C1 1.5270 (0.0057) 112.12 (0.33) C3 1.5303 (0.0062) 109.85 (0.35) 111.80 (0.35) H2 1.0000 107.62 107.62 107.62 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4118 (0.0054) C4 1.5252 (0.0062) 109.51 (0.36) C2 1.5303 (0.0062) 112.18 (0.34) 108.36 (0.37) H3 1.0000 108.91 108.91 108.91 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2390 (0.0056) O4A 1.2668 (0.0058) 125.93 (0.43) C3 1.5252 (0.0062) 118.85 (0.43) 115.18 (0.40) C4 - O4B O4A O1A - Distance Angles C1 1.2531 (0.0050) O1A - O1B - Distance Angles C1 1.2585 (0.0051) O1B - O2 - Distance Angles C2 1.4132 (0.0050) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4118 (0.0054) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2668 (0.0058) O4A - O4B - Distance Angles C4 1.2390 (0.0056) O4B - C21 - Distance Angles C22 1.5301 (0.0080) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C21 1.5301 (0.0079) C26 1.5330 (0.0087) 108.42 (0.54) C27 1.5369 (0.0077) 108.94 (0.49) 107.70 (0.53) C23 1.5400 (0.0076) 113.54 (0.50) 104.96 (0.44) 112.96 (0.50) C22 - C21 C26 C27 C23 - Distance Angles C22 1.5400 (0.0077) C24 1.5469 (0.0074) 124.04 (0.44) H23A 0.9900 106.32 106.32 H23B 0.9900 106.32 106.32 106.42 C23 - C22 C24 H23A C24 - Distance Angles N25 1.5055 (0.0070) C28 1.5214 (0.0070) 106.27 (0.46) C29 1.5306 (0.0069) 106.49 (0.46) 111.03 (0.44) C23 1.5469 (0.0074) 102.85 (0.37) 115.07 (0.48) 114.09 (0.46) C24 - N25 C28 C29 C26 - Distance Angles C22 1.5330 (0.0087) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C22 1.5369 (0.0077) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B C28 - Distance Angles C24 1.5214 (0.0070) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5306 (0.0069) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5055 (0.0070) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles C32 1.5398 (0.0067) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C32 H31A H31B C32 - Distance Angles C36 1.5194 (0.0068) C37 1.5268 (0.0068) 109.84 (0.43) C31 1.5398 (0.0067) 108.68 (0.42) 107.68 (0.42) C33 1.5497 (0.0063) 113.08 (0.40) 112.72 (0.40) 104.52 (0.37) C32 - C36 C37 C31 C33 - Distance Angles C34 1.5367 (0.0060) C32 1.5497 (0.0063) 124.73 (0.38) H33A 0.9900 106.14 106.14 H33B 0.9900 106.14 106.14 106.35 C33 - C34 C32 H33A C34 - Distance Angles N35 1.5174 (0.0059) C38 1.5201 (0.0067) 106.17 (0.39) C39 1.5268 (0.0066) 105.45 (0.38) 110.85 (0.42) C33 1.5367 (0.0060) 103.74 (0.33) 114.18 (0.40) 115.35 (0.40) C34 - N35 C38 C39 C36 - Distance Angles C32 1.5194 (0.0068) H36A 0.9800 109.47 H36B 0.9800 109.47 109.47 H36C 0.9800 109.47 109.47 109.47 C36 - C32 H36A H36B C37 - Distance Angles C32 1.5268 (0.0068) H37A 0.9800 109.47 H37B 0.9800 109.47 109.47 H37C 0.9800 109.47 109.47 109.47 C37 - C32 H37A H37B C38 - Distance Angles C34 1.5201 (0.0067) H38A 0.9800 109.47 H38B 0.9800 109.47 109.47 H38C 0.9800 109.47 109.47 109.47 C38 - C34 H38A H38B C39 - Distance Angles C34 1.5268 (0.0066) H39A 0.9800 109.47 H39B 0.9800 109.47 109.47 H39C 0.9800 109.47 109.47 109.47 C39 - C34 H39A H39B N35 - Distance Angles C34 1.5174 (0.0059) H35A 0.9100 109.47 H35B 0.9100 109.47 109.47 H35C 0.9100 109.47 109.47 109.47 N35 - C34 H35A H35B O2W - Distance Angles H21W 0.8385 (0.0189) H22W 0.8330 (0.0189) 107.57 (3.01) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.15 2.642(4) 117.1 O2-H2O...O1A 0.91 1.96 2.839(5) 161.7 N25-H25A...O3 0.91 2.46 3.076(5) 125.5 N25-H25A...O4B 0.839(19) 2.62(5) 3.087(5) 116(4) O2W-H21W...O1A 0.84 2.10 2.777(16) 137.7 O2-H2O...O1WB_$1b 0.84 2.12 2.809(6) 138.5 O2-H2O...O1WA_$1a 0.91 1.99 2.894(5) 171.9 N25-H25B...O2_$1 0.91 2.10 2.920(7) 149.3 N25-H25C...O1WA_$1a 0.84 1.82 2.657(4) 171.5 O3-H3O...O1B_$2 0.91 1.81 2.680(5) 158.3 N35-H35C...O1A_$2 0.833(19) 1.96(2) 2.766(4) 164(6) O2W-H22W...O1B_$2 0.91 1.88 2.757(5) 161.1 N35-H35A...O4A_$3 0.91 1.93 2.818(5) 164.0 N35-H35B...O2W_$4 0.839(19) 2.40(3) 3.112(5) 143(5) O2W-H21W...O4A_$5 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 0.4200 (0.0493) x + 1.7803 (0.0792) y - 13.7768 (0.0611) z = 1.3363 (0.0265) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 4.7360 (0.0554) x - 4.5986 (0.0832) y + 9.0373 (0.0541) z = 2.4888 (0.0718) Angle to previous plane (with approximate esd) = 41.37 ( 0.55 ) * 0.0000 (0.0000) C4 * 0.0000 (0.0000) O4A * 0.0000 (0.0000) O4B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 39 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.2054 for 5901 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.76 at 0.0222 0.4165 0.1320 [ 2.04 A from H28A ] Deepest hole -0.31 at 0.2464 0.0198 0.1035 [ 0.60 A from H22W ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4402 / 27066 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0222 0.4165 0.1320 1.00000 0.05 1.76 2.04 H28A 2.17 O1WB 2.19 H25C 2.30 O1WA Q2 1 0.8664 0.6248 -0.0609 1.00000 0.05 0.52 0.98 O1WA 1.65 H25C 2.56 N25 2.58 H21W Q3 1 0.8186 0.5229 0.0284 1.00000 0.05 0.41 0.82 O1WA 1.53 O1WB 1.87 O4B 2.34 H25C Q4 1 0.8813 0.6215 0.0448 1.00000 0.05 0.32 0.97 O1WA 1.32 O1WB 1.94 O4A 2.39 H2O Q5 1 0.5023 0.0602 -0.1110 1.00000 0.05 0.32 0.78 O1B 1.00 C1 1.58 O1A 1.66 H3O Q6 1 0.9362 0.6141 -0.0098 1.00000 0.05 0.31 0.95 O1WA 2.08 O1WB 2.15 O4A 2.41 H21W Q7 1 0.7983 0.4836 0.0849 1.00000 0.05 0.29 1.02 O1WB 1.49 O1WA 1.70 O4B 2.36 H2O Q8 1 0.0452 0.0564 0.0285 1.00000 0.05 0.27 1.23 O2W 1.29 H21W 1.60 H22W 1.75 H35B Q9 1 0.2990 0.0854 0.3112 1.00000 0.05 0.26 1.05 H29A 1.16 H29B 1.31 C29 1.90 H29C Q10 1 0.5877 -0.0191 -0.1120 1.00000 0.05 0.25 0.66 O1B 1.29 H3O 1.83 C1 1.95 H22W Shortest distances between peaks (including symmetry equivalents) 3 7 0.84 4 6 0.90 5 10 1.04 2 6 1.05 3 4 1.37 3 6 1.39 1 2 1.43 2 3 1.50 4 7 1.62 2 4 1.68 6 7 1.98 1 6 2.00 8 8 2.02 1 7 2.10 2 7 2.32 3 6 2.37 1 4 2.49 6 6 2.50 1 3 2.50 1 3 2.51 6 7 2.52 1 6 2.70 1 4 2.86 2 7 2.86 2 6 2.90 2 3 2.92 4 6 2.93 3 4 2.96 3 3 2.97 Time profile in seconds ----------------------- 0.09: 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 0.02: Analyse other restraints etc. 0.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.50: Structure factors and derivatives 3.48: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0009p-1 finished at 15:22:32 Total CPU time: 6.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++