+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0075p-1 started at 13:19:32 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0075p-1 in P-1 CELL 0.71073 10.0617 10.7224 12.7612 90.665 105.835 99.831 ZERR 2.00 0.0006 0.0006 0.0008 0.003 0.003 0.003 LATT 1 SFAC C H N O S UNIT 44 60 8 18 6 V = 1302.59 F(000) = 620.0 Mu = 0.34 mm-1 Cell Wt = 1181.36 Rho = 1.506 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N42 O31A HTAB N42 S31 HTAB N2 O1C HTAB N32 O31C HTAB N42 O41B HTAB N42 S41 EQIV_$1 x, y-1, z HTAB N2 O41C_$1 HTAB N21 O41A_$1 EQIV_$2 -x+1, -y+1, -z+1 HTAB N2 O31A_$2 HTAB N21 O31C_$2 HTAB N42 O1A_$2 HTAB N42 O31B_$2 EQIV_$3 x+1, y, z HTAB N21 O1A_$3 EQIV_$4 -x+2, -y+1, -z+1 HTAB N21 O41B_$4 EQIV_$5 x, y+1, z HTAB N32 N2_$5 HTAB N32 O1A_$5 EQIV_$6 x-1, y, z HTAB N32 O41B_$6 HTAB N32 O41A_$6 HTAB N32 S41_$6 EQIV_$7 -x+1, -y+2, -z+1 HTAB N32 O41C_$7 SIZE 0.14 0.09 0.02 FMAP 2 PLAN 10 ACTA BOND $H WGHT 0.00000 6.81530 L.S. 4 TEMP -153.00 FVAR 0.58909 MOLE 1 C1 1 0.296750 0.111156 0.169443 11.00000 0.03078 0.01810 = 0.02131 -0.00020 0.00843 0.00469 C2 1 0.391489 0.034988 0.224999 11.00000 0.02097 0.01803 = 0.02844 0.00161 0.01027 0.00101 C3 1 0.423142 -0.060186 0.163849 11.00000 0.02619 0.02356 = 0.03909 0.00025 0.01522 0.00927 AFIX 43 H3 2 0.486276 -0.112967 0.199594 11.00000 -1.20000 AFIX 0 C4 1 0.363790 -0.077574 0.053136 11.00000 0.05743 0.02973 = 0.03287 -0.00094 0.02394 0.01225 AFIX 43 H4 2 0.386035 -0.142681 0.013341 11.00000 -1.20000 AFIX 0 C5 1 0.272355 -0.002087 -0.001346 11.00000 0.08749 0.02852 = 0.01631 -0.00039 0.01150 0.02320 AFIX 43 H5 2 0.232298 -0.014402 -0.078095 11.00000 -1.20000 AFIX 0 C6 1 0.240114 0.091256 0.057185 11.00000 0.05308 0.02518 = 0.02279 0.00236 0.00403 0.01901 AFIX 43 H6 2 0.177408 0.143540 0.019822 11.00000 -1.20000 AFIX 0 N2 3 0.443747 0.045222 0.337962 11.00000 0.02398 0.01956 = 0.02680 -0.00063 0.00305 0.00932 AFIX 93 H2A 2 0.496700 -0.007845 0.371345 11.00000 -1.20000 H2B 2 0.423900 0.104772 0.376143 11.00000 -1.20000 AFIX 0 O1A 4 0.160874 0.162072 0.305023 11.00000 0.02982 0.01920 = 0.04192 0.00392 0.02119 0.00504 O1B 4 0.166882 0.301634 0.157810 11.00000 0.05401 0.02635 = 0.02241 0.00351 0.00204 0.02314 O1C 4 0.373816 0.303921 0.309771 11.00000 0.02499 0.02016 = 0.02931 -0.00528 0.00494 -0.00129 S1 5 0.245717 0.229897 0.239357 11.00000 0.02478 0.01324 = 0.01989 -0.00011 0.00580 0.00498 MOLE 2 C22 1 0.986039 0.381441 0.353849 11.00000 0.02871 0.02498 = 0.05524 0.00303 0.02259 0.00531 AFIX 23 H22A 2 1.073493 0.396023 0.330836 11.00000 -1.20000 H22B 2 1.008937 0.408768 0.432075 11.00000 -1.20000 AFIX 0 C23 1 0.878263 0.452721 0.284985 11.00000 0.04182 0.02983 = 0.07995 0.01693 0.02595 0.01176 AFIX 23 H23A 2 0.812984 0.473369 0.325502 11.00000 -1.20000 H23B 2 0.924203 0.531923 0.260790 11.00000 -1.20000 AFIX 0 C24 1 0.804088 0.359754 0.190802 11.00000 0.12114 0.09506 = 0.04746 0.02623 0.01693 0.07741 AFIX 23 H24A 2 0.710538 0.379197 0.153632 11.00000 -1.20000 H24B 2 0.859401 0.361030 0.137345 11.00000 -1.20000 AFIX 0 C25 1 0.790259 0.234519 0.239383 11.00000 0.08645 0.04275 = 0.04630 -0.01294 -0.02999 0.02754 AFIX 23 H25A 2 0.787453 0.165694 0.186005 11.00000 -1.20000 H25B 2 0.703678 0.217197 0.263470 11.00000 -1.20000 AFIX 0 N21 3 0.917199 0.244922 0.334104 11.00000 0.02637 0.02197 = 0.02397 0.00144 0.00957 0.01116 AFIX 23 H21A 2 0.978118 0.196716 0.319444 11.00000 -1.20000 H21B 2 0.892233 0.216086 0.394918 11.00000 -1.20000 AFIX 0 MOLE 3 C31 1 0.211559 0.696077 0.306758 11.00000 0.01566 0.01977 = 0.02324 0.00281 0.01107 -0.00055 C32 1 0.152943 0.803758 0.277620 11.00000 0.01686 0.01807 = 0.02463 0.00068 0.00793 0.00063 C33 1 0.076310 0.816691 0.172315 11.00000 0.02016 0.02201 = 0.02443 0.00376 0.00327 0.00429 AFIX 43 H33 2 0.033630 0.888999 0.154246 11.00000 -1.20000 AFIX 0 C34 1 0.062574 0.721245 0.092502 11.00000 0.02651 0.03568 = 0.02294 -0.00627 0.00175 0.00882 AFIX 43 H34 2 0.010396 0.728460 0.019282 11.00000 -1.20000 AFIX 0 C35 1 0.125000 0.616184 0.120137 11.00000 0.02444 0.02455 = 0.02683 -0.01140 0.00564 0.00173 AFIX 43 H35 2 0.117088 0.552419 0.065354 11.00000 -1.20000 AFIX 0 C36 1 0.199183 0.603319 0.227474 11.00000 0.02265 0.01582 = 0.02986 -0.00184 0.00666 0.00120 AFIX 43 H36 2 0.241185 0.530724 0.246011 11.00000 -1.20000 AFIX 0 N32 3 0.175000 0.908226 0.360445 11.00000 0.02246 0.01399 = 0.01917 0.00258 0.00646 0.00401 AFIX 137 H32A 2 0.265865 0.949168 0.377488 11.00000 -1.50000 H32B 2 0.155792 0.876157 0.421489 11.00000 -1.50000 H32C 2 0.116933 0.963729 0.333399 11.00000 -1.50000 AFIX 0 O31A 4 0.428173 0.781144 0.467534 11.00000 0.02468 0.01819 = 0.02287 -0.00178 -0.00141 0.00492 O31B 4 0.339584 0.555245 0.450156 11.00000 0.03245 0.01912 = 0.03266 0.00715 0.00850 0.00907 O31C 4 0.209086 0.701825 0.506873 11.00000 0.03828 0.04704 = 0.03058 0.01337 0.01958 0.02450 S31 5 0.303960 0.681067 0.444542 11.00000 0.02467 0.01724 = 0.02148 0.00366 0.00744 0.00745 MOLE 4 C41 1 0.717855 0.761320 0.302332 11.00000 0.01722 0.02004 = 0.01954 -0.00081 0.00441 0.00467 C42 1 0.647830 0.671909 0.355595 11.00000 0.01737 0.02018 = 0.01918 0.00248 0.00557 0.00494 C43 1 0.556614 0.566890 0.298868 11.00000 0.01558 0.01925 = 0.03003 0.00027 0.00634 0.00051 AFIX 43 H43 2 0.511307 0.504950 0.336467 11.00000 -1.20000 AFIX 0 C44 1 0.531483 0.552201 0.187399 11.00000 0.02982 0.02711 = 0.02604 -0.00608 0.00550 0.00248 AFIX 43 H44 2 0.465621 0.481761 0.147791 11.00000 -1.20000 AFIX 0 C45 1 0.601520 0.639359 0.132664 11.00000 0.03209 0.03324 = 0.02299 -0.00378 0.00708 0.00517 AFIX 43 H45 2 0.586047 0.627760 0.056074 11.00000 -1.20000 AFIX 0 C46 1 0.695069 0.744416 0.191153 11.00000 0.02235 0.02694 = 0.02482 0.00337 0.01131 0.00537 AFIX 43 H46 2 0.743378 0.804691 0.154119 11.00000 -1.20000 AFIX 0 N42 3 0.666294 0.687535 0.472649 11.00000 0.02259 0.01580 = 0.02378 0.00311 0.00582 0.00226 AFIX 137 H42A 2 0.751055 0.737150 0.504884 11.00000 -1.50000 H42B 2 0.662712 0.610252 0.501546 11.00000 -1.50000 H42C 2 0.596639 0.724953 0.484570 11.00000 -1.50000 AFIX 0 O41A 4 0.894791 0.966131 0.297867 11.00000 0.02345 0.01709 = 0.02887 0.00464 0.01081 0.00248 O41B 4 0.934645 0.846506 0.461679 11.00000 0.01856 0.02113 = 0.02599 0.00474 -0.00113 0.00254 O41C 4 0.745810 0.967896 0.419457 11.00000 0.02443 0.02230 = 0.02773 -0.00513 0.00731 0.00486 S41 5 0.833487 0.898594 0.376033 11.00000 0.01875 0.01472 = 0.02077 0.00061 0.00530 0.00214 HKLF 4 Covalent radii and connectivity table for 06skc0075p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C6 C2 S1 C2 - N2 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 N2 - C2 O1A - S1 O1B - S1 O1C - S1 S1 - O1B O1C O1A C1 C22 - N21 C23 C23 - C24 C22 C24 - C25 C23 C25 - C24 N21 N21 - C25 C22 C31 - C36 C32 S31 C32 - C33 C31 N32 C33 - C32 C34 C34 - C35 C33 C35 - C34 C36 C36 - C31 C35 N32 - C32 O31A - S31 O31B - S31 O31C - S31 S31 - O31C O31B O31A C31 C41 - C46 C42 S41 C42 - C43 C41 N42 C43 - C44 C42 C44 - C43 C45 C45 - C44 C46 C46 - C41 C45 N42 - C42 O41A - S41 O41B - S41 O41C - S41 S41 - O41A O41C O41B C41 Operators for generating equivalent atoms: $1 x, y-1, z $2 -x+1, -y+1, -z+1 $3 x+1, y, z $4 -x+2, -y+1, -z+1 $5 x, y+1, z $6 x-1, y, z $7 -x+1, -y+2, -z+1 33645 Reflections read, of which 235 rejected -13 =< h =< 13, -13 =< k =< 13, -16 =< l =< 16, 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) 8 1 0 35.98 11.14 2 55.83 -8 -9 1 -16.88 7.10 3 51.35 10 2 1 37.95 11.25 2 85.75 -7 -9 2 -0.67 5.05 3 28.76 -7 -7 2 40.29 11.25 2 96.71 7 8 2 0.72 5.17 4 28.50 -10 -6 3 -4.18 5.96 3 31.18 -9 -7 4 -11.09 4.78 4 27.39 -11 -1 5 3.43 6.63 2 51.61 -8 -8 6 -11.75 5.49 4 36.60 -7 -6 6 -8.90 4.37 4 22.83 -6 -9 7 6.82 6.97 2 47.89 -10 -5 7 3.64 5.85 4 40.67 -8 -7 8 18.92 8.31 4 45.51 0 -3 8 -5.63 7.67 2 39.28 -11 -2 8 26.21 6.29 3 34.78 -9 -5 9 22.09 7.37 4 38.55 -10 -3 10 6.47 5.18 4 31.72 -8 -7 11 117.67 14.66 2 89.16 -6 -4 11 6.86 6.88 4 35.49 -8 -3 11 -2.68 4.47 5 24.02 21 Inconsistent equivalents 5944 Unique reflections, of which 0 suppressed R(int) = 0.1208 R(sigma) = 0.0957 Friedel opposites merged Maximum memory for data reduction = 4051 / 59211 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 = 5032 / 436982 wR2 = 0.1711 before cycle 1 for 5944 data and 345 / 345 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58909 0.00118 0.003 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U11 S41 Max. shift = 0.000 A for H32C Max. dU = 0.000 for C45 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5032 / 436982 wR2 = 0.1711 before cycle 2 for 5944 data and 345 / 345 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58909 0.00118 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 S41 Max. shift = 0.000 A for H32C Max. dU = 0.000 for C45 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5032 / 436982 wR2 = 0.1711 before cycle 3 for 5944 data and 345 / 345 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58909 0.00118 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H32C Max. dU = 0.000 for C46 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5032 / 436982 wR2 = 0.1711 before cycle 4 for 5944 data and 345 / 345 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58909 0.00118 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S41 Max. shift = 0.000 A for H32A Max. dU = 0.000 for C24 Largest correlation matrix elements 0.621 U12 C24 / U11 C24 0.620 U12 C24 / U22 C24 0.569 U13 C24 / U23 C24 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.4863 -0.1130 0.1996 43 0.950 0.000 C3 C4 C2 H4 0.3860 -0.1427 0.0133 43 0.950 0.000 C4 C3 C5 H5 0.2323 -0.0144 -0.0781 43 0.950 0.000 C5 C6 C4 H6 0.1774 0.1435 0.0198 43 0.950 0.000 C6 C5 C1 H2A 0.4967 -0.0078 0.3713 93 0.880 0.000 N2 C2 C3 H2B 0.4239 0.1048 0.3761 93 0.880 0.000 N2 C2 C3 H22A 1.0735 0.3960 0.3308 23 0.990 0.000 C22 N21 C23 H22B 1.0089 0.4088 0.4321 23 0.990 0.000 C22 N21 C23 H23A 0.8130 0.4734 0.3255 23 0.990 0.000 C23 C24 C22 H23B 0.9242 0.5319 0.2608 23 0.990 0.000 C23 C24 C22 H24A 0.7105 0.3792 0.1536 23 0.990 0.000 C24 C25 C23 H24B 0.8594 0.3610 0.1373 23 0.990 0.000 C24 C25 C23 H25A 0.7875 0.1657 0.1860 23 0.990 0.000 C25 C24 N21 H25B 0.7037 0.2172 0.2635 23 0.990 0.000 C25 C24 N21 H21A 0.9781 0.1967 0.3194 23 0.920 0.000 N21 C25 C22 H21B 0.8922 0.2161 0.3949 23 0.920 0.000 N21 C25 C22 H33 0.0336 0.8890 0.1542 43 0.950 0.000 C33 C32 C34 H34 0.0104 0.7285 0.0193 43 0.950 0.000 C34 C35 C33 H35 0.1171 0.5524 0.0654 43 0.950 0.000 C35 C34 C36 H36 0.2412 0.5307 0.2460 43 0.950 0.000 C36 C31 C35 H32A 0.2659 0.9492 0.3775 137 0.910 0.000 N32 C32 H32A H32B 0.1558 0.8762 0.4215 137 0.910 0.000 N32 C32 H32A H32C 0.1169 0.9637 0.3334 137 0.910 0.000 N32 C32 H32A H43 0.5113 0.5049 0.3365 43 0.950 0.000 C43 C44 C42 H44 0.4656 0.4818 0.1478 43 0.950 0.000 C44 C43 C45 H45 0.5860 0.6278 0.0561 43 0.950 0.000 C45 C44 C46 H46 0.7434 0.8047 0.1541 43 0.950 0.000 C46 C41 C45 H42A 0.7511 0.7372 0.5049 137 0.910 0.000 N42 C42 H42A H42B 0.6627 0.6103 0.5015 137 0.910 0.000 N42 C42 H42A H42C 0.5966 0.7250 0.4846 137 0.910 0.000 N42 C42 H42A 06skc0075p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.29675 0.11116 0.16944 1.00000 0.03078 0.01810 0.02131 -0.00020 0.00843 0.00469 0.02314 0.00979 0.00052 0.00043 0.00038 0.00000 0.00271 0.00220 0.00244 0.00183 0.00207 0.00197 0.00103 C2 0.39149 0.03499 0.22500 1.00000 0.02097 0.01803 0.02844 0.00161 0.01027 0.00101 0.02211 0.00971 0.00049 0.00042 0.00040 0.00000 0.00242 0.00218 0.00261 0.00190 0.00204 0.00188 0.00101 C3 0.42314 -0.06019 0.16385 1.00000 0.02619 0.02356 0.03909 0.00025 0.01522 0.00927 0.02782 0.01065 0.00053 0.00046 0.00044 0.00000 0.00267 0.00245 0.00306 0.00218 0.00232 0.00210 0.00113 H3 0.48628 -0.11297 0.19959 1.00000 0.03338 0.00000 0.00000 C4 0.36379 -0.07757 0.05314 1.00000 0.05743 0.02973 0.03287 -0.00094 0.02394 0.01225 0.03723 0.01221 0.00065 0.00051 0.00045 0.00000 0.00389 0.00280 0.00303 0.00234 0.00283 0.00269 0.00135 H4 0.38603 -0.14268 0.01334 1.00000 0.04467 0.00000 0.00000 C5 0.27236 -0.00209 -0.00135 1.00000 0.08749 0.02852 0.01631 -0.00039 0.01150 0.02320 0.04316 0.01277 0.00074 0.00051 0.00043 0.00000 0.00496 0.00278 0.00255 0.00212 0.00285 0.00305 0.00161 H5 0.23230 -0.01440 -0.07809 1.00000 0.05179 0.00000 0.00000 C6 0.24011 0.09126 0.05718 1.00000 0.05308 0.02518 0.02279 0.00236 0.00403 0.01901 0.03353 0.01116 0.00062 0.00048 0.00041 0.00000 0.00363 0.00257 0.00264 0.00207 0.00247 0.00251 0.00130 H6 0.17741 0.14354 0.01982 1.00000 0.04023 0.00000 0.00000 N2 0.44375 0.04522 0.33796 1.00000 0.02398 0.01956 0.02680 -0.00063 0.00305 0.00932 0.02361 0.00792 0.00041 0.00036 0.00032 0.00000 0.00214 0.00192 0.00219 0.00163 0.00174 0.00167 0.00089 H2A 0.49670 -0.00784 0.37135 1.00000 0.02833 0.00000 0.00000 H2B 0.42390 0.10477 0.37614 1.00000 0.02833 0.00000 0.00000 O1A 0.16087 0.16207 0.30502 1.00000 0.02982 0.01920 0.04192 0.00392 0.02119 0.00504 0.02799 0.00728 0.00036 0.00030 0.00029 0.00000 0.00195 0.00165 0.00218 0.00150 0.00169 0.00145 0.00080 O1B 0.16688 0.30163 0.15781 1.00000 0.05401 0.02635 0.02241 0.00351 0.00204 0.02314 0.03402 0.00762 0.00041 0.00032 0.00028 0.00000 0.00248 0.00183 0.00185 0.00146 0.00171 0.00175 0.00091 O1C 0.37382 0.30392 0.30977 1.00000 0.02499 0.02016 0.02931 -0.00528 0.00494 -0.00129 0.02606 0.00653 0.00035 0.00030 0.00028 0.00000 0.00182 0.00163 0.00189 0.00139 0.00149 0.00139 0.00077 S1 0.24572 0.22990 0.23936 1.00000 0.02478 0.01324 0.01989 -0.00011 0.00580 0.00498 0.01921 0.00234 0.00012 0.00010 0.00009 0.00000 0.00061 0.00050 0.00057 0.00041 0.00047 0.00044 0.00026 C22 0.98604 0.38144 0.35385 1.00000 0.02871 0.02498 0.05524 0.00303 0.02259 0.00531 0.03407 0.01178 0.00056 0.00047 0.00050 0.00000 0.00287 0.00260 0.00369 0.00246 0.00268 0.00223 0.00128 H22A 1.07349 0.39602 0.33084 1.00000 0.04088 0.00000 0.00000 H22B 1.00894 0.40877 0.43208 1.00000 0.04088 0.00000 0.00000 C23 0.87826 0.45272 0.28498 1.00000 0.04182 0.02983 0.07995 0.01693 0.02594 0.01176 0.04798 0.01406 0.00065 0.00055 0.00059 0.00000 0.00362 0.00302 0.00505 0.00316 0.00348 0.00271 0.00168 H23A 0.81298 0.47337 0.32550 1.00000 0.05758 0.00000 0.00000 H23B 0.92420 0.53192 0.26079 1.00000 0.05758 0.00000 0.00000 C24 0.80409 0.35975 0.19080 1.00000 0.12114 0.09506 0.04746 0.02623 0.01694 0.07741 0.08195 0.01975 0.00102 0.00081 0.00062 0.00000 0.00763 0.00642 0.00451 0.00442 0.00476 0.00603 0.00290 H24A 0.71054 0.37920 0.15363 1.00000 0.09834 0.00000 0.00000 H24B 0.85940 0.36103 0.13734 1.00000 0.09834 0.00000 0.00000 C25 0.79026 0.23452 0.23938 1.00000 0.08645 0.04275 0.04630 -0.01294 -0.02999 0.02754 0.06640 0.01325 0.00085 0.00061 0.00055 0.00000 0.00560 0.00371 0.00401 0.00307 0.00380 0.00376 0.00242 H25A 0.78745 0.16569 0.18600 1.00000 0.07968 0.00000 0.00000 H25B 0.70368 0.21720 0.26347 1.00000 0.07968 0.00000 0.00000 N21 0.91720 0.24492 0.33410 1.00000 0.02637 0.02197 0.02397 0.00144 0.00957 0.01116 0.02276 0.00801 0.00041 0.00036 0.00032 0.00000 0.00221 0.00198 0.00212 0.00163 0.00176 0.00172 0.00087 H21A 0.97812 0.19672 0.31944 1.00000 0.02732 0.00000 0.00000 H21B 0.89223 0.21609 0.39492 1.00000 0.02732 0.00000 0.00000 C31 0.21156 0.69608 0.30676 1.00000 0.01566 0.01977 0.02324 0.00280 0.01107 -0.00055 0.01887 0.00927 0.00046 0.00041 0.00038 0.00000 0.00221 0.00219 0.00238 0.00183 0.00188 0.00181 0.00094 C32 0.15294 0.80376 0.27762 1.00000 0.01686 0.01807 0.02463 0.00068 0.00793 0.00063 0.01973 0.00926 0.00047 0.00041 0.00038 0.00000 0.00225 0.00214 0.00245 0.00183 0.00190 0.00180 0.00095 C33 0.07631 0.81669 0.17232 1.00000 0.02016 0.02201 0.02443 0.00376 0.00327 0.00429 0.02271 0.00952 0.00049 0.00044 0.00039 0.00000 0.00241 0.00229 0.00249 0.00190 0.00196 0.00193 0.00101 H33 0.03363 0.88900 0.15425 1.00000 0.02726 0.00000 0.00000 C34 0.06257 0.72124 0.09250 1.00000 0.02651 0.03568 0.02294 -0.00627 0.00175 0.00882 0.02908 0.01025 0.00053 0.00049 0.00042 0.00000 0.00272 0.00282 0.00258 0.00214 0.00212 0.00228 0.00116 H34 0.01040 0.72846 0.01928 1.00000 0.03490 0.00000 0.00000 C35 0.12500 0.61618 0.12014 1.00000 0.02444 0.02455 0.02683 -0.01140 0.00564 0.00173 0.02601 0.00967 0.00051 0.00045 0.00041 0.00000 0.00258 0.00244 0.00262 0.00203 0.00209 0.00205 0.00109 H35 0.11709 0.55242 0.06535 1.00000 0.03121 0.00000 0.00000 C36 0.19918 0.60332 0.22747 1.00000 0.02265 0.01582 0.02985 -0.00184 0.00666 0.00120 0.02322 0.00937 0.00050 0.00042 0.00040 0.00000 0.00249 0.00214 0.00268 0.00191 0.00208 0.00189 0.00103 H36 0.24119 0.53072 0.24601 1.00000 0.02786 0.00000 0.00000 N32 0.17500 0.90823 0.36045 1.00000 0.02246 0.01399 0.01917 0.00258 0.00646 0.00401 0.01831 0.00754 0.00040 0.00033 0.00030 0.00000 0.00202 0.00175 0.00196 0.00147 0.00160 0.00154 0.00080 H32A 0.26586 0.94917 0.37749 1.00000 0.02747 0.00000 0.00000 H32B 0.15579 0.87616 0.42149 1.00000 0.02747 0.00000 0.00000 H32C 0.11693 0.96373 0.33340 1.00000 0.02747 0.00000 0.00000 O31A 0.42817 0.78114 0.46753 1.00000 0.02468 0.01819 0.02287 -0.00178 -0.00141 0.00492 0.02342 0.00633 0.00034 0.00029 0.00026 0.00000 0.00179 0.00156 0.00173 0.00130 0.00140 0.00136 0.00074 O31B 0.33958 0.55524 0.45016 1.00000 0.03245 0.01912 0.03266 0.00715 0.00850 0.00907 0.02760 0.00711 0.00036 0.00030 0.00028 0.00000 0.00199 0.00165 0.00199 0.00142 0.00160 0.00146 0.00079 O31C 0.20909 0.70182 0.50687 1.00000 0.03828 0.04704 0.03058 0.01337 0.01958 0.02450 0.03450 0.00832 0.00039 0.00036 0.00029 0.00000 0.00219 0.00228 0.00205 0.00172 0.00174 0.00184 0.00090 S31 0.30396 0.68107 0.44454 1.00000 0.02467 0.01724 0.02148 0.00366 0.00744 0.00745 0.02046 0.00244 0.00013 0.00010 0.00010 0.00000 0.00062 0.00054 0.00059 0.00044 0.00048 0.00046 0.00026 C41 0.71786 0.76132 0.30233 1.00000 0.01722 0.02004 0.01954 -0.00081 0.00441 0.00467 0.01894 0.00916 0.00047 0.00042 0.00037 0.00000 0.00224 0.00217 0.00227 0.00178 0.00183 0.00182 0.00094 C42 0.64783 0.67191 0.35560 1.00000 0.01737 0.02018 0.01918 0.00248 0.00557 0.00494 0.01862 0.00925 0.00047 0.00042 0.00036 0.00000 0.00226 0.00218 0.00228 0.00177 0.00183 0.00182 0.00094 C43 0.55661 0.56689 0.29887 1.00000 0.01558 0.01925 0.03003 0.00027 0.00634 0.00051 0.02196 0.00945 0.00047 0.00043 0.00040 0.00000 0.00227 0.00218 0.00261 0.00190 0.00196 0.00182 0.00100 H43 0.51131 0.50495 0.33647 1.00000 0.02635 0.00000 0.00000 C44 0.53148 0.55220 0.18740 1.00000 0.02982 0.02711 0.02604 -0.00608 0.00550 0.00248 0.02850 0.01035 0.00055 0.00047 0.00041 0.00000 0.00280 0.00254 0.00267 0.00208 0.00220 0.00218 0.00113 H44 0.46562 0.48176 0.14779 1.00000 0.03421 0.00000 0.00000 C45 0.60152 0.63936 0.13266 1.00000 0.03209 0.03324 0.02299 -0.00378 0.00708 0.00517 0.02969 0.01053 0.00055 0.00048 0.00042 0.00000 0.00288 0.00277 0.00259 0.00213 0.00221 0.00231 0.00116 H45 0.58605 0.62776 0.05607 1.00000 0.03563 0.00000 0.00000 C46 0.69507 0.74442 0.19115 1.00000 0.02235 0.02694 0.02482 0.00337 0.01131 0.00537 0.02363 0.00997 0.00050 0.00045 0.00039 0.00000 0.00248 0.00249 0.00252 0.00199 0.00204 0.00204 0.00103 H46 0.74338 0.80469 0.15412 1.00000 0.02836 0.00000 0.00000 N42 0.66629 0.68753 0.47265 1.00000 0.02259 0.01580 0.02378 0.00311 0.00582 0.00226 0.02099 0.00779 0.00041 0.00034 0.00031 0.00000 0.00208 0.00181 0.00208 0.00154 0.00168 0.00159 0.00085 H42A 0.75106 0.73715 0.50488 1.00000 0.03148 0.00000 0.00000 H42B 0.66271 0.61025 0.50155 1.00000 0.03148 0.00000 0.00000 H42C 0.59664 0.72495 0.48457 1.00000 0.03148 0.00000 0.00000 O41A 0.89479 0.96613 0.29787 1.00000 0.02345 0.01709 0.02887 0.00464 0.01081 0.00248 0.02255 0.00661 0.00033 0.00028 0.00027 0.00000 0.00176 0.00154 0.00185 0.00134 0.00145 0.00134 0.00072 O41B 0.93464 0.84651 0.46168 1.00000 0.01856 0.02113 0.02599 0.00474 -0.00113 0.00254 0.02346 0.00644 0.00033 0.00029 0.00026 0.00000 0.00167 0.00161 0.00181 0.00135 0.00138 0.00134 0.00074 O41C 0.74581 0.96790 0.41946 1.00000 0.02443 0.02230 0.02773 -0.00513 0.00731 0.00486 0.02479 0.00659 0.00034 0.00030 0.00027 0.00000 0.00180 0.00167 0.00185 0.00139 0.00147 0.00140 0.00075 S41 0.83349 0.89859 0.37603 1.00000 0.01875 0.01472 0.02077 0.00061 0.00530 0.00214 0.01823 0.00228 0.00012 0.00010 0.00009 0.00000 0.00057 0.00051 0.00058 0.00042 0.00045 0.00043 0.00025 Final Structure Factor Calculation for 06skc0075p-1 in P-1 Total number of l.s. parameters = 345 Maximum vector length = 511 Memory required = 4687 / 24017 wR2 = 0.1711 before cycle 5 for 5944 data and 0 / 345 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0848 for 3976 Fo > 4sig(Fo) and 0.1441 for all 5944 data wR2 = 0.1711, GooF = S = 1.101, Restrained GooF = 1.101 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0308 0.0215 0.0171 C1 0.0292 0.0212 0.0160 C2 0.0404 0.0276 0.0154 C3 0.0595 0.0331 0.0191 C4 0.0911 0.0242 0.0142 C5 0.0596 0.0234 0.0176 C6 0.0330 0.0231 0.0147 N2 0.0462 0.0192 0.0186 O1A 0.0637 0.0242 0.0141 O1B 0.0334 0.0291 0.0157 O1C 0.0251 0.0201 0.0124 S1 0.0569 0.0249 0.0204 C22 0.0827 0.0361 0.0252 C23 0.1597 0.0606 0.0255 C24 0.1407 0.0341 0.0244 C25 0.0303 0.0237 0.0143 N21 0.0252 0.0221 0.0092 C31 0.0251 0.0198 0.0144 C32 0.0281 0.0217 0.0184 C33 0.0427 0.0253 0.0193 C34 0.0396 0.0251 0.0134 C35 0.0309 0.0236 0.0151 C36 0.0225 0.0191 0.0134 N32 0.0352 0.0184 0.0166 O31A 0.0343 0.0330 0.0155 O31B 0.0601 0.0250 0.0184 O31C 0.0258 0.0209 0.0147 S31 0.0226 0.0180 0.0162 C41 0.0211 0.0184 0.0163 C42 0.0304 0.0211 0.0144 C43 0.0348 0.0314 0.0193 C44 0.0360 0.0324 0.0206 C45 0.0285 0.0255 0.0169 C46 0.0253 0.0226 0.0151 N42 0.0300 0.0224 0.0152 O41A 0.0352 0.0200 0.0152 O41B 0.0328 0.0245 0.0171 O41C 0.0209 0.0191 0.0147 S41 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.037 0.051 0.066 0.085 0.107 0.137 0.191 1.000 Number in group 654. 538. 611. 612. 568. 593. 588. 594. 590. 596. GooF 1.217 1.167 1.139 1.205 1.154 1.070 1.011 1.020 0.941 1.039 K 15.692 2.861 1.759 1.177 1.000 1.013 0.967 0.980 0.996 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 602. 602. 578. 610. 590. 584. 604. 590. 589. 595. GooF 1.278 1.218 1.213 1.155 1.106 1.086 0.982 0.904 0.872 1.114 K 1.117 1.097 1.128 1.072 1.029 1.037 1.000 1.000 1.006 1.006 R1 0.342 0.297 0.250 0.210 0.181 0.138 0.096 0.066 0.059 0.041 Recommended weighting scheme: WGHT 0.0000 6.8154 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 0 1 1079.79 1996.88 6.45 0.287 6.67 -2 -1 15 155.75 12.00 3.85 0.022 0.84 -6 3 15 153.69 3.91 3.79 0.013 0.81 -11 7 0 253.31 0.10 3.77 0.002 0.82 9 1 7 39.53 208.87 3.77 0.093 0.80 0 0 3 114.21 28.99 3.77 0.035 4.08 -8 -4 8 -39.22 93.69 3.74 0.062 0.97 9 -6 7 173.78 4.96 3.73 0.014 0.79 -11 7 4 168.93 8.62 3.59 0.019 0.84 2 8 9 -28.18 71.81 3.59 0.054 0.85 1 3 11 173.39 34.29 3.52 0.038 1.00 0 0 6 2092.08 1645.60 3.42 0.261 2.04 -3 -8 3 56.65 1.22 3.40 0.007 1.15 -1 1 16 114.65 5.21 3.34 0.015 0.78 -3 -8 12 92.94 285.67 3.33 0.109 0.83 10 4 3 136.63 327.38 3.31 0.116 0.79 7 -9 8 38.76 186.25 3.25 0.088 0.77 -3 -8 13 530.72 913.29 3.23 0.194 0.79 -9 7 11 251.11 567.67 3.20 0.153 0.81 10 1 1 85.72 0.65 3.19 0.005 0.91 -5 -4 11 497.86 1.25 3.16 0.007 1.00 7 -6 6 90.88 2.13 3.16 0.009 0.95 6 -6 9 90.81 1.16 3.14 0.007 0.86 -1 3 1 39.07 0.15 3.13 0.002 3.41 -4 12 2 149.08 7.59 3.06 0.018 0.87 9 -1 1 72.25 1.24 3.05 0.007 1.04 7 4 2 149.70 292.89 3.04 0.110 1.06 0 -11 10 -11.23 94.12 3.04 0.062 0.78 -8 -4 10 513.00 303.41 3.03 0.112 0.91 -1 -4 13 167.44 4.98 3.00 0.014 0.92 0 13 4 17.92 106.65 2.99 0.066 0.77 -4 -8 6 220.58 0.11 2.98 0.002 1.03 11 -2 3 244.08 70.68 2.97 0.054 0.82 -8 -1 9 90.80 327.83 2.97 0.116 1.04 -9 4 9 109.72 5.27 2.94 0.015 0.96 -4 5 14 620.54 391.34 2.93 0.127 0.84 1 -6 3 74.22 20.49 2.93 0.029 1.64 -3 12 6 215.57 3.79 2.92 0.013 0.82 -3 0 5 261.86 426.70 2.92 0.133 2.27 -5 2 14 216.16 33.61 2.87 0.037 0.89 -2 -5 15 351.23 175.72 2.86 0.085 0.79 -9 6 9 -14.81 75.61 2.85 0.056 0.90 -7 11 4 156.52 1.42 2.84 0.008 0.86 3 3 9 63.05 209.68 2.84 0.093 1.05 -6 8 11 161.93 3.75 2.84 0.012 0.85 4 2 11 288.99 142.54 2.84 0.077 0.88 4 8 7 86.55 1.11 2.83 0.007 0.85 -6 12 2 186.33 58.20 2.82 0.049 0.84 4 0 11 136.95 37.44 2.81 0.039 0.92 7 -7 4 902.31 600.05 2.77 0.158 0.99 Bond lengths and angles C1 - Distance Angles C6 1.3886 (0.0066) C2 1.4102 (0.0066) 119.30 (0.44) S1 1.7685 (0.0047) 119.00 (0.37) 121.70 (0.36) C1 - C6 C2 C2 - Distance Angles N2 1.3891 (0.0060) C3 1.4071 (0.0065) 120.06 (0.43) C1 1.4102 (0.0066) 121.55 (0.42) 118.17 (0.45) C2 - N2 C3 C3 - Distance Angles C4 1.3722 (0.0073) C2 1.4071 (0.0065) 120.70 (0.47) H3 0.9500 119.65 119.65 C3 - C4 C2 C4 - Distance Angles C3 1.3722 (0.0073) C5 1.3796 (0.0079) 121.10 (0.49) H4 0.9500 119.45 119.45 C4 - C3 C5 C5 - Distance Angles C6 1.3750 (0.0071) C4 1.3796 (0.0079) 118.95 (0.50) H5 0.9500 120.52 120.52 C5 - C6 C4 C6 - Distance Angles C5 1.3750 (0.0071) C1 1.3886 (0.0066) 121.77 (0.49) H6 0.9500 119.11 119.11 C6 - C5 C1 N2 - Distance Angles C2 1.3891 (0.0060) H2A 0.8800 120.00 H2B 0.8800 120.00 120.00 N2 - C2 H2A O1A - Distance Angles S1 1.4671 (0.0035) O1A - O1B - Distance Angles S1 1.4423 (0.0034) O1B - O1C - Distance Angles S1 1.4494 (0.0033) O1C - S1 - Distance Angles O1B 1.4423 (0.0034) O1C 1.4494 (0.0033) 113.89 (0.21) O1A 1.4671 (0.0035) 112.74 (0.23) 110.20 (0.21) C1 1.7685 (0.0047) 107.17 (0.22) 106.56 (0.22) 105.70 (0.21) S1 - O1B O1C O1A C22 - Distance Angles N21 1.4953 (0.0061) C23 1.5202 (0.0078) 104.79 (0.44) H22A 0.9900 110.79 110.79 H22B 0.9900 110.79 110.79 108.86 C22 - N21 C23 H22A C23 - Distance Angles C24 1.4912 (0.0103) C22 1.5202 (0.0078) 102.29 (0.50) H23A 0.9900 111.31 111.31 H23B 0.9900 111.31 111.31 109.20 C23 - C24 C22 H23A C24 - Distance Angles C25 1.4864 (0.0100) C23 1.4912 (0.0103) 104.94 (0.55) H24A 0.9900 110.76 110.76 H24B 0.9900 110.76 110.76 108.84 C24 - C25 C23 H24A C25 - Distance Angles C24 1.4864 (0.0100) N21 1.4868 (0.0069) 104.82 (0.58) H25A 0.9900 110.78 110.79 H25B 0.9900 110.78 110.79 108.86 C25 - C24 N21 H25A N21 - Distance Angles C25 1.4868 (0.0069) C22 1.4953 (0.0061) 107.89 (0.41) H21A 0.9200 110.13 110.13 H21B 0.9200 110.13 110.13 108.44 N21 - C25 C22 H21A C31 - Distance Angles C36 1.3762 (0.0063) C32 1.3936 (0.0063) 119.37 (0.44) S31 1.7741 (0.0047) 120.67 (0.36) 119.95 (0.35) C31 - C36 C32 C32 - Distance Angles C33 1.3766 (0.0063) C31 1.3936 (0.0063) 121.58 (0.43) N32 1.4767 (0.0056) 118.64 (0.40) 119.77 (0.40) C32 - C33 C31 C33 - Distance Angles C32 1.3766 (0.0063) C34 1.3980 (0.0066) 118.65 (0.44) H33 0.9500 120.68 120.68 C33 - C32 C34 C34 - Distance Angles C35 1.3849 (0.0069) C33 1.3980 (0.0066) 120.02 (0.46) H34 0.9500 119.99 119.99 C34 - C35 C33 C35 - Distance Angles C34 1.3849 (0.0069) C36 1.3907 (0.0067) 120.50 (0.43) H35 0.9500 119.75 119.75 C35 - C34 C36 C36 - Distance Angles C31 1.3762 (0.0063) C35 1.3907 (0.0067) 119.79 (0.44) H36 0.9500 120.10 120.10 C36 - C31 C35 N32 - Distance Angles C32 1.4767 (0.0056) H32A 0.9100 109.47 H32B 0.9100 109.47 109.47 H32C 0.9100 109.47 109.47 109.47 N32 - C32 H32A H32B O31A - Distance Angles S31 1.4609 (0.0034) O31A - O31B - Distance Angles S31 1.4516 (0.0033) O31B - O31C - Distance Angles S31 1.4409 (0.0036) O31C - S31 - Distance Angles O31C 1.4409 (0.0036) O31B 1.4516 (0.0033) 114.45 (0.22) O31A 1.4609 (0.0034) 112.30 (0.22) 112.34 (0.20) C31 1.7741 (0.0047) 105.12 (0.21) 106.65 (0.21) 105.07 (0.20) S31 - O31C O31B O31A C41 - Distance Angles C46 1.3787 (0.0064) C42 1.3868 (0.0063) 119.21 (0.42) S41 1.7862 (0.0045) 120.20 (0.36) 120.58 (0.34) C41 - C46 C42 C42 - Distance Angles C43 1.3784 (0.0061) C41 1.3868 (0.0064) 120.85 (0.42) N42 1.4581 (0.0057) 118.11 (0.41) 121.03 (0.39) C42 - C43 C41 C43 - Distance Angles C44 1.3774 (0.0067) C42 1.3784 (0.0061) 119.67 (0.45) H43 0.9500 120.16 120.17 C43 - C44 C42 C44 - Distance Angles C43 1.3774 (0.0067) C45 1.3845 (0.0073) 120.47 (0.46) H44 0.9500 119.76 119.76 C44 - C43 C45 C45 - Distance Angles C44 1.3845 (0.0073) C46 1.3953 (0.0068) 119.32 (0.47) H45 0.9500 120.34 120.34 C45 - C44 C46 C46 - Distance Angles C41 1.3787 (0.0064) C45 1.3953 (0.0068) 120.44 (0.46) H46 0.9500 119.78 119.78 C46 - C41 C45 N42 - Distance Angles C42 1.4581 (0.0057) H42A 0.9100 109.47 H42B 0.9100 109.47 109.47 H42C 0.9100 109.47 109.47 109.47 N42 - C42 H42A H42B O41A - Distance Angles S41 1.4491 (0.0034) O41A - O41B - Distance Angles S41 1.4641 (0.0032) O41B - O41C - Distance Angles S41 1.4555 (0.0034) O41C - S41 - Distance Angles O41A 1.4491 (0.0034) O41C 1.4555 (0.0034) 113.99 (0.19) O41B 1.4641 (0.0032) 113.81 (0.20) 112.55 (0.20) C41 1.7862 (0.0045) 106.01 (0.21) 105.52 (0.20) 103.81 (0.20) S41 - O41A O41C O41B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.85 2.737(5) 163.1 N42-H42C...O31A 0.91 2.80 3.553(4) 140.6 N42-H42C...S31 0.88 2.39 2.978(5) 124.6 N2-H2B...O1C 0.91 2.24 2.918(5) 130.3 N32-H32B...O31C 0.91 2.22 2.976(5) 140.3 N42-H42A...O41B 0.91 2.59 3.061(4) 112.9 N42-H42A...S41 0.88 2.47 3.188(5) 138.8 N2-H2A...O41C_$1 0.92 2.46 2.980(5) 116.1 N21-H21A...O41A_$1 0.88 2.32 2.935(5) 126.8 N2-H2B...O31A_$2 0.92 2.09 2.773(5) 130.1 N21-H21B...O31C_$2 0.91 2.51 3.149(5) 128.1 N42-H42A...O1A_$2 0.91 1.88 2.791(5) 174.5 N42-H42B...O31B_$2 0.92 1.99 2.858(5) 156.2 N21-H21A...O1A_$3 0.92 2.35 2.901(5) 118.2 N21-H21B...O41B_$4 0.91 2.10 2.937(6) 153.3 N32-H32A...N2_$5 0.91 2.15 2.837(5) 131.4 N32-H32C...O1A_$5 0.91 2.39 3.022(5) 126.8 N32-H32B...O41B_$6 0.91 2.16 2.890(5) 136.6 N32-H32C...O41A_$6 0.91 3.02 3.480(4) 113.5 N32-H32C...S41_$6 0.91 2.48 2.936(5) 111.2 N32-H32B...O41C_$7 FMAP and GRID set by program FMAP 2 3 32 GRID -1.724 -2 -2 1.724 2 2 R1 = 0.1433 for 5944 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.64 at 0.7486 0.3527 0.2382 [ 0.92 A from C24 ] Deepest hole -0.58 at 0.3975 0.1054 0.3594 [ 0.29 A from H2B ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4450 / 26615 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7486 0.3527 0.2382 1.00000 0.05 0.64 0.92 C24 1.10 H24A 1.40 C25 1.51 H25B Q2 1 0.0421 -0.1017 -0.1258 1.00000 0.05 0.48 1.91 H5 2.26 H25A 2.48 C5 2.53 H33 Q3 1 0.2472 0.5812 0.4984 1.00000 0.05 0.44 1.31 O31B 1.40 S31 1.42 O31C 2.38 H42B Q4 1 0.3294 0.5407 0.5664 1.00000 0.05 0.43 1.52 O31B 1.85 H42B 1.88 H43 2.17 S31 Q5 1 0.4814 0.1312 0.3587 1.00000 0.05 0.43 0.69 H2B 0.94 N2 1.53 H2A 1.90 C2 Q6 1 0.6012 0.0167 0.3606 1.00000 0.05 0.42 1.09 H2A 1.61 N2 1.62 O41C 2.21 H2B Q7 1 0.8654 0.2408 0.2093 1.00000 0.05 0.41 0.93 C25 1.00 H25A 1.50 C24 1.53 N21 Q8 1 0.7154 0.1635 0.2055 1.00000 0.05 0.40 0.83 H25A 0.98 C25 0.98 H25B 2.17 C24 Q9 1 0.2962 -0.1452 0.1101 1.00000 0.05 0.40 1.28 C4 1.43 C3 1.72 H4 1.91 H3 Q10 1 0.8167 0.4988 0.1030 1.00000 0.05 0.39 1.64 H24B 1.77 H24A 1.88 C24 2.00 H23B Shortest distances between peaks (including symmetry equivalents) 3 4 1.17 7 8 1.58 5 6 1.86 1 7 1.91 1 8 2.02 2 7 2.28 1 10 2.50 6 8 2.90 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.53: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: 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 4.44: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0075p-1 finished at 13:19:41 Total CPU time: 8.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++