+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0077p212121 started at 10:54:32 on 05-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0077p212121 in P2(1)2(1)2(1) CELL 0.71073 5.0003 5.9383 19.9866 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0002 0.0010 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O UNIT 16 24 24 V = 593.47 F(000) = 312.0 Mu = 0.16 mm-1 Cell Wt = 600.35 Rho = 1.680 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O3 O4A EQIV_$1 x-1/2, -y+5/2, -z HTAB O1B O1A_$1 EQIV_$2 x+1, y, z HTAB O2 O1B_$2 EQIV_$3 -x+2, y+1/2, -z+1/2 HTAB O3 O4A_$3 EQIV_$4 x, y-1, z HTAB O4B O3_$4 FMAP 2 PLAN 5 SIZE 0.06 0.08 0.12 ACTA BOND $H WGHT 0.00870 0.68490 L.S. 4 TEMP -153.00 FVAR 1.19715 MOLE 1 C1 1 0.580205 0.989504 0.050119 11.00000 0.01609 0.01666 = 0.00927 -0.00184 -0.00400 -0.00192 C2 1 0.647087 0.767837 0.083882 11.00000 0.01239 0.01229 = 0.01468 -0.00122 -0.00015 -0.00039 AFIX 13 H2 2 0.535144 0.646988 0.063151 11.00000 -1.20000 AFIX 0 C3 1 0.584673 0.776095 0.159395 11.00000 0.01675 0.01270 = 0.01463 -0.00045 -0.00090 0.00063 AFIX 13 H3 2 0.387024 0.789493 0.165903 11.00000 -1.20000 AFIX 0 C4 1 0.681311 0.556393 0.190084 11.00000 0.01793 0.01339 = 0.01110 0.00154 0.00305 -0.00052 O1A 3 0.749746 1.100082 0.021763 11.00000 0.01357 0.01985 = 0.02060 0.00535 0.00044 -0.00194 O1B 3 0.325434 1.044444 0.056339 11.00000 0.01351 0.01451 = 0.02085 0.00475 -0.00132 0.00040 AFIX 147 H1 2 0.292709 1.158080 0.032687 11.00000 -1.50000 AFIX 0 O2 3 0.919053 0.712458 0.074201 11.00000 0.01610 0.01463 = 0.02411 0.00427 0.00370 0.00305 AFIX 147 H2A 2 1.009292 0.831175 0.070662 11.00000 -1.50000 AFIX 0 O3 3 0.712635 0.962568 0.189451 11.00000 0.02548 0.00820 = 0.02003 -0.00041 -0.00667 -0.00122 AFIX 147 H3A 2 0.832817 0.916751 0.215470 11.00000 -1.50000 AFIX 0 O4A 3 0.851469 0.552195 0.232674 11.00000 0.02457 0.01633 = 0.02234 0.00257 -0.00776 0.00210 O4B 3 0.559296 0.381472 0.163519 11.00000 0.03011 0.01015 = 0.02114 0.00099 -0.00531 -0.00064 AFIX 147 H4B 2 0.618367 0.262635 0.180877 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0077p212121 in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 Operators for generating equivalent atoms: $1 x-1/2, -y+5/2, -z $2 x+1, y, z $3 -x+2, y+1/2, -z+1/2 $4 x, y-1, z 6364 Reflections read, of which 49 rejected -6 =< h =< 6, -7 =< k =< 7, -25 =< l =< 25, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 832 Unique reflections, of which 0 suppressed R(int) = 0.0773 R(sigma) = 0.0426 Friedel opposites merged Maximum memory for data reduction = 1210 / 8071 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 = 1461 / 123813 wR2 = 0.0873 before cycle 1 for 832 data and 95 / 95 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0087 * P )^2 + 0.68 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19716 0.00338 0.004 OSF Mean shift/esd = 0.002 Maximum = -0.005 for U13 C4 Max. shift = 0.000 A for H2A Max. dU = 0.000 for O4A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1461 / 123813 wR2 = 0.0873 before cycle 2 for 832 data and 95 / 95 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0087 * P )^2 + 0.68 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19717 0.00338 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U13 C4 Max. shift = 0.000 A for H2A Max. dU = 0.000 for O4A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1461 / 123813 wR2 = 0.0873 before cycle 3 for 832 data and 95 / 95 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0087 * P )^2 + 0.68 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19717 0.00338 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1461 / 123813 wR2 = 0.0873 before cycle 4 for 832 data and 95 / 95 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0087 * P )^2 + 0.68 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19716 0.00338 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for O4A No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5351 0.6470 0.0632 13 1.000 0.000 C2 O2 C1 C3 H3 0.3870 0.7895 0.1659 13 1.000 0.000 C3 O3 C4 C2 H1 0.2927 1.1581 0.0327 147 0.840 0.000 O1B C1 H1 H2A 1.0093 0.8312 0.0707 147 0.840 0.000 O2 C2 H2A H3A 0.8328 0.9168 0.2155 147 0.840 0.000 O3 C3 H3A H4B 0.6184 0.2626 0.1809 147 0.840 0.000 O4B C4 H4B 06skc0077p212121 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.58021 0.98950 0.05012 1.00000 0.01609 0.01666 0.00927 -0.00184 -0.00400 -0.00193 0.01401 0.00483 0.00060 0.00048 0.00014 0.00000 0.00138 0.00148 0.00124 0.00107 0.00112 0.00128 0.00061 C2 0.64709 0.76784 0.08388 1.00000 0.01239 0.01229 0.01468 -0.00122 -0.00015 -0.00039 0.01312 0.00494 0.00057 0.00049 0.00014 0.00000 0.00133 0.00133 0.00133 0.00117 0.00118 0.00119 0.00059 H2 0.53514 0.64699 0.06315 1.00000 0.01574 0.00000 0.00000 C3 0.58467 0.77610 0.15939 1.00000 0.01675 0.01270 0.01463 -0.00045 -0.00090 0.00063 0.01469 0.00500 0.00064 0.00047 0.00014 0.00000 0.00143 0.00131 0.00134 0.00113 0.00117 0.00135 0.00061 H3 0.38703 0.78949 0.16590 1.00000 0.01763 0.00000 0.00000 C4 0.68131 0.55639 0.19008 1.00000 0.01792 0.01339 0.01110 0.00154 0.00304 -0.00053 0.01414 0.00515 0.00059 0.00050 0.00014 0.00000 0.00150 0.00131 0.00127 0.00121 0.00119 0.00123 0.00059 O1A 0.74975 1.10008 0.02176 1.00000 0.01358 0.01985 0.02060 0.00534 0.00044 -0.00194 0.01801 0.00368 0.00042 0.00036 0.00010 0.00000 0.00102 0.00107 0.00108 0.00093 0.00092 0.00096 0.00048 O1B 0.32544 1.04444 0.05634 1.00000 0.01351 0.01451 0.02085 0.00475 -0.00132 0.00040 0.01629 0.00363 0.00040 0.00037 0.00010 0.00000 0.00097 0.00097 0.00106 0.00092 0.00087 0.00089 0.00046 H1 0.29271 1.15808 0.03269 1.00000 0.02444 0.00000 0.00000 O2 0.91905 0.71246 0.07420 1.00000 0.01610 0.01463 0.02411 0.00427 0.00371 0.00305 0.01828 0.00394 0.00043 0.00035 0.00011 0.00000 0.00103 0.00099 0.00113 0.00093 0.00090 0.00092 0.00048 H2A 1.00929 0.83118 0.07066 1.00000 0.02742 0.00000 0.00000 O3 0.71264 0.96257 0.18945 1.00000 0.02548 0.00820 0.02003 -0.00041 -0.00667 -0.00122 0.01791 0.00348 0.00046 0.00033 0.00010 0.00000 0.00126 0.00089 0.00106 0.00086 0.00096 0.00088 0.00048 H3A 0.83282 0.91675 0.21547 1.00000 0.02686 0.00000 0.00000 O4A 0.85147 0.55219 0.23267 1.00000 0.02457 0.01633 0.02235 0.00257 -0.00776 0.00209 0.02108 0.00378 0.00045 0.00037 0.00011 0.00000 0.00117 0.00099 0.00108 0.00096 0.00096 0.00101 0.00050 O4B 0.55930 0.38147 0.16352 1.00000 0.03011 0.01015 0.02114 0.00099 -0.00531 -0.00064 0.02046 0.00382 0.00051 0.00034 0.00011 0.00000 0.00127 0.00091 0.00110 0.00082 0.00102 0.00106 0.00051 H4B 0.61837 0.26264 0.18088 1.00000 0.03070 0.00000 0.00000 Final Structure Factor Calculation for 06skc0077p212121 in P2(1)2(1)2(1) Total number of l.s. parameters = 95 Maximum vector length = 511 Memory required = 1368 / 24024 wR2 = 0.0873 before cycle 5 for 832 data and 2 / 95 parameters GooF = S = 1.087; Restrained GooF = 1.087 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0087 * P )^2 + 0.68 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0406 for 730 Fo > 4sig(Fo) and 0.0504 for all 832 data wR2 = 0.0873, GooF = S = 1.087, Restrained GooF = 1.087 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 10.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0186 0.0166 0.0068 C1 0.0152 0.0126 0.0116 C2 0.0172 0.0143 0.0126 C3 0.0191 0.0140 0.0093 C4 0.0257 0.0160 0.0123 O1A 0.0235 0.0139 0.0115 O1B 0.0276 0.0152 0.0121 O2 0.0300 0.0157 0.0080 O3 0.0313 0.0193 0.0126 O4A 0.0326 0.0187 0.0101 O4B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.044 0.059 0.074 0.093 0.113 0.140 0.177 0.252 1.000 Number in group 88. 80. 87. 81. 82. 84. 80. 85. 83. 82. GooF 1.167 1.150 1.137 1.054 1.160 1.046 0.968 1.017 0.954 1.176 K 1.547 1.131 1.022 1.024 0.966 1.013 0.995 1.009 1.006 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.93 0.98 1.07 1.18 1.38 1.77 inf Number in group 87. 81. 84. 83. 85. 80. 84. 81. 84. 83. GooF 1.157 1.154 1.333 1.140 1.017 0.922 0.819 0.893 1.047 1.262 K 1.035 1.065 1.026 1.035 0.974 0.991 0.990 1.006 1.015 0.990 R1 0.140 0.098 0.110 0.091 0.051 0.046 0.028 0.030 0.029 0.023 Recommended weighting scheme: WGHT 0.0090 0.6844 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 5 12 21.02 4.09 3.94 0.024 0.90 6 0 0 87.94 35.70 3.56 0.071 0.83 3 0 20 126.51 82.85 3.48 0.109 0.86 1 6 6 89.20 129.49 3.12 0.136 0.93 5 0 4 31.93 59.55 2.96 0.092 0.98 1 0 1 1579.79 1742.39 2.91 0.498 4.85 1 1 20 3.98 15.32 2.89 0.047 0.97 1 3 2 250.09 214.68 2.57 0.175 1.81 4 0 0 181.19 141.29 2.55 0.142 1.25 3 0 6 26.35 14.67 2.53 0.046 1.49 2 3 18 32.46 18.32 2.53 0.051 0.90 4 5 1 21.38 41.58 2.51 0.077 0.86 1 1 7 1063.85 977.95 2.45 0.373 2.29 5 1 11 -0.82 6.91 2.43 0.031 0.87 6 0 1 14.21 0.04 2.43 0.002 0.83 0 2 19 2.79 12.69 2.40 0.043 0.99 1 2 1 54.37 40.52 2.35 0.076 2.53 1 5 7 126.87 151.60 2.30 0.147 1.07 1 3 22 14.34 3.51 2.28 0.022 0.81 3 0 2 878.84 796.89 2.27 0.337 1.64 5 2 10 15.60 26.96 2.26 0.062 0.86 4 2 6 25.85 37.73 2.25 0.073 1.09 4 0 20 19.19 7.65 2.25 0.033 0.78 4 3 15 102.72 81.10 2.23 0.107 0.83 2 5 18 18.06 6.70 2.21 0.031 0.77 3 1 1 393.65 353.07 2.20 0.224 1.60 0 7 7 -4.81 4.12 2.20 0.024 0.81 0 1 1 843.53 921.58 2.17 0.362 5.69 2 1 4 47.96 35.65 2.17 0.071 2.09 1 7 2 12.96 5.67 2.15 0.028 0.83 4 0 18 27.18 41.24 2.13 0.077 0.83 6 1 5 29.04 16.84 2.13 0.049 0.81 4 0 14 50.45 70.64 2.12 0.100 0.94 1 2 0 1158.92 1074.57 2.11 0.391 2.55 0 7 3 126.11 101.02 2.09 0.120 0.84 2 0 21 6.59 17.81 2.09 0.050 0.89 6 1 9 67.82 50.96 2.08 0.085 0.77 2 0 16 115.82 141.78 2.03 0.142 1.12 0 7 8 91.37 61.98 2.03 0.094 0.80 2 1 5 391.29 354.61 1.98 0.225 2.00 5 0 16 -3.71 1.75 1.98 0.016 0.78 2 2 8 271.76 303.10 1.97 0.208 1.52 0 0 10 624.52 689.94 1.97 0.313 2.00 3 6 11 0.03 14.19 1.96 0.045 0.77 2 5 17 11.43 4.12 1.95 0.024 0.79 1 1 3 844.23 909.61 1.93 0.360 3.32 1 1 0 93.58 111.25 1.93 0.126 3.82 1 5 15 38.61 53.93 1.91 0.088 0.87 5 2 8 55.05 40.32 1.91 0.076 0.89 1 3 0 14.33 8.59 1.90 0.035 1.84 Bond lengths and angles C1 - Distance Angles O1A 1.2129 (0.0035) O1B 1.3209 (0.0037) 125.76 (0.27) C2 1.5165 (0.0038) 121.58 (0.27) 112.66 (0.24) C1 - O1A O1B C2 - Distance Angles O2 1.4124 (0.0036) C1 1.5165 (0.0038) 110.70 (0.24) C3 1.5419 (0.0039) 109.66 (0.24) 111.30 (0.23) H2 1.0000 108.37 108.37 108.37 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4130 (0.0034) C4 1.5205 (0.0038) 110.92 (0.23) C2 1.5419 (0.0039) 110.45 (0.24) 107.65 (0.23) H3 1.0000 109.26 109.26 109.26 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2038 (0.0034) O4B 1.3165 (0.0036) 126.61 (0.28) C3 1.5205 (0.0038) 121.85 (0.27) 111.53 (0.23) C4 - O4A O4B O1A - Distance Angles C1 1.2129 (0.0035) O1A - O1B - Distance Angles C1 1.3209 (0.0037) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4124 (0.0036) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4130 (0.0034) H3A 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2038 (0.0035) O4A - O4B - Distance Angles C4 1.3165 (0.0036) H4B 0.8400 109.47 O4B - C4 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.19 2.677(3) 116.6 O3-H3A...O4A 0.84 1.81 2.653(3) 175.1 O1B-H1...O1A_$1 0.84 2.05 2.854(3) 161.2 O2-H2A...O1B_$2 0.84 2.05 2.731(3) 137.4 O3-H3A...O4A_$3 0.84 1.85 2.654(3) 159.5 O4B-H4B...O3_$4 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0504 for 832 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.9148 0.0283 0.1441 [ 1.41 A from O3 ] Deepest hole -0.26 at 0.7425 0.8618 0.0467 [ 1.04 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1342 / 12219 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9148 1.0283 0.1441 1.00000 0.05 0.25 1.41 O3 1.62 H3A 1.94 H2A 2.16 H4B Q2 1 0.7066 1.1608 0.0787 1.00000 0.05 0.24 1.21 O1A 1.33 C1 2.08 O1B 2.17 H4B Q3 1 0.8920 0.7562 0.2546 1.00000 0.05 0.24 1.27 H3A 1.30 O4A 2.00 O3 2.04 C4 Q4 1 0.7347 1.2014 -0.0075 1.00000 0.05 0.23 0.84 O1A 1.02 H1 1.85 O1B 1.87 C1 Q5 1 0.7670 0.9034 0.2837 1.00000 0.05 0.22 1.40 H3A 1.93 O3 1.95 O4B 2.13 O4A Shortest distances between peaks (including symmetry equivalents) 3 5 1.22 2 4 1.75 1 2 1.85 4 4 2.58 1 3 2.62 1 3 2.74 3 5 2.81 2 4 2.87 1 5 2.98 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. 0.31: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.13: Structure factors and derivatives 0.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0077p212121 finished at 10:54:32 Total CPU time: 0.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++