+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0007p-1 started at 14:02:18 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0007p-1 in P-1 CELL 0.71073 7.3760 7.6241 10.2107 88.858 71.015 82.337 ZERR 2.00 0.0015 0.0025 0.0028 0.025 0.015 0.020 LATT 1 SFAC C H N O UNIT 16 28 4 14 V = 537.95 F(000) = 264.0 Mu = 0.14 mm-1 Cell Wt = 500.42 Rho = 1.545 MERG 2 OMIT -3.00 55.00 EXTI 0.02558 DFIX 0.84 0.02 H1W O1W H2W O1W DANG 1.35 0.02 H1W H2W SHEL 7 0.77 HTAB O2 O1A HTAB O3 O1W EQIV_$1 x, y+1, z HTAB N23 O3_$1 EQIV_$2 -x, -y, -z+2 HTAB N21 O2_$2 HTAB O2 O1A_$2 EQIV_$3 x, y-1, z HTAB O4B O1B_$3 EQIV_$4 -x+1, -y, -z+1 HTAB O1W O1B_$4 EQIV_$5 x+1, y, z HTAB O1W O4A_$5 FMAP 2 PLAN 5 SIZE 0.06 0.10 0.12 ACTA BOND $H WGHT 0.04050 0.19130 L.S. 8 TEMP -153.00 FVAR 1.04356 MOLE 1 C1 1 0.183372 0.101536 0.760787 11.00000 0.01711 0.02471 = 0.02700 -0.00520 -0.00818 0.00213 C2 1 0.143361 -0.074870 0.717641 11.00000 0.02480 0.02855 = 0.01714 0.00231 -0.00417 -0.00692 AFIX 13 H2 2 0.077574 -0.053310 0.646136 11.00000 -1.20000 AFIX 0 C3 1 0.332864 -0.198071 0.654139 11.00000 0.02358 0.02841 = 0.02274 0.00099 -0.00854 -0.00564 AFIX 13 H3 2 0.407007 -0.151546 0.562892 11.00000 -1.20000 AFIX 0 C4 1 0.282848 -0.379478 0.631800 11.00000 0.02382 0.02297 = 0.02524 -0.00184 -0.00117 -0.00415 O1B 4 0.276440 0.192197 0.659213 11.00000 0.03251 0.02780 = 0.02339 0.00386 -0.00898 -0.00913 O1A 4 0.126696 0.147340 0.884880 11.00000 0.02413 0.02803 = 0.02400 -0.00317 -0.00440 -0.00310 O2 4 0.021658 -0.161674 0.831270 11.00000 0.02646 0.03098 = 0.01936 -0.00168 -0.00320 -0.00989 AFIX 147 H2O 2 0.006720 -0.107150 0.905511 11.00000 -1.50000 AFIX 0 O3 4 0.442780 -0.198938 0.747020 11.00000 0.01997 0.03202 = 0.02501 -0.00063 -0.00705 -0.00553 AFIX 147 H3O 2 0.561112 -0.207118 0.701186 11.00000 -1.50000 AFIX 0 O4A 4 0.173521 -0.398872 0.566170 11.00000 0.03391 0.02829 = 0.03340 -0.00269 -0.01657 -0.00221 O4B 4 0.363943 -0.508751 0.688791 11.00000 0.03144 0.01971 = 0.03519 0.00085 -0.01443 -0.00477 AFIX 147 H4 2 0.317515 -0.601983 0.683049 11.00000 -1.50000 AFIX 0 MOLE 2 C24 1 0.305815 0.696837 1.130862 11.00000 0.01860 0.03066 = 0.02673 0.00008 -0.00993 -0.00086 C25 1 0.224042 0.574863 1.220563 11.00000 0.02715 0.03088 = 0.02257 -0.00446 -0.00792 -0.00444 AFIX 43 H25 2 0.202619 0.575544 1.317479 11.00000 -1.20000 AFIX 0 C22 1 0.230234 0.492674 1.014461 11.00000 0.02209 0.03156 = 0.02414 0.00045 -0.00652 -0.00171 AFIX 43 H22 2 0.214572 0.427905 0.941226 11.00000 -1.20000 AFIX 0 C26 1 0.381279 0.860142 1.154034 11.00000 0.02779 0.03238 = 0.04592 -0.00489 -0.00973 -0.00467 AFIX 137 H26A 2 0.361766 0.875234 1.252986 11.00000 -1.50000 H26B 2 0.312225 0.962483 1.122729 11.00000 -1.50000 H26C 2 0.519728 0.850652 1.101702 11.00000 -1.50000 AFIX 0 N21 3 0.177366 0.449549 1.146490 11.00000 0.02349 0.03418 = 0.02697 0.00337 -0.00444 -0.00729 AFIX 43 H21 2 0.121601 0.356168 1.181093 11.00000 0.04102 AFIX 0 N23 3 0.308526 0.641059 1.001579 11.00000 0.02258 0.02962 = 0.02309 0.00283 -0.00498 -0.00263 AFIX 43 H23 2 0.354957 0.695734 0.923458 11.00000 0.03863 AFIX 0 MOLE 3 O1W 4 0.811829 -0.198929 0.581483 11.00000 0.02759 0.04548 = 0.02555 0.00091 -0.00916 -0.00591 AFIX 1 H1W 2 0.790761 -0.206598 0.505949 11.00000 0.07247 H2W 2 0.914503 -0.266821 0.574525 11.00000 0.12133 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04skc0007p-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 - O4A O4B C3 O1B - C1 O1A - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C24 - C25 N23 C26 C25 - C24 N21 C22 - N23 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 O1W - no bonds found Operators for generating equivalent atoms: $1 x, y+1, z $2 -x, -y, -z+2 $3 x, y-1, z $4 -x+1, -y, -z+1 $5 x+1, y, z 9408 Reflections read, of which 0 rejected -8 =< h =< 9, -9 =< k =< 9, -12 =< l =< 12, Max. 2-theta = 52.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 3 0 2.91 1.58 6 8.17 7 5 0 -2.60 1.81 2 14.53 6 7 0 -1.80 2.20 3 15.21 6 -1 1 2.85 0.75 7 4.43 -5 0 1 12.04 1.80 3 17.24 7 4 1 1.96 1.11 6 8.60 6 6 1 0.50 1.66 4 9.80 -5 -7 2 0.80 1.46 4 8.43 -7 -2 2 16.24 3.19 3 23.55 -6 0 2 10.42 1.56 4 19.44 8 2 2 2.06 1.82 5 10.56 7 5 2 0.73 1.65 4 8.57 3 -6 3 111.30 30.84 2 352.96 -6 -5 3 10.91 2.15 4 15.07 5 -4 3 0.48 0.82 7 5.13 -6 -2 3 2.39 2.28 2 16.05 4 -2 3 3.62 0.68 7 3.88 -4 -6 4 -1.03 1.46 6 7.81 -3 -4 4 17.78 1.76 7 8.99 -3 -3 4 1.45 0.90 7 5.50 3 -2 4 4.33 0.55 7 4.73 -5 -1 4 0.43 1.11 4 7.70 -2 -1 4 4.25 0.68 8 3.86 -5 2 4 4.26 1.55 4 13.07 7 3 4 4.67 1.36 5 8.10 -2 -6 5 8.51 1.68 6 9.83 -2 -5 5 4.99 1.02 7 5.35 6 -5 5 3.16 1.09 6 10.79 5 -4 5 5.71 1.08 7 6.23 7 -3 5 1.54 1.08 5 7.83 -4 -1 5 1.54 0.85 4 6.33 0 -1 5 12.48 0.97 5 5.39 5 0 5 2.77 1.13 6 6.00 6 3 5 -0.28 0.97 5 4.93 -3 -7 6 30.42 3.28 3 19.31 -2 -5 6 7.86 1.32 7 10.86 -4 -4 6 -0.74 0.95 5 5.86 -2 -3 6 -1.39 0.71 8 4.94 1 -3 6 -0.98 0.36 6 2.30 4 -3 6 -0.26 0.49 7 4.40 7 -3 6 5.92 1.39 5 10.67 -2 -1 6 226.83 10.52 8 79.05 6 0 6 3.46 0.81 6 6.89 -4 3 6 25.08 3.45 3 19.26 -1 -7 7 0.47 0.99 3 8.74 -3 -5 7 1.26 1.49 3 12.06 4 -5 7 0.88 0.44 5 4.56 -2 -4 7 6.92 1.33 7 6.71 0 -4 7 5.63 0.82 5 6.34 5 -4 7 0.06 0.48 6 9.44 ** etc. ** 59 Inconsistent equivalents 2055 Unique reflections, of which 0 suppressed R(int) = 0.1435 R(sigma) = 0.1269 Friedel opposites merged Maximum memory for data reduction = 1944 / 20755 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 = 2393 / 200900 wR2 = 0.1429 before cycle 1 for 2055 data and 161 / 161 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04357 0.00414 0.003 OSF 2 0.02554 0.00692 -0.006 EXTI Mean shift/esd = 0.006 Maximum = -0.022 for U11 C2 Max. shift = 0.001 A for H3O Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 2 for 2055 data and 161 / 161 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04357 0.00414 -0.001 OSF 2 0.02551 0.00692 -0.004 EXTI Mean shift/esd = 0.002 Maximum = 0.013 for tors H3O Max. shift = 0.001 A for H3O Max. dU = 0.000 for H21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 3 for 2055 data and 161 / 161 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 -0.001 OSF 2 0.02551 0.00692 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.006 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 4 for 2055 data and 161 / 161 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 0.000 OSF 2 0.02551 0.00692 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 5 for 2055 data and 161 / 161 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 0.000 OSF 2 0.02550 0.00692 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 6 for 2055 data and 161 / 161 parameters Summary of restraints applied in cycle 6 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 0.000 OSF 2 0.02550 0.00692 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 7 for 2055 data and 161 / 161 parameters Summary of restraints applied in cycle 7 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 0.000 OSF 2 0.02550 0.00692 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2393 / 200900 wR2 = 0.1429 before cycle 8 for 2055 data and 161 / 161 parameters Summary of restraints applied in cycle 8 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04356 0.00414 0.000 OSF 2 0.02550 0.00692 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z N21 Max. shift = 0.000 A for H3O Max. dU = 0.000 for H23 Largest correlation matrix elements 0.582 EXTI / OSF Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0776 -0.0533 0.6461 13 1.000 0.000 C2 O2 C1 C3 H3 0.4070 -0.1515 0.5629 13 1.000 0.000 C3 O3 C4 C2 H2O 0.0066 -0.1071 0.9055 147 0.840 0.000 O2 C2 H2O H3O 0.5611 -0.2069 0.7012 147 0.840 0.000 O3 C3 H3O H4 0.3175 -0.6020 0.6831 147 0.840 0.000 O4B C4 H4 H25 0.2026 0.5756 1.3175 43 0.950 0.000 C25 C24 N21 H22 0.2146 0.4279 0.9412 43 0.950 0.000 C22 N23 N21 H26A 0.3617 0.8753 1.2530 137 0.980 0.000 C26 C24 H26A H26B 0.3123 0.9625 1.1227 137 0.980 0.000 C26 C24 H26A H26C 0.5197 0.8506 1.1017 137 0.980 0.000 C26 C24 H26A H21 0.1216 0.3562 1.1811 43 0.880 0.000 N21 C22 C25 H23 0.3550 0.6957 0.9235 43 0.880 0.000 N23 C22 C24 04skc0007p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.18337 0.10154 0.76079 1.00000 0.01713 0.02469 0.02702 -0.00522 -0.00817 0.00213 0.02309 0.00507 0.00042 0.00049 0.00034 0.00000 0.00157 0.00230 0.00201 0.00167 0.00150 0.00144 0.00083 C2 0.14337 -0.07488 0.71763 1.00000 0.02475 0.02854 0.01715 0.00231 -0.00417 -0.00693 0.02383 0.00516 0.00044 0.00049 0.00032 0.00000 0.00169 0.00234 0.00167 0.00155 0.00140 0.00155 0.00084 H2 0.07758 -0.05333 0.64613 1.00000 0.02860 0.00000 0.00000 C3 0.33287 -0.19807 0.65414 1.00000 0.02356 0.02844 0.02273 0.00100 -0.00852 -0.00566 0.02447 0.00507 0.00043 0.00049 0.00034 0.00000 0.00170 0.00242 0.00178 0.00160 0.00144 0.00155 0.00085 H3 0.40701 -0.15154 0.56289 1.00000 0.02936 0.00000 0.00000 C4 0.28285 -0.37949 0.63180 1.00000 0.02385 0.02297 0.02524 -0.00183 -0.00118 -0.00417 0.02555 0.00528 0.00044 0.00049 0.00034 0.00000 0.00174 0.00237 0.00194 0.00165 0.00159 0.00159 0.00088 O1B 0.27644 0.19220 0.65921 1.00000 0.03251 0.02781 0.02339 0.00385 -0.00898 -0.00913 0.02749 0.00341 0.00030 0.00033 0.00022 0.00000 0.00127 0.00166 0.00125 0.00113 0.00104 0.00113 0.00064 O1A 0.12669 0.14734 0.88488 1.00000 0.02411 0.02803 0.02402 -0.00316 -0.00441 -0.00310 0.02621 0.00341 0.00029 0.00032 0.00022 0.00000 0.00117 0.00163 0.00134 0.00112 0.00102 0.00106 0.00062 O2 0.02166 -0.16168 0.83127 1.00000 0.02644 0.03097 0.01937 -0.00168 -0.00321 -0.00986 0.02602 0.00339 0.00030 0.00033 0.00021 0.00000 0.00117 0.00164 0.00122 0.00109 0.00100 0.00107 0.00063 H2O 0.00663 -0.10708 0.90550 1.00000 0.03903 0.00000 0.00000 O3 0.44278 -0.19894 0.74702 1.00000 0.01999 0.03200 0.02503 -0.00064 -0.00705 -0.00554 0.02553 0.00332 0.00029 0.00033 0.00021 0.00000 0.00109 0.00164 0.00125 0.00112 0.00096 0.00106 0.00062 H3O 0.56109 -0.20691 0.70119 1.00000 0.03829 0.00000 0.00000 O4A 0.17352 -0.39887 0.56617 1.00000 0.03389 0.02830 0.03340 -0.00270 -0.01656 -0.00221 0.03063 0.00358 0.00031 0.00034 0.00023 0.00000 0.00130 0.00168 0.00139 0.00119 0.00112 0.00115 0.00065 O4B 0.36395 -0.50875 0.68879 1.00000 0.03143 0.01973 0.03518 0.00086 -0.01443 -0.00478 0.02778 0.00350 0.00031 0.00033 0.00024 0.00000 0.00125 0.00158 0.00141 0.00120 0.00110 0.00110 0.00063 H4 0.31746 -0.60197 0.68311 1.00000 0.04167 0.00000 0.00000 C24 0.30581 0.69684 1.13086 1.00000 0.01862 0.03067 0.02671 0.00007 -0.00994 -0.00086 0.02493 0.00512 0.00043 0.00049 0.00034 0.00000 0.00157 0.00249 0.00193 0.00170 0.00142 0.00151 0.00086 C25 0.22404 0.57487 1.22056 1.00000 0.02714 0.03090 0.02257 -0.00448 -0.00790 -0.00446 0.02679 0.00517 0.00043 0.00050 0.00034 0.00000 0.00181 0.00247 0.00181 0.00172 0.00152 0.00166 0.00089 H25 0.20261 0.57555 1.31748 1.00000 0.03215 0.00000 0.00000 C22 0.23024 0.49267 1.01446 1.00000 0.02206 0.03156 0.02413 0.00043 -0.00650 -0.00170 0.02635 0.00560 0.00043 0.00052 0.00035 0.00000 0.00166 0.00246 0.00196 0.00166 0.00146 0.00162 0.00087 H22 0.21458 0.42790 0.94122 1.00000 0.03161 0.00000 0.00000 C26 0.38127 0.86015 1.15403 1.00000 0.02779 0.03237 0.04591 -0.00488 -0.00973 -0.00467 0.03577 0.00562 0.00048 0.00053 0.00040 0.00000 0.00181 0.00269 0.00229 0.00194 0.00169 0.00173 0.00100 H26A 0.36169 0.87527 1.25299 1.00000 0.05365 0.00000 0.00000 H26B 0.31227 0.96248 1.12268 1.00000 0.05365 0.00000 0.00000 H26C 0.51974 0.85063 1.10175 1.00000 0.05365 0.00000 0.00000 N21 0.17736 0.44954 1.14649 1.00000 0.02349 0.03417 0.02699 0.00337 -0.00444 -0.00730 0.02885 0.00447 0.00037 0.00043 0.00028 0.00000 0.00143 0.00211 0.00169 0.00148 0.00127 0.00139 0.00077 H21 0.12160 0.35616 1.18109 1.00000 0.04073 0.00000 0.01150 N23 0.30853 0.64106 1.00157 1.00000 0.02259 0.02961 0.02310 0.00285 -0.00499 -0.00262 0.02581 0.00438 0.00036 0.00041 0.00029 0.00000 0.00140 0.00207 0.00162 0.00139 0.00120 0.00136 0.00074 H23 0.35495 0.69574 0.92345 1.00000 0.03835 0.00000 0.01118 O1W 0.81183 -0.19893 0.58148 1.00000 0.02761 0.04545 0.02556 0.00090 -0.00917 -0.00590 0.03265 0.00362 0.00030 0.00036 0.00022 0.00000 0.00124 0.00190 0.00131 0.00122 0.00105 0.00117 0.00069 H1W 0.79076 -0.20660 0.50595 1.00000 0.07247 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 H2W 0.91450 -0.26682 0.57453 1.00000 0.12133 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 Final Structure Factor Calculation for 04skc0007p-1 in P-1 Total number of l.s. parameters = 161 Maximum vector length = 511 Memory required = 2232 / 22995 wR2 = 0.1429 before cycle 9 for 2055 data and 0 / 161 parameters Summary of restraints applied in cycle 9 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 0.001 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.071; Restrained GooF = 1.070 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0670 for 1234 Fo > 4sig(Fo) and 0.1397 for all 2055 data wR2 = 0.1429, GooF = S = 1.071, Restrained GooF = 1.070 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0324 0.0216 0.0152 C1 0.0303 0.0249 0.0163 C2 0.0290 0.0233 0.0211 C3 0.0350 0.0223 0.0193 C4 0.0352 0.0259 0.0214 O1B 0.0315 0.0264 0.0207 O1A 0.0373 0.0224 0.0184 O2 0.0326 0.0249 0.0191 O3 0.0394 0.0283 0.0242 O4A 0.0365 0.0276 0.0192 O4B 0.0316 0.0267 0.0165 C24 0.0338 0.0270 0.0196 C25 0.0323 0.0250 0.0218 C22 0.0496 0.0304 0.0273 C26 0.0350 0.0312 0.0204 N21 0.0316 0.0251 0.0208 N23 0.0455 0.0274 0.0251 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.020 0.032 0.042 0.056 0.072 0.093 0.123 0.174 1.000 Number in group 206. 220. 207. 197. 204. 208. 203. 200. 207. 203. GooF 1.150 1.026 0.979 0.955 1.166 1.159 1.178 0.959 1.081 1.016 K 22.817 9.125 1.898 1.139 1.090 1.165 0.970 1.006 1.000 1.010 Resolution(A) 0.81 0.85 0.88 0.92 0.97 1.03 1.11 1.22 1.40 1.75 inf Number in group 209. 212. 195. 208. 204. 205. 207. 205. 204. 206. GooF 1.056 0.947 1.039 1.109 1.132 1.051 1.005 1.078 1.072 1.199 K 0.976 1.165 1.119 1.291 1.031 1.079 1.021 1.048 1.023 1.013 R1 0.383 0.332 0.281 0.262 0.164 0.122 0.082 0.088 0.063 0.037 Recommended weighting scheme: WGHT 0.0406 0.1869 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) 3 -2 10 181.34 303.70 5.05 0.186 0.97 -3 1 6 27.53 0.84 3.68 0.010 1.13 9 1 4 4.69 54.03 3.67 0.079 0.82 -2 2 3 45.12 21.37 3.63 0.049 1.73 -1 -7 4 84.50 37.29 3.57 0.065 0.98 7 3 7 78.95 31.80 3.55 0.060 0.94 1 -1 3 59.07 34.51 3.35 0.063 3.03 7 4 4 27.86 0.01 3.34 0.001 0.97 2 4 6 48.10 25.57 3.12 0.054 1.28 3 -4 4 31.69 56.90 3.11 0.081 1.32 -1 0 1 565.86 680.69 3.06 0.279 4.91 2 7 3 141.98 197.62 3.04 0.150 1.04 -1 2 1 24.65 3.05 3.03 0.019 2.85 3 -5 7 148.82 253.87 3.01 0.170 1.00 8 1 5 30.97 0.30 2.99 0.006 0.91 -6 1 2 47.83 0.92 2.90 0.010 1.02 4 -4 2 20.44 0.10 2.84 0.003 1.23 -2 0 9 104.42 143.84 2.82 0.128 0.94 4 -2 5 593.42 6.82 2.82 0.028 1.40 1 0 9 32.41 6.09 2.81 0.026 1.12 -6 3 0 17.79 0.60 2.81 0.008 1.00 0 2 4 244.93 199.14 2.80 0.151 2.01 -2 -7 2 27.18 0.35 2.80 0.006 1.03 -7 -4 3 22.31 33.08 2.77 0.062 0.83 3 2 0 299.59 356.41 2.73 0.202 2.10 4 5 8 -9.68 19.30 2.72 0.047 0.97 0 8 0 52.47 5.29 2.70 0.025 0.94 2 -1 1 10231.56 8746.13 2.69 1.000 3.13 2 -2 2 382.51 317.22 2.68 0.190 2.39 8 5 2 -2.22 2.01 2.63 0.015 0.83 -1 5 8 31.30 0.17 2.57 0.004 0.88 8 5 5 13.25 52.07 2.57 0.077 0.83 0 3 1 29.87 51.50 2.57 0.077 2.42 1 1 2 206.68 169.42 2.52 0.139 4.15 4 6 7 89.84 42.93 2.51 0.070 0.94 6 3 10 25.55 57.11 2.49 0.081 0.87 -1 6 5 49.34 21.42 2.48 0.049 0.99 1 -6 9 -2.30 45.77 2.48 0.072 0.84 3 -1 7 13.21 33.70 2.47 0.062 1.36 1 -2 9 22.46 3.18 2.47 0.019 1.07 3 1 6 76.23 51.75 2.42 0.077 1.57 3 6 5 47.79 73.36 2.41 0.092 1.07 -2 -8 1 53.34 21.72 2.41 0.050 0.93 4 7 2 30.14 1.45 2.41 0.013 0.99 4 -3 10 37.89 0.38 2.40 0.007 0.91 6 7 5 11.06 61.34 2.40 0.084 0.85 -7 -3 3 14.88 7.46 2.35 0.029 0.85 2 0 1 23.37 16.25 2.34 0.043 3.65 -2 -4 2 23.51 10.14 2.33 0.034 1.58 2 -8 1 -13.78 8.36 2.33 0.031 0.89 Bond lengths and angles C1 - Distance Angles O1A 1.2395 (0.0038) O1B 1.2882 (0.0038) 125.72 (0.33) C2 1.5180 (0.0049) 120.04 (0.30) 114.23 (0.27) C1 - O1A O1B C2 - Distance Angles O2 1.4284 (0.0036) C1 1.5180 (0.0049) 112.30 (0.26) C3 1.5299 (0.0048) 108.48 (0.28) 110.42 (0.25) H2 1.0000 108.52 108.52 108.52 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4337 (0.0038) C4 1.5181 (0.0050) 113.15 (0.29) C2 1.5299 (0.0048) 107.63 (0.26) 107.95 (0.25) H3 1.0000 109.35 109.35 109.35 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2282 (0.0038) O4B 1.3093 (0.0042) 124.21 (0.33) C3 1.5181 (0.0050) 121.35 (0.33) 114.43 (0.29) C4 - O4A O4B O1B - Distance Angles C1 1.2882 (0.0038) O1B - O1A - Distance Angles C1 1.2395 (0.0038) O1A - O2 - Distance Angles C2 1.4284 (0.0036) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4337 (0.0038) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2282 (0.0038) O4A - O4B - Distance Angles C4 1.3093 (0.0042) H4 0.8400 109.47 O4B - C4 C24 - Distance Angles C25 1.3505 (0.0047) N23 1.3881 (0.0044) 105.86 (0.31) C26 1.4827 (0.0051) 130.79 (0.33) 123.34 (0.31) C24 - C25 N23 C25 - Distance Angles C24 1.3505 (0.0047) N21 1.3746 (0.0045) 107.73 (0.29) H25 0.9500 126.14 126.14 C25 - C24 N21 C22 - Distance Angles N23 1.3227 (0.0045) N21 1.3237 (0.0042) 108.57 (0.32) H22 0.9500 125.72 125.72 C22 - N23 N21 C26 - Distance Angles C24 1.4827 (0.0051) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3237 (0.0042) C25 1.3746 (0.0045) 108.66 (0.31) H21 0.8800 125.67 125.67 N21 - C22 C25 N23 - Distance Angles C22 1.3227 (0.0045) C24 1.3881 (0.0044) 109.18 (0.29) H23 0.8800 125.41 125.41 N23 - C22 C24 O1W - Distance Angles H1W 0.8394 H2W 0.8416 106.97 O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.22 2.695(3) 116.3 O2-H2O...O1A 0.84 1.86 2.697(3) 171.1 O3-H3O...O1W 0.88 1.91 2.783(4) 174.7 N23-H23...O3_$1 0.88 1.96 2.765(4) 151.4 N21-H21...O2_$2 0.84 2.08 2.743(3) 135.5 O2-H2O...O1A_$2 0.84 1.67 2.501(3) 167.2 O4B-H4...O1B_$3 0.84 1.90 2.738(3) 172.1 O1W-H1W...O1B_$4 0.84 2.01 2.849(3) 171.8 O1W-H2W...O4A_$5 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.1397 for 2055 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.2154 0.3438 0.9420 [ 0.64 A from H22 ] Deepest hole -0.31 at 0.0600 0.1163 0.7222 [ 1.10 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2216 / 15920 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2154 0.3438 0.9420 1.00000 0.05 0.29 0.64 H22 1.40 C22 1.89 O1A 2.17 N21 Q2 1 0.0826 -0.1363 1.0231 1.00000 0.05 0.27 1.48 H2O 1.54 O1A 1.96 H2O 2.16 O2 Q3 1 0.4701 0.9123 1.0000 1.00000 0.05 0.26 1.27 H26C 1.42 H26B 1.56 C26 2.03 H26B Q4 1 0.0128 0.0802 0.9651 1.00000 0.05 0.24 1.14 O1A 1.30 H2O 1.57 H2O 2.07 C1 Q5 1 -0.0053 -0.2560 0.8080 1.00000 0.05 0.23 0.83 O2 1.20 H21 1.55 H2O 1.91 C2 Shortest distances between peaks (including symmetry equivalents) 2 4 0.75 4 4 1.41 3 3 1.46 2 4 1.81 2 2 2.38 1 4 2.62 1 5 2.65 4 5 2.68 2 5 2.69 1 2 2.80 2 3 2.86 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 0.00: Analyse other restraints etc. 0.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.44: Structure factors and derivatives 0.78: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0007p-1 finished at 14:02:20 Total CPU time: 2.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++