+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s94 started at 10:01:01 on 09-Oct-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s94 in P2(1)2(1)2(1) CELL 0.71073 4.7254 9.6175 27.4069 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0007 0.0024 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 48 80 8 12 V = 1245.55 F(000) = 520.0 Mu = 0.09 mm-1 Cell Wt = 961.20 Rho = 1.281 MERG 2 OMIT -3.00 55.00 OMIT 4 3 1 OMIT 3 0 6 EXTI 0.04609 SHEL 7 0.77 DFIX 0.84 O1W H1WA O1W H1WB DANG 1.35 H1WA H1WB EQIV $1 X+1, Y, Z EQIV $2 X+1/2, -Y-1/2, -Z+2 HTAB N2 O2_$1 HTAB O1W O1 HTAB O1W O1W_$2 FMAP 2 PLAN 5 SIZE 0.04 0.08 0.36 ACTA BOND $H WGHT 0.08580 0.89810 L.S. 10 TEMP -153.00 FVAR 0.45813 MOLE 1 C1 1 0.253846 0.261057 0.871818 11.00000 0.03562 0.03355 = 0.02668 -0.00040 0.00081 0.00314 AFIX 13 H1 2 0.464185 0.249942 0.872758 11.00000 -1.20000 AFIX 0 C2 1 0.173144 0.416068 0.867261 11.00000 0.10806 0.03232 = 0.03861 0.00965 0.02693 0.01444 AFIX 23 H2A 2 0.345479 0.473153 0.862716 11.00000 -1.20000 H2B 2 0.048259 0.430058 0.838676 11.00000 -1.20000 AFIX 0 C3 1 0.033831 0.455780 0.909698 11.00000 0.19969 0.03971 = 0.12433 0.02443 0.11675 0.04040 AFIX 23 H3A 2 -0.143680 0.504374 0.900905 11.00000 -1.20000 H3B 2 0.154297 0.522014 0.927952 11.00000 -1.20000 AFIX 0 C4 1 -0.033636 0.336705 0.941356 11.00000 0.03037 0.03991 = 0.02813 -0.01078 0.00342 0.00317 AFIX 23 H4A 2 0.027830 0.353868 0.975360 11.00000 -1.20000 H4B 2 -0.239003 0.316358 0.941083 11.00000 -1.20000 AFIX 0 C5 1 0.143976 0.096295 0.940906 11.00000 0.03148 0.03430 = 0.01821 -0.00104 -0.00570 0.00168 C6 1 0.333270 -0.013269 0.917635 11.00000 0.03274 0.03466 = 0.02715 0.00408 -0.00285 0.00265 AFIX 23 H6A 2 0.449857 -0.058431 0.943122 11.00000 -1.20000 H6B 2 0.462407 0.031617 0.893950 11.00000 -1.20000 AFIX 0 C7 1 0.152616 -0.123948 0.891305 11.00000 0.03760 0.04125 = 0.02543 -0.00171 0.00461 -0.00377 AFIX 23 H7A 2 0.072498 -0.189394 0.915524 11.00000 -1.20000 H7B 2 -0.006331 -0.078264 0.874078 11.00000 -1.20000 AFIX 0 C8 1 0.331509 -0.202324 0.855312 11.00000 0.04393 0.03248 = 0.04297 -0.00419 0.00620 -0.00541 AFIX 43 H8 2 0.474412 -0.261305 0.868198 11.00000 -1.20000 AFIX 0 C9 1 0.307704 -0.196508 0.807148 11.00000 0.04451 0.03657 = 0.04020 -0.01073 0.00977 -0.00688 AFIX 43 H9 2 0.437184 -0.251034 0.788790 11.00000 -1.20000 AFIX 0 C10 1 0.096095 -0.112178 0.778580 11.00000 0.05093 0.04949 = 0.02285 -0.00165 -0.00195 -0.01956 AFIX 23 H10A 2 -0.070229 -0.093101 0.799500 11.00000 -1.20000 H10B 2 0.030668 -0.167423 0.750265 11.00000 -1.20000 AFIX 0 C11 1 0.217181 0.025936 0.760284 11.00000 0.04381 0.04572 = 0.02351 -0.00171 -0.00082 -0.01042 AFIX 23 H11A 2 0.380184 0.006724 0.738615 11.00000 -1.20000 H11B 2 0.071205 0.074399 0.740735 11.00000 -1.20000 AFIX 0 C12 1 0.128680 0.177253 0.830355 11.00000 0.02236 0.05021 = 0.01812 0.00624 0.00151 0.00198 N1 3 0.128490 0.223119 0.919144 11.00000 0.03306 0.03227 = 0.01924 0.00061 0.00179 0.00399 N2 3 0.309190 0.117299 0.799793 11.00000 0.02253 0.04124 = 0.02533 -0.00250 0.00008 -0.00665 AFIX 43 H2 2 0.491335 0.133205 0.803474 11.00000 -1.20000 AFIX 0 O1 4 0.009902 0.071793 0.978511 11.00000 0.04311 0.04094 = 0.02177 0.00087 0.00250 -0.00173 O2 4 -0.131452 0.167530 0.826015 11.00000 0.02406 0.09126 = 0.03044 -0.00070 -0.00123 0.00032 MOLE 2 O1W 4 0.042861 -0.191898 1.019951 11.00000 0.04453 0.04967 = 0.04828 0.01275 0.00502 -0.00141 H1WA 2 0.019272 -0.110298 1.009561 11.00000 -1.20000 H1WB 2 0.201761 -0.218954 1.008658 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for s94 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 C12 C2 C2 - C3 C1 C3 - C2 C4 C4 - N1 C3 C5 - O1 N1 C6 C6 - C5 C7 C7 - C8 C6 C8 - C9 C7 C9 - C8 C10 C10 - C9 C11 C11 - N2 C10 C12 - O2 N2 C1 N1 - C5 C4 C1 N2 - C12 C11 O1 - C5 O2 - C12 O1W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 x+1/2, -y-1/2, -z+2 8997 Reflections read, of which 57 rejected -6 =< h =< 5, -12 =< k =< 12, -35 =< l =< 32, Max. 2-theta = 54.84 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 4 0 139.83 2.90 4 49.88 4 4 0 12.06 0.85 5 5.12 2 8 0 21.78 3.30 2 21.54 -4 3 1 9.10 0.97 2 13.02 3 4 1 6.41 0.51 7 21.38 1 0 2 1357.58 58.72 2 775.09 1 3 2 16.40 0.86 9 5.58 -3 4 2 4.79 0.42 7 3.74 4 4 2 14.77 0.87 5 5.19 -4 3 3 18.40 0.92 4 7.35 -2 3 3 190.98 5.13 8 30.70 3 3 3 12.70 0.61 6 4.56 2 4 3 16.93 0.83 8 4.97 2 3 4 18.84 0.93 7 24.14 1 4 4 434.22 15.28 7 79.49 3 4 4 3.07 0.44 7 2.82 2 7 4 11.37 1.11 5 6.32 1 1 5 427.41 16.69 6 92.54 3 1 5 28.69 0.84 4 10.51 1 3 5 6.21 0.43 7 24.52 1 2 6 136.17 5.09 6 77.96 4 4 6 11.25 0.78 4 5.89 1 6 6 5.58 0.52 6 7.26 3 7 6 4.37 1.96 2 11.90 -1 1 7 143.65 5.33 5 55.94 0 1 7 130.44 4.94 5 139.99 1 1 7 146.33 5.80 7 62.33 4 2 7 21.16 0.83 5 6.12 5 3 7 6.55 0.90 2 6.04 1 4 7 8.92 0.73 6 5.43 2 5 7 1.40 0.42 8 4.01 3 7 7 25.14 1.80 3 16.67 0 0 8 44.53 1.56 3 13.95 0 1 8 69.94 3.43 3 27.63 1 2 8 81.39 4.32 5 27.05 2 6 8 13.00 1.17 4 12.65 3 6 8 3.40 1.00 2 9.42 1 1 9 34.17 1.54 6 60.78 0 2 9 6.91 0.52 6 9.48 1 3 9 8.06 0.51 8 16.63 0 5 9 146.38 1.81 7 65.32 1 5 9 20.79 1.05 6 7.33 2 5 9 4.61 0.61 6 3.78 1 8 9 11.51 1.42 4 7.82 0 1 10 10.62 0.89 4 253.48 1 2 10 100.88 7.57 3 178.06 2 2 10 52.06 2.62 4 24.50 3 2 10 59.41 3.01 3 15.23 0 3 10 277.65 9.94 5 88.91 0 4 10 8.85 1.19 4 14.62 ** etc. ** 133 Inconsistent equivalents 2609 Unique reflections, of which 0 suppressed R(int) = 0.2385 R(sigma) = 0.1808 Friedel opposites not merged Maximum memory for data reduction = 2057 / 26807 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 = 2536 / 200900 wR2 = 0.2348 before cycle 1 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45816 0.00284 0.011 OSF 2 0.04624 0.01231 0.013 EXTI Mean shift/esd = 0.004 Maximum = 0.013 for y H1WA Max. shift = 0.001 A for H1WA Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 2 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.006 OSF 2 0.04631 0.01232 0.005 EXTI Mean shift/esd = 0.001 Maximum = 0.006 for OSF Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 3 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x H1WA Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 4 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x H1WA Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 5 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x H1WA Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 6 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C3 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 7 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 8 for 2609 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for C9 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 9 for 2609 data and 161 / 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H3B Max. dU = 0.000 for C10 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2536 / 200900 wR2 = 0.2348 before cycle 10 for 2609 data and 161 / 161 parameters Summary of restraints applied in cycle 10 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45818 0.00284 0.000 OSF 2 0.04631 0.01233 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C10 Largest correlation matrix elements 0.683 U13 C3 / U11 C3 0.576 EXTI / OSF 0.531 z C3 / x C3 0.643 U13 C3 / U33 C3 0.558 z H1WB / x H1WB 0.512 y H1WB / x H1WB 0.613 z H1WA / y H1WA 0.535 U12 C3 / U23 C3 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.4642 0.2499 0.8728 13 1.000 0.000 C1 N1 C12 C2 H2A 0.3455 0.4731 0.8627 23 0.990 0.000 C2 C3 C1 H2B 0.0483 0.4301 0.8387 23 0.990 0.000 C2 C3 C1 H3A -0.1437 0.5044 0.9009 23 0.990 0.000 C3 C2 C4 H3B 0.1543 0.5220 0.9280 23 0.990 0.000 C3 C2 C4 H4A 0.0278 0.3539 0.9754 23 0.990 0.000 C4 N1 C3 H4B -0.2390 0.3164 0.9411 23 0.990 0.000 C4 N1 C3 H6A 0.4498 -0.0584 0.9431 23 0.990 0.000 C6 C5 C7 H6B 0.4624 0.0316 0.8940 23 0.990 0.000 C6 C5 C7 H7A 0.0725 -0.1894 0.9155 23 0.990 0.000 C7 C8 C6 H7B -0.0063 -0.0783 0.8741 23 0.990 0.000 C7 C8 C6 H8 0.4744 -0.2613 0.8682 43 0.950 0.000 C8 C9 C7 H9 0.4372 -0.2510 0.7888 43 0.950 0.000 C9 C8 C10 H10A -0.0702 -0.0931 0.7995 23 0.990 0.000 C10 C9 C11 H10B 0.0307 -0.1674 0.7503 23 0.990 0.000 C10 C9 C11 H11A 0.3802 0.0067 0.7386 23 0.990 0.000 C11 N2 C10 H11B 0.0712 0.0744 0.7407 23 0.990 0.000 C11 N2 C10 H2 0.4913 0.1332 0.8035 43 0.880 0.000 N2 C12 C11 s94 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.25385 0.26106 0.87182 1.00000 0.03561 0.03355 0.02670 -0.00041 0.00083 0.00311 0.03195 0.00783 0.00096 0.00046 0.00017 0.00000 0.00219 0.00240 0.00231 0.00189 0.00176 0.00194 0.00104 H1 0.46418 0.24995 0.87276 1.00000 0.03834 0.00000 0.00000 C2 0.17315 0.41606 0.86726 1.00000 0.10804 0.03236 0.03861 0.00966 0.02696 0.01444 0.05967 0.01266 0.00165 0.00053 0.00021 0.00000 0.00457 0.00264 0.00301 0.00236 0.00334 0.00311 0.00166 H2A 0.34548 0.47315 0.86272 1.00000 0.07161 0.00000 0.00000 H2B 0.04825 0.43005 0.83868 1.00000 0.07161 0.00000 0.00000 C3 0.03384 0.45578 0.90970 1.00000 0.19966 0.03973 0.12436 0.02443 0.11675 0.04038 0.12125 0.02057 0.00232 0.00066 0.00035 0.00000 0.00981 0.00352 0.00762 0.00422 0.00781 0.00487 0.00441 H3A -0.14366 0.50438 0.90091 1.00000 0.14550 0.00000 0.00000 H3B 0.15432 0.52201 0.92795 1.00000 0.14550 0.00000 0.00000 C4 -0.03363 0.33670 0.94136 1.00000 0.03037 0.03993 0.02813 -0.01078 0.00341 0.00316 0.03281 0.00777 0.00091 0.00048 0.00016 0.00000 0.00217 0.00249 0.00222 0.00198 0.00186 0.00200 0.00102 H4A 0.02783 0.35386 0.97536 1.00000 0.03937 0.00000 0.00000 H4B -0.23900 0.31635 0.94108 1.00000 0.03937 0.00000 0.00000 C5 0.14399 0.09630 0.94091 1.00000 0.03149 0.03431 0.01822 -0.00104 -0.00570 0.00166 0.02801 0.00714 0.00090 0.00045 0.00015 0.00000 0.00207 0.00234 0.00185 0.00171 0.00176 0.00193 0.00091 C6 0.33325 -0.01327 0.91763 1.00000 0.03274 0.03468 0.02715 0.00408 -0.00286 0.00266 0.03152 0.00753 0.00091 0.00045 0.00016 0.00000 0.00224 0.00232 0.00221 0.00195 0.00180 0.00201 0.00098 H6A 0.44984 -0.05844 0.94312 1.00000 0.03783 0.00000 0.00000 H6B 0.46240 0.03161 0.89395 1.00000 0.03783 0.00000 0.00000 C7 0.15262 -0.12394 0.89130 1.00000 0.03759 0.04128 0.02544 -0.00170 0.00461 -0.00374 0.03477 0.00786 0.00097 0.00048 0.00016 0.00000 0.00226 0.00258 0.00223 0.00194 0.00193 0.00216 0.00105 H7A 0.07250 -0.18939 0.91552 1.00000 0.04173 0.00000 0.00000 H7B -0.00633 -0.07826 0.87408 1.00000 0.04173 0.00000 0.00000 C8 0.33150 -0.20233 0.85531 1.00000 0.04392 0.03250 0.04297 -0.00419 0.00618 -0.00542 0.03980 0.00838 0.00107 0.00048 0.00019 0.00000 0.00259 0.00245 0.00281 0.00214 0.00226 0.00229 0.00114 H8 0.47440 -0.26131 0.86820 1.00000 0.04776 0.00000 0.00000 C9 0.30770 -0.19651 0.80715 1.00000 0.04451 0.03659 0.04020 -0.01073 0.00977 -0.00689 0.04043 0.00829 0.00103 0.00048 0.00019 0.00000 0.00260 0.00255 0.00276 0.00225 0.00221 0.00219 0.00117 H9 0.43718 -0.25104 0.78879 1.00000 0.04852 0.00000 0.00000 C10 0.09609 -0.11218 0.77858 1.00000 0.05096 0.04953 0.02286 -0.00166 -0.00196 -0.01958 0.04111 0.00782 0.00106 0.00052 0.00017 0.00000 0.00287 0.00286 0.00231 0.00211 0.00200 0.00241 0.00123 H10A -0.07024 -0.09310 0.79950 1.00000 0.04934 0.00000 0.00000 H10B 0.03067 -0.16742 0.75026 1.00000 0.04934 0.00000 0.00000 C11 0.21718 0.02594 0.76028 1.00000 0.04383 0.04576 0.02350 -0.00170 -0.00081 -0.01042 0.03770 0.00796 0.00103 0.00050 0.00017 0.00000 0.00258 0.00272 0.00225 0.00210 0.00183 0.00231 0.00113 H11A 0.38018 0.00673 0.73861 1.00000 0.04523 0.00000 0.00000 H11B 0.07120 0.07440 0.74073 1.00000 0.04523 0.00000 0.00000 C12 0.12869 0.17726 0.83036 1.00000 0.02237 0.05020 0.01813 0.00624 0.00151 0.00199 0.03023 0.00759 0.00083 0.00049 0.00015 0.00000 0.00185 0.00272 0.00201 0.00198 0.00167 0.00199 0.00098 N1 0.12849 0.22312 0.91914 1.00000 0.03306 0.03229 0.01925 0.00060 0.00180 0.00397 0.02820 0.00617 0.00076 0.00037 0.00012 0.00000 0.00177 0.00192 0.00169 0.00148 0.00148 0.00157 0.00083 N2 0.30919 0.11730 0.79979 1.00000 0.02254 0.04126 0.02533 -0.00250 0.00008 -0.00666 0.02971 0.00584 0.00071 0.00036 0.00013 0.00000 0.00172 0.00205 0.00186 0.00162 0.00136 0.00156 0.00087 H2 0.49134 0.13321 0.80347 1.00000 0.03565 0.00000 0.00000 O1 0.00991 0.07179 0.97851 1.00000 0.04311 0.04096 0.02179 0.00087 0.00249 -0.00173 0.03529 0.00548 0.00071 0.00032 0.00011 0.00000 0.00167 0.00177 0.00156 0.00142 0.00140 0.00150 0.00079 O2 -0.13146 0.16753 0.82602 1.00000 0.02407 0.09130 0.03044 -0.00071 -0.00124 0.00033 0.04860 0.00594 0.00060 0.00044 0.00012 0.00000 0.00149 0.00274 0.00182 0.00187 0.00140 0.00174 0.00098 O1W 0.04286 -0.19189 1.01995 1.00000 0.04452 0.04969 0.04830 0.01275 0.00502 -0.00142 0.04750 0.00699 0.00077 0.00040 0.00015 0.00000 0.00197 0.00217 0.00223 0.00193 0.00169 0.00172 0.00095 H1WA 0.01945 -0.11024 1.00958 1.00000 0.05700 0.10496 0.01143 0.00302 0.00215 0.00000 0.00000 H1WB 0.20171 -0.21896 1.00864 1.00000 0.05700 0.10375 0.00726 0.00513 0.00211 0.00000 0.00000 Final Structure Factor Calculation for s94 in P2(1)2(1)2(1) Total number of l.s. parameters = 161 Maximum vector length = 511 Memory required = 2377 / 25046 wR2 = 0.2348 before cycle 11 for 2609 data and 2 / 161 parameters Summary of restraints applied in cycle 11 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.059; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0858 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0859 for 1722 Fo > 4sig(Fo) and 0.1314 for all 2609 data wR2 = 0.2348, GooF = S = 1.059, Restrained GooF = 1.059 for all data Flack x parameter = 1.6381 with esd 3.2353 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0379 0.0314 0.0265 C1 0.1205 0.0336 0.0249 C2 0.2934 0.0409 0.0294 C3 may be split into 0.0762 0.4605 0.9150 and -0.0085 0.4510 0.9044 0.0464 0.0323 0.0198 C4 0.0359 0.0320 0.0161 C5 0.0370 0.0337 0.0238 C6 0.0444 0.0360 0.0239 C7 0.0520 0.0373 0.0301 C8 0.0591 0.0348 0.0274 C9 0.0698 0.0314 0.0221 C10 0.0553 0.0346 0.0232 C11 0.0515 0.0224 0.0167 C12 0.0368 0.0287 0.0190 N1 0.0437 0.0251 0.0203 N2 0.0442 0.0402 0.0214 O1 0.0913 0.0307 0.0238 O2 0.0621 0.0463 0.0341 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.023 0.030 0.037 0.046 0.055 0.072 0.095 0.130 1.000 Number in group 279. 266. 252. 273. 258. 244. 257. 268. 250. 262. GooF 0.880 1.053 1.088 0.953 1.161 1.162 1.065 1.163 1.071 0.977 K 2.205 1.431 1.139 1.034 1.076 1.040 1.042 1.021 1.004 0.959 Resolution(A) 0.77 0.80 0.84 0.88 0.93 1.00 1.07 1.18 1.36 1.69 inf Number in group 263. 260. 268. 253. 264. 258. 259. 266. 256. 262. GooF 1.008 1.049 1.067 1.150 1.083 1.141 0.984 0.940 1.041 1.113 K 1.023 1.155 1.098 1.133 1.048 1.021 1.018 0.966 0.989 0.960 R1 0.312 0.243 0.242 0.225 0.175 0.139 0.094 0.083 0.075 0.067 Recommended weighting scheme: WGHT 0.0860 0.8935 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -2 9 12 -15.94 51.38 5.32 0.054 0.90 0 6 21 43.18 5.86 4.62 0.018 1.01 3 0 9 32.87 7.82 4.48 0.021 1.40 3 0 2 39.03 14.07 4.15 0.028 1.56 -5 5 5 44.07 5.24 3.84 0.017 0.84 2 0 6 96.35 172.63 3.82 0.099 2.10 4 4 21 95.21 33.04 3.78 0.043 0.82 -2 10 11 -5.24 39.22 3.68 0.047 0.84 -1 11 5 20.23 63.92 3.60 0.060 0.85 2 9 0 10.63 57.91 3.60 0.057 0.97 0 3 6 236.60 142.23 3.58 0.090 2.62 0 11 7 -8.77 43.54 3.56 0.050 0.85 -5 2 8 137.25 73.55 3.48 0.065 0.90 3 0 28 184.25 96.19 3.46 0.074 0.83 0 3 3 365.26 238.97 3.44 0.117 3.02 -4 5 12 8.31 28.34 3.43 0.040 0.92 0 9 16 -4.89 24.23 3.40 0.037 0.91 5 0 2 212.43 125.63 3.36 0.085 0.94 4 5 3 32.87 107.76 3.34 0.078 1.00 -2 11 7 1.01 33.37 3.27 0.044 0.80 0 9 2 304.87 195.36 3.26 0.105 1.07 2 0 10 21.46 5.08 3.11 0.017 1.79 1 7 19 2.44 83.48 3.10 0.069 0.97 0 8 17 -6.47 11.02 3.05 0.025 0.96 0 3 26 66.00 25.40 3.03 0.038 1.00 -2 7 16 9.25 42.84 2.97 0.049 0.98 5 0 13 31.96 2.27 2.96 0.011 0.86 2 0 1 429.28 597.15 2.92 0.184 2.35 2 4 28 42.77 11.23 2.90 0.025 0.85 1 1 21 217.74 380.81 2.85 0.147 1.25 0 0 34 -14.51 14.89 2.82 0.029 0.81 0 10 11 0.93 26.23 2.79 0.039 0.90 3 0 3 68.87 35.24 2.74 0.045 1.55 -1 2 25 56.99 103.98 2.73 0.077 1.04 -1 3 5 24.36 11.61 2.73 0.026 2.39 5 0 4 224.64 141.77 2.72 0.090 0.94 0 2 2 23.58 11.56 2.72 0.026 4.54 -2 11 10 -15.29 13.59 2.65 0.028 0.79 -3 4 25 91.83 34.49 2.65 0.044 0.84 2 6 24 -2.41 19.33 2.64 0.033 0.87 3 1 13 126.81 185.48 2.62 0.103 1.25 0 8 26 30.58 75.64 2.60 0.066 0.79 -4 2 15 175.74 121.63 2.58 0.083 0.97 4 0 16 42.84 21.35 2.54 0.035 0.97 -1 3 1 1811.51 1371.80 2.53 0.279 2.64 4 2 19 61.20 30.41 2.52 0.042 0.90 -2 8 9 168.43 83.82 2.50 0.069 1.01 2 2 6 253.07 367.10 2.49 0.144 1.92 -3 4 22 -4.87 14.19 2.47 0.028 0.91 -4 2 19 64.14 30.39 2.46 0.042 0.90 Bond lengths and angles C1 - Distance Angles N1 1.4719 (0.0055) C12 1.5135 (0.0061) 111.86 (0.35) C2 1.5438 (0.0068) 102.20 (0.38) 110.92 (0.42) H1 1.0000 110.54 110.54 110.54 C1 - N1 C12 C2 C2 - Distance Angles C3 1.3900 (0.0085) C1 1.5438 (0.0068) 108.34 (0.48) H2A 0.9900 110.03 110.03 H2B 0.9900 110.03 110.03 108.39 C2 - C3 C1 H2A C3 - Distance Angles C2 1.3900 (0.0085) C4 1.4718 (0.0078) 112.46 (0.49) H3A 0.9900 109.11 109.11 H3B 0.9900 109.11 109.11 107.85 C3 - C2 C4 H3A C4 - Distance Angles N1 1.4666 (0.0055) C3 1.4718 (0.0079) 102.81 (0.38) H4A 0.9900 111.20 111.20 H4B 0.9900 111.20 111.20 109.13 C4 - N1 C3 H4A C5 - Distance Angles O1 1.2326 (0.0052) N1 1.3597 (0.0055) 120.71 (0.40) C6 1.5222 (0.0061) 121.33 (0.39) 117.96 (0.35) C5 - O1 N1 C6 - Distance Angles C5 1.5222 (0.0061) C7 1.5435 (0.0063) 110.39 (0.35) H6A 0.9900 109.58 109.58 H6B 0.9900 109.58 109.58 108.12 C6 - C5 C7 H6A C7 - Distance Angles C8 1.5020 (0.0063) C6 1.5435 (0.0063) 110.00 (0.36) H7A 0.9900 109.66 109.66 H7B 0.9900 109.66 109.66 108.17 C7 - C8 C6 H7A C8 - Distance Angles C9 1.3260 (0.0072) C7 1.5020 (0.0063) 125.80 (0.49) H8 0.9500 117.10 117.10 C8 - C9 C7 C9 - Distance Angles C8 1.3260 (0.0072) C10 1.5069 (0.0070) 126.60 (0.46) H9 0.9500 116.70 116.70 C9 - C8 C10 C10 - Distance Angles C9 1.5069 (0.0070) C11 1.5308 (0.0067) 112.91 (0.39) H10A 0.9900 109.00 109.00 H10B 0.9900 109.00 109.00 107.79 C10 - C9 C11 H10A C11 - Distance Angles N2 1.4607 (0.0056) C10 1.5308 (0.0066) 112.98 (0.38) H11A 0.9900 108.99 108.99 H11B 0.9900 108.99 108.99 107.78 C11 - N2 C10 H11A C12 - Distance Angles O2 1.2386 (0.0047) N2 1.3273 (0.0052) 122.98 (0.43) C1 1.5135 (0.0061) 120.01 (0.41) 117.00 (0.35) C12 - O2 N2 N1 - Distance Angles C5 1.3597 (0.0055) C4 1.4666 (0.0055) 120.94 (0.35) C1 1.4719 (0.0056) 125.96 (0.36) 113.04 (0.35) N1 - C5 C4 N2 - Distance Angles C12 1.3273 (0.0052) C11 1.4607 (0.0056) 122.54 (0.35) H2 0.8800 118.73 118.73 N2 - C12 C11 O1 - Distance Angles C5 1.2326 (0.0052) O1 - O2 - Distance Angles C12 1.2386 (0.0047) O2 - O1W - Distance Angles H1WA 0.8425 (0.0193) H1WB 0.8528 (0.0194) 106.11 (4.09) O1W - H1WA Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.92 2.781(4) 167.8 N2-H2...O2_$1 0.842(19) 1.95(2) 2.783(5) 171(5) O1W-H1WA...O1 0.853(19) 1.99(2) 2.833(5) 172(5) O1W-H1WB...O1W_$2 FMAP and GRID set by program FMAP 2 3 32 GRID -0.862 -2 -2 0.862 2 2 R1 = 0.1161 for 1632 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.4329 0.9370 0.0810 [ 0.83 A from H3A ] Deepest hole -0.38 at 0.7620 0.1461 0.1478 [ 0.84 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2248 / 16282 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0671 0.5630 0.9190 1.00000 0.05 0.34 0.83 H3A 1.14 H3B 1.16 C3 2.27 C4 Q2 1 -0.1390 0.4067 0.8602 1.00000 0.05 0.34 1.09 H2B 1.46 H3A 1.49 C2 1.65 C3 Q3 1 0.0610 0.4791 0.9209 1.00000 0.05 0.29 0.40 C3 0.63 H3B 1.14 H3A 1.55 C4 Q4 1 -0.1161 0.1830 0.8621 1.00000 0.05 0.28 1.00 O2 1.45 C12 1.92 C1 1.98 N1 Q5 1 -0.2836 0.4621 0.8728 1.00000 0.05 0.28 1.09 H3A 1.78 H2A 1.81 C3 1.85 H2B Shortest distances between peaks (including symmetry equivalents) 2 5 0.93 1 3 1.01 1 5 1.90 2 3 2.04 3 5 2.10 2 4 2.15 1 2 2.23 4 5 2.81 Time profile in seconds ----------------------- 0.06: 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. 0.03: 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 3.36: Structure factors and derivatives 1.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s94 finished at 10:01:18 Total CPU time: 5.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++