+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0051p21c started at 12:29:23 on 27-Nov-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0051p21c in P2(1)/c CELL 0.71073 3.9015 17.3293 13.8628 90.000 96.299 90.000 ZERR 4.00 0.0002 0.0010 0.0007 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 48 8 16 V = 931.61 F(000) = 424.0 Mu = 0.12 mm-1 Cell Wt = 800.78 Rho = 1.427 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N23 O31A EQIV_$1 -x, y-1/2, -z+3/2 HTAB O1B O31A_$1 EQIV_$2 x, -y+1/2, z-1/2 HTAB N21 O31B_$2 FMAP 2 PLAN 10 EQIV_$3 -x, -y+1, -z+2 MPLA C31 O31A O31B MPLA C31_$3 O31A_$3 O31B_$3 SIZE 0.06 0.07 0.10 ACTA BOND $H WGHT 0.04250 0.45420 L.S. 8 TEMP -153.00 FVAR 0.69871 MOLE 1 C1 1 0.236282 -0.033445 0.880977 11.00000 0.01999 0.02194 = 0.01797 0.00014 0.00170 0.00183 C2 1 0.427741 0.020029 0.953501 11.00000 0.02207 0.02164 = 0.01883 -0.00135 0.00080 -0.00064 AFIX 23 H2A 2 0.269745 0.061636 0.969633 11.00000 -1.20000 H2B 2 0.619801 0.044291 0.923465 11.00000 -1.20000 AFIX 0 O1A 4 0.184000 -0.100878 0.896665 11.00000 0.04534 0.02368 = 0.02450 0.00154 -0.00731 -0.00942 O1B 4 0.126105 0.002169 0.799398 11.00000 0.04016 0.02306 = 0.01853 0.00078 -0.00659 -0.00409 AFIX 147 H1 2 0.025855 -0.029618 0.760160 11.00000 0.05831 AFIX 0 MOLE 2 C22 1 0.303148 0.258726 0.670504 11.00000 0.02914 0.02299 = 0.01954 -0.00048 0.00261 0.00082 AFIX 43 H22 2 0.167542 0.290089 0.624843 11.00000 -1.20000 AFIX 0 C24 1 0.603701 0.218332 0.805022 11.00000 0.02145 0.01930 = 0.02102 0.00203 0.00257 -0.00073 C25 1 0.600740 0.161664 0.737838 11.00000 0.02703 0.01871 = 0.02220 0.00124 0.00262 0.00371 AFIX 43 H25 2 0.709013 0.112679 0.746580 11.00000 -1.20000 AFIX 0 C26 1 0.767291 0.222330 0.906884 11.00000 0.02740 0.02556 = 0.02322 -0.00073 -0.00118 -0.00018 AFIX 137 H26A 2 0.587838 0.223311 0.951101 11.00000 -1.50000 H26B 2 0.907206 0.269282 0.915765 11.00000 -1.50000 H26C 2 0.914711 0.177034 0.920958 11.00000 -1.50000 AFIX 0 N21 3 0.412077 0.187902 0.654377 11.00000 0.02971 0.02109 = 0.01790 -0.00288 0.00173 0.00102 AFIX 43 H21 2 0.370941 0.162043 0.599700 11.00000 0.04217 AFIX 0 N23 3 0.414442 0.278490 0.760637 11.00000 0.02714 0.01785 = 0.01918 -0.00179 0.00333 0.00193 AFIX 43 H23 2 0.374377 0.322914 0.788039 11.00000 0.04717 AFIX 0 MOLE 3 C31 1 0.188420 0.423557 0.916594 11.00000 0.01971 0.01773 = 0.01701 -0.00110 -0.00029 -0.00311 C32 1 0.024476 0.497638 0.946285 11.00000 0.02168 0.01778 = 0.01671 0.00052 0.00120 0.00160 AFIX 23 H32B 2 -0.203312 0.503342 0.907806 11.00000 -1.20000 H32A 2 0.169789 0.541529 0.929859 11.00000 -1.20000 AFIX 0 O31B 4 0.314123 0.376068 0.977558 11.00000 0.03344 0.02159 = 0.01871 0.00217 -0.00099 0.00475 O31A 4 0.196117 0.413533 0.825376 11.00000 0.03725 0.02476 = 0.01402 -0.00197 -0.00102 0.00998 HKLF 4 Covalent radii and connectivity table for 06skc0051p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C2_$4 O1A - C1 O1B - C1 C22 - N23 N21 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 C31 - O31B O31A C32 C32 - C31 C32_$3 O31B - C31 O31A - C31 Operators for generating equivalent atoms: $1 -x, y-1/2, -z+3/2 $2 x, -y+1/2, z-1/2 $3 -x, -y+1, -z+2 $4 -x+1, -y, -z+2 10034 Reflections read, of which 254 rejected -5 =< h =< 4, -22 =< k =< 22, -17 =< l =< 17, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2117 Unique reflections, of which 0 suppressed R(int) = 0.0718 R(sigma) = 0.0599 Friedel opposites merged Maximum memory for data reduction = 1678 / 21320 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 = 2050 / 166941 wR2 = 0.1169 before cycle 1 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.001 OSF Mean shift/esd = 0.002 Maximum = -0.006 for U23 O1A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 2 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U23 O1A Max. shift = 0.000 A for H26B Max. dU = 0.000 for H21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 3 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O31B Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 4 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O31A Max. shift = 0.000 A for C1 Max. dU = 0.000 for H21 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 5 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O31A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 6 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O31A Max. shift = 0.000 A for C2 Max. dU = 0.000 for H21 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 7 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O31A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H23 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2050 / 166941 wR2 = 0.1169 before cycle 8 for 2117 data and 132 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69871 0.00182 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O31A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.2697 0.0616 0.9696 23 0.990 0.000 C2 C1 C2_$4 H2B 0.6198 0.0443 0.9235 23 0.990 0.000 C2 C1 C2_$4 H1 0.0259 -0.0296 0.7602 147 0.840 0.000 O1B C1 H1 H22 0.1675 0.2901 0.6248 43 0.950 0.000 C22 N23 N21 H25 0.7090 0.1127 0.7466 43 0.950 0.000 C25 C24 N21 H26A 0.5878 0.2233 0.9511 137 0.980 0.000 C26 C24 H26A H26B 0.9072 0.2693 0.9158 137 0.980 0.000 C26 C24 H26A H26C 0.9147 0.1770 0.9210 137 0.980 0.000 C26 C24 H26A H21 0.3709 0.1620 0.5997 43 0.880 0.000 N21 C22 C25 H23 0.3744 0.3229 0.7880 43 0.880 0.000 N23 C22 C24 H32B -0.2033 0.5033 0.9078 23 0.990 0.000 C32 C31 C32_$3 H32A 0.1698 0.5415 0.9299 23 0.990 0.000 C32 C31 C32_$3 06skc0051p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.23628 -0.03345 0.88098 1.00000 0.01999 0.02194 0.01797 0.00014 0.00170 0.00183 0.01999 0.00330 0.00045 0.00011 0.00012 0.00000 0.00090 0.00098 0.00089 0.00074 0.00068 0.00078 0.00039 C2 0.42774 0.02003 0.95350 1.00000 0.02207 0.02164 0.01883 -0.00135 0.00080 -0.00064 0.02095 0.00315 0.00047 0.00011 0.00012 0.00000 0.00092 0.00099 0.00089 0.00074 0.00070 0.00075 0.00041 H2A 0.26975 0.06164 0.96963 1.00000 0.02514 0.00000 0.00000 H2B 0.61980 0.04429 0.92347 1.00000 0.02514 0.00000 0.00000 O1A 0.18400 -0.10088 0.89667 1.00000 0.04534 0.02368 0.02450 0.00154 -0.00731 -0.00942 0.03200 0.00239 0.00038 0.00008 0.00010 0.00000 0.00089 0.00079 0.00071 0.00058 0.00060 0.00066 0.00036 O1B 0.12611 0.00217 0.79940 1.00000 0.04016 0.02306 0.01853 0.00078 -0.00659 -0.00409 0.02798 0.00245 0.00037 0.00008 0.00009 0.00000 0.00083 0.00073 0.00067 0.00057 0.00057 0.00064 0.00034 H1 0.02586 -0.02962 0.76016 1.00000 0.05831 0.00000 0.00842 C22 0.30315 0.25873 0.67050 1.00000 0.02914 0.02299 0.01954 -0.00048 0.00261 0.00082 0.02389 0.00337 0.00049 0.00011 0.00013 0.00000 0.00102 0.00101 0.00093 0.00077 0.00074 0.00084 0.00042 H22 0.16754 0.29009 0.62484 1.00000 0.02867 0.00000 0.00000 C24 0.60370 0.21833 0.80502 1.00000 0.02145 0.01930 0.02102 0.00203 0.00257 -0.00073 0.02057 0.00330 0.00047 0.00011 0.00013 0.00000 0.00091 0.00095 0.00091 0.00073 0.00068 0.00076 0.00040 C25 0.60074 0.16166 0.73784 1.00000 0.02703 0.01871 0.02220 0.00124 0.00262 0.00371 0.02265 0.00339 0.00049 0.00011 0.00013 0.00000 0.00097 0.00096 0.00092 0.00075 0.00072 0.00081 0.00041 H25 0.70901 0.11268 0.74658 1.00000 0.02718 0.00000 0.00000 C26 0.76729 0.22233 0.90688 1.00000 0.02740 0.02556 0.02322 -0.00073 -0.00118 -0.00018 0.02569 0.00344 0.00050 0.00012 0.00013 0.00000 0.00102 0.00106 0.00097 0.00079 0.00075 0.00085 0.00044 H26A 0.58784 0.22331 0.95110 1.00000 0.03853 0.00000 0.00000 H26B 0.90721 0.26928 0.91577 1.00000 0.03853 0.00000 0.00000 H26C 0.91471 0.17703 0.92096 1.00000 0.03853 0.00000 0.00000 N21 0.41208 0.18790 0.65438 1.00000 0.02971 0.02109 0.01790 -0.00288 0.00173 0.00102 0.02296 0.00282 0.00041 0.00009 0.00011 0.00000 0.00087 0.00085 0.00077 0.00065 0.00062 0.00070 0.00037 H21 0.37094 0.16204 0.59970 1.00000 0.04217 0.00000 0.00671 N23 0.41444 0.27849 0.76064 1.00000 0.02714 0.01785 0.01918 -0.00179 0.00333 0.00193 0.02133 0.00277 0.00040 0.00009 0.00011 0.00000 0.00084 0.00081 0.00078 0.00062 0.00061 0.00068 0.00036 H23 0.37438 0.32291 0.78804 1.00000 0.04717 0.00000 0.00723 C31 0.18842 0.42356 0.91659 1.00000 0.01971 0.01773 0.01701 -0.00110 -0.00029 -0.00311 0.01832 0.00304 0.00045 0.00010 0.00012 0.00000 0.00089 0.00092 0.00087 0.00071 0.00067 0.00073 0.00039 C32 0.02448 0.49764 0.94629 1.00000 0.02168 0.01778 0.01671 0.00052 0.00120 0.00160 0.01879 0.00321 0.00046 0.00010 0.00012 0.00000 0.00092 0.00090 0.00086 0.00069 0.00067 0.00075 0.00039 H32B -0.20331 0.50334 0.90781 1.00000 0.02255 0.00000 0.00000 H32A 0.16979 0.54153 0.92986 1.00000 0.02255 0.00000 0.00000 O31B 0.31412 0.37607 0.97756 1.00000 0.03344 0.02159 0.01871 0.00217 -0.00099 0.00475 0.02487 0.00230 0.00034 0.00007 0.00009 0.00000 0.00076 0.00071 0.00066 0.00054 0.00053 0.00059 0.00033 O31A 0.19612 0.41353 0.82538 1.00000 0.03725 0.02476 0.01402 -0.00197 -0.00102 0.00998 0.02563 0.00234 0.00035 0.00008 0.00009 0.00000 0.00079 0.00074 0.00063 0.00053 0.00053 0.00061 0.00034 Final Structure Factor Calculation for 06skc0051p21c in P2(1)/c Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1918 / 22995 wR2 = 0.1169 before cycle 9 for 2117 data and 0 / 132 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 0.45 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0490 for 1562 Fo > 4sig(Fo) and 0.0744 for all 2117 data wR2 = 0.1169, GooF = S = 1.022, Restrained GooF = 1.022 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0231 0.0190 0.0179 C1 0.0228 0.0222 0.0179 C2 0.0545 0.0226 0.0189 O1A 0.0460 0.0223 0.0157 O1B 0.0293 0.0230 0.0194 C22 0.0225 0.0215 0.0177 C24 0.0284 0.0224 0.0171 C25 0.0303 0.0257 0.0211 C26 0.0301 0.0226 0.0162 N21 0.0275 0.0204 0.0160 N23 0.0225 0.0184 0.0141 C31 0.0224 0.0177 0.0162 C32 0.0361 0.0224 0.0162 O31B 0.0440 0.0192 0.0136 O31A Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.032 0.042 0.054 0.069 0.089 0.128 1.000 Number in group 221. 222. 218. 193. 220. 198. 209. 213. 213. 210. GooF 0.871 1.017 1.110 1.011 1.090 1.059 0.995 1.054 0.996 1.001 K 3.567 1.564 1.063 1.018 0.980 1.005 1.004 1.029 1.019 0.982 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.67 inf Number in group 219. 209. 215. 207. 211. 212. 213. 207. 212. 212. GooF 0.949 0.947 1.021 1.045 0.991 0.894 0.891 0.994 1.056 1.356 K 1.004 1.068 1.091 1.014 1.013 1.010 1.003 1.002 1.024 0.972 R1 0.226 0.169 0.152 0.110 0.098 0.057 0.038 0.046 0.040 0.034 Recommended weighting scheme: WGHT 0.0425 0.4542 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 6 6 46.15 8.34 6.81 0.019 1.80 -3 6 3 95.45 38.42 5.32 0.042 1.17 0 4 0 3492.62 4283.81 3.59 0.439 4.33 -4 7 5 110.81 152.43 3.39 0.083 0.89 1 0 6 206.97 160.04 3.37 0.085 1.89 -1 0 2 221.52 176.27 3.22 0.089 3.55 0 4 14 18.54 5.42 3.08 0.016 0.96 -1 0 10 24.33 9.26 3.05 0.020 1.35 0 6 1 140.28 106.92 3.04 0.069 2.83 0 2 2 3928.08 4551.25 2.94 0.452 5.39 2 5 9 65.49 92.08 2.90 0.064 1.08 2 4 2 344.32 287.22 2.86 0.114 1.67 2 12 12 48.00 14.35 2.81 0.025 0.79 3 9 6 44.31 64.72 2.80 0.054 0.94 4 3 2 31.56 17.02 2.80 0.028 0.93 2 7 8 32.26 56.65 2.79 0.050 1.10 0 0 4 90.96 116.98 2.78 0.073 3.44 2 6 13 227.44 165.34 2.78 0.086 0.85 -2 17 3 18.77 36.29 2.74 0.040 0.89 -1 9 5 8.50 2.78 2.73 0.011 1.50 3 13 1 36.82 22.58 2.72 0.032 0.92 2 6 7 72.45 97.97 2.71 0.066 1.19 -3 9 6 16.15 7.19 2.70 0.018 1.01 0 7 7 45.94 30.92 2.70 0.037 1.54 1 16 8 100.23 63.85 2.68 0.054 0.88 -2 15 6 421.09 336.37 2.68 0.123 0.93 0 3 3 530.84 615.79 2.66 0.166 3.60 1 2 6 45.69 32.00 2.65 0.038 1.84 1 0 12 49.78 30.36 2.64 0.037 1.07 -1 11 13 74.13 46.29 2.64 0.046 0.87 1 20 6 -8.75 12.08 2.63 0.023 0.79 -3 6 6 816.52 693.40 2.62 0.177 1.09 -4 12 1 12.38 34.44 2.62 0.039 0.81 1 5 1 43.71 27.18 2.61 0.035 2.51 0 12 3 179.45 141.77 2.59 0.080 1.38 0 20 0 126.81 73.69 2.56 0.058 0.87 -2 14 1 50.02 91.37 2.55 0.064 1.05 -2 1 4 15.14 7.82 2.54 0.019 1.77 -4 8 2 34.48 15.65 2.53 0.027 0.89 0 1 5 435.54 377.06 2.53 0.130 2.72 1 5 5 5.16 12.12 2.52 0.023 1.82 -2 10 12 25.99 40.76 2.51 0.043 0.89 3 10 8 19.02 1.82 2.51 0.009 0.86 2 18 6 99.06 50.98 2.50 0.048 0.79 2 13 10 24.15 46.36 2.50 0.046 0.83 1 4 4 8.68 3.08 2.44 0.012 2.13 3 13 3 38.08 57.70 2.42 0.051 0.90 -3 6 11 22.25 36.85 2.39 0.041 0.91 -2 15 3 23.75 10.16 2.37 0.021 0.98 0 7 12 0.58 7.36 2.37 0.018 1.04 Bond lengths and angles C1 - Distance Angles O1A 1.2100 (0.0023) O1B 1.3183 (0.0021) 124.11 (0.17) C2 1.5042 (0.0025) 123.78 (0.16) 112.10 (0.16) C1 - O1A O1B C2 - Distance Angles C1 1.5042 (0.0025) C2_$4 1.5173 (0.0035) 113.39 (0.19) H2A 0.9900 108.89 108.89 H2B 0.9900 108.89 108.89 107.73 C2 - C1 C2_$4 H2A O1A - Distance Angles C1 1.2100 (0.0023) O1A - O1B - Distance Angles C1 1.3183 (0.0021) H1 0.8400 109.47 O1B - C1 C22 - Distance Angles N23 1.3221 (0.0024) N21 1.3258 (0.0025) 108.73 (0.17) H22 0.9500 125.64 125.64 C22 - N23 N21 C24 - Distance Angles C25 1.3526 (0.0026) N23 1.3824 (0.0024) 106.10 (0.16) C26 1.4861 (0.0025) 131.18 (0.18) 122.72 (0.16) C24 - C25 N23 C25 - Distance Angles C24 1.3526 (0.0026) N21 1.3785 (0.0024) 107.57 (0.16) H25 0.9500 126.21 126.21 C25 - C24 N21 C26 - Distance Angles C24 1.4861 (0.0025) 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 1.3258 (0.0025) C25 1.3785 (0.0024) 108.38 (0.15) H21 0.8800 125.81 125.81 N21 - C22 C25 N23 - Distance Angles C22 1.3221 (0.0024) C24 1.3824 (0.0024) 109.23 (0.16) H23 0.8800 125.39 125.39 N23 - C22 C24 C31 - Distance Angles O31B 1.2414 (0.0021) O31A 1.2800 (0.0020) 122.16 (0.16) C32 1.5114 (0.0025) 121.67 (0.15) 116.16 (0.15) C31 - O31B O31A C32 - Distance Angles C31 1.5114 (0.0025) C32_$3 1.5243 (0.0032) 114.44 (0.19) H32B 0.9900 108.65 108.65 H32A 0.9900 108.65 108.65 107.59 C32 - C31 C32_$3 H32B O31B - Distance Angles C31 1.2414 (0.0021) O31B - O31A - Distance Angles C31 1.2800 (0.0020) O31A - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.82 2.679(2) 166.3 N23-H23...O31A 0.84 1.70 2.5406(18) 174.3 O1B-H1...O31A_$1 0.88 1.81 2.679(2) 169.9 N21-H21...O31B_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 3.4231 (0.0060) x + 8.2656 (0.0476) y - 0.6195 (0.0197) z = 3.5781 (0.0333) * 0.0000 (0.0000) C31 * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B Rms deviation of fitted atoms = 0.0000 3.4231 (0.0061) x + 8.2656 (0.0476) y - 0.6195 (0.0198) z = 3.4485 (0.0484) Angle to previous plane (with approximate esd) = 0.00 ( 0.38 ) * 0.0000 (0.0001) C31_$3 * 0.0000 (0.0000) O31A_$3 * 0.0000 (0.0000) O31B_$3 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 12 GRID -5.556 24 -2 5.556 1 2 R1 = 0.0744 for 2117 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.4239 0.2798 0.5372 [ 1.42 A from H26A ] Deepest hole -0.26 at 0.3790 0.2791 0.2395 [ 1.04 A from N23 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2500 / 23505 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4239 0.2202 1.0372 1.00000 0.05 0.22 1.42 H26A 1.67 H22 1.99 C22 2.24 H21 Q2 1 0.3819 0.3813 0.8115 1.00000 0.05 0.20 0.95 O31A 1.06 H23 1.86 C31 1.92 N23 Q3 1 0.3357 -0.1391 0.9561 1.00000 0.05 0.20 1.17 O1A 1.95 H26A 2.12 C1 2.16 H26C Q4 1 0.5647 0.2758 0.9579 1.00000 0.05 0.20 0.92 H26A 1.45 C26 1.52 H26B 2.03 O31B Q5 1 0.3354 0.1845 0.9770 1.00000 0.05 0.19 1.28 H26A 1.74 H26C 2.14 C26 2.15 H2A Q6 1 0.3458 -0.0259 0.8013 1.00000 0.05 0.19 0.98 O1B 1.23 C1 1.32 H1 2.00 O1A Q7 1 0.2025 0.0231 0.6993 1.00000 0.05 0.19 1.47 H1 1.50 O1B 1.52 H32B 2.16 C32 Q8 1 0.7413 0.1214 0.9517 1.00000 0.05 0.19 1.28 H26C 1.46 H2B 1.86 C26 1.87 H26A Q9 1 0.6066 0.1667 0.9662 1.00000 0.05 0.19 1.00 H26A 1.43 H26C 1.45 C26 2.20 H2B Q10 1 0.1300 0.4004 1.0118 1.00000 0.05 0.18 1.00 O31B 1.42 C31 1.80 H32A 1.81 H21 Shortest distances between peaks (including symmetry equivalents) 8 9 0.98 1 5 1.06 5 9 1.13 3 9 1.18 3 8 1.38 1 9 1.58 1 4 1.60 1 3 1.69 6 7 1.69 3 5 1.69 4 5 1.85 4 9 1.90 5 8 1.99 1 8 2.49 2 6 2.55 3 4 2.66 2 4 2.77 4 8 2.77 4 10 2.89 7 10 2.90 3 6 2.91 2 7 2.96 Time profile in seconds ----------------------- 0.08: 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. 0.55: 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 0.59: Structure factors and derivatives 0.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0051p21c finished at 12:29:25 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++