+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 05mbh1006 started at 11:41:24 on 15-Feb-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 05mbh1006 in C2/c CELL 0.71073 5.0016 14.2136 9.5196 90.000 94.335 90.000 ZERR 4.00 0.0010 0.0028 0.0019 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 32 24 16 V = 674.82 F(000) = 344.0 Mu = 0.13 mm-1 Cell Wt = 664.51 Rho = 1.635 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.07 0.10 0.20 ACTA EQIV $1 -X+1/2, -Y+1/2, -Z+2 HTAB O1 O2_$1 BOND $H WGHT 0.07470 0.36980 L.S. 8 TEMP -153.00 FVAR 0.74675 MOLE 1 O1 3 0.087442 0.145194 0.921374 11.00000 0.01936 0.02267 = 0.02558 -0.00620 0.00991 -0.00175 O2 3 0.484763 0.213928 0.899704 11.00000 0.02201 0.01859 = 0.01804 -0.00199 0.00791 -0.00230 C2 1 0.404735 0.061212 0.800532 11.00000 0.01584 0.01752 = 0.01353 -0.00062 0.00143 0.00035 C4 1 0.399705 -0.109310 0.796184 11.00000 0.02308 0.01757 = 0.01794 0.00218 0.00118 -0.00280 C1 1 0.329667 0.148494 0.875284 11.00000 0.01786 0.01875 = 0.01230 0.00111 0.00335 0.00136 C3 1 0.305429 -0.024103 0.846122 11.00000 0.01758 0.02208 = 0.01459 0.00069 0.00374 -0.00088 H3 2 0.176554 -0.024071 0.915983 11.00000 0.02343 H4 2 0.329388 -0.167597 0.829543 11.00000 0.02639 H1 2 0.067638 0.197376 0.979596 11.00000 0.06407 HKLF 4 Covalent radii and connectivity table for 05mbh1006 in C2/c C 0.770 H 0.320 O 0.660 O1 - C1 O2 - C1 C2 - C3 C2_$2 C1 C4 - C4_$2 C3 C1 - O2 O1 C2 C3 - C2 C4 Operators for generating equivalent atoms: $1 -x+1/2, -y+1/2, -z+2 $2 -x+1, y, -z+3/2 3274 Reflections read, of which 50 rejected -6 =< h =< 6, -18 =< k =< 18, -11 =< l =< 12, Max. 2-theta = 54.92 0 Systematic absence violations 0 Inconsistent equivalents 774 Unique reflections, of which 0 suppressed R(int) = 0.0337 R(sigma) = 0.0331 Friedel opposites merged Maximum memory for data reduction = 788 / 9215 Least-squares cycle 1 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 1 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74677 0.00376 0.006 OSF Mean shift/esd = 0.013 Maximum = 0.058 for U22 C3 Max. shift = 0.001 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 2 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74682 0.00376 0.014 OSF Mean shift/esd = 0.005 Maximum = 0.020 for U22 C3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 3 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for x H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 4 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 5 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 6 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 7 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 945 / 92859 wR2 = 0.1197 before cycle 8 for 774 data and 67 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74683 0.00376 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H4 No correlation matrix elements larger than 0.500 05mbh1006 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.08744 0.14519 0.92137 1.00000 0.01939 0.02268 0.02561 -0.00620 0.00992 -0.00175 0.02214 0.00200 0.00021 0.00008 0.00012 0.00000 0.00063 0.00059 0.00063 0.00046 0.00045 0.00041 0.00034 O2 0.48476 0.21393 0.89970 1.00000 0.02203 0.01860 0.01805 -0.00199 0.00793 -0.00230 0.01924 0.00181 0.00020 0.00007 0.00011 0.00000 0.00062 0.00059 0.00061 0.00039 0.00044 0.00039 0.00034 C2 0.40474 0.06121 0.80053 1.00000 0.01586 0.01754 0.01355 -0.00061 0.00142 0.00036 0.01563 0.00244 0.00028 0.00010 0.00015 0.00000 0.00072 0.00077 0.00070 0.00052 0.00054 0.00051 0.00037 C4 0.39971 -0.10931 0.79618 1.00000 0.02310 0.01759 0.01796 0.00219 0.00117 -0.00281 0.01957 0.00269 0.00031 0.00011 0.00016 0.00000 0.00080 0.00078 0.00076 0.00055 0.00060 0.00055 0.00039 C1 0.32967 0.14849 0.87528 1.00000 0.01789 0.01877 0.01230 0.00112 0.00335 0.00136 0.01621 0.00254 0.00029 0.00010 0.00015 0.00000 0.00076 0.00074 0.00069 0.00052 0.00053 0.00051 0.00037 C3 0.30542 -0.02410 0.84612 1.00000 0.01758 0.02214 0.01460 0.00069 0.00375 -0.00088 0.01798 0.00264 0.00030 0.00010 0.00016 0.00000 0.00074 0.00080 0.00072 0.00056 0.00058 0.00052 0.00038 H3 0.17657 -0.02403 0.91597 1.00000 0.02344 0.03229 0.00383 0.00128 0.00212 0.00000 0.00468 H4 0.32952 -0.16755 0.82953 1.00000 0.02642 0.03421 0.00355 0.00142 0.00218 0.00000 0.00476 H1 0.06763 0.19733 0.97947 1.00000 0.06414 0.05148 0.00537 0.00195 0.00320 0.00000 0.00801 Final Structure Factor Calculation for 05mbh1006 in C2/c Total number of l.s. parameters = 67 Maximum vector length = 511 Memory required = 878 / 21973 wR2 = 0.1197 before cycle 9 for 774 data and 0 / 67 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0747 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0423 for 643 Fo > 4sig(Fo) and 0.0534 for all 774 data wR2 = 0.1197, GooF = S = 1.053, Restrained GooF = 1.053 for all data Occupancy sum of asymmetric unit = 6.00 for non-hydrogen and 3.00 for hydrogen atoms Principal mean square atomic displacements U 0.0339 0.0201 0.0124 O1 0.0273 0.0176 0.0128 O2 0.0177 0.0158 0.0134 C2 0.0246 0.0191 0.0150 C4 0.0203 0.0171 0.0113 C1 0.0223 0.0188 0.0128 C3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.025 0.038 0.052 0.067 0.082 0.106 0.136 0.191 1.000 Number in group 88. 68. 78. 83. 72. 75. 80. 76. 78. 76. GooF 0.913 1.112 0.978 1.116 1.079 1.068 1.185 0.999 1.089 0.976 K 0.442 0.895 0.943 0.932 0.973 0.985 1.000 1.037 1.042 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.31 1.66 inf Number in group 78. 77. 80. 76. 78. 77. 76. 78. 76. 78. GooF 0.926 1.132 1.164 0.952 1.045 0.877 1.153 1.102 0.820 1.261 K 0.965 1.061 1.042 1.025 1.053 1.018 1.058 1.038 1.032 0.962 R1 0.123 0.098 0.105 0.071 0.053 0.041 0.047 0.035 0.028 0.035 Recommended weighting scheme: WGHT 0.0749 0.3661 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) 4 2 0 189.96 291.02 4.50 0.123 1.23 1 5 1 12.87 4.94 4.02 0.016 2.37 -1 11 5 98.94 146.76 3.63 0.087 1.05 -5 5 7 214.33 137.10 3.50 0.084 0.80 -2 2 4 117.26 165.23 3.45 0.092 1.73 -3 1 6 31.55 53.67 3.36 0.053 1.19 -2 10 5 28.85 47.72 3.35 0.050 1.05 -1 13 5 81.56 114.80 2.83 0.077 0.94 -2 2 2 8.51 3.56 2.81 0.014 2.17 -1 1 1 524.53 660.47 2.75 0.185 4.34 -4 2 8 38.93 61.27 2.71 0.056 0.89 5 9 2 8.68 21.07 2.62 0.033 0.82 1 1 11 63.06 88.62 2.48 0.068 0.84 0 16 4 538.84 423.94 2.47 0.148 0.83 2 14 5 60.90 84.63 2.37 0.066 0.83 -3 11 7 828.87 675.78 2.32 0.187 0.83 -1 11 4 -0.28 4.06 2.22 0.014 1.12 -6 2 2 -10.33 5.17 2.21 0.016 0.82 5 1 0 28.08 41.79 2.20 0.046 1.00 0 14 6 449.74 369.43 2.17 0.138 0.85 -2 10 7 244.90 200.22 2.15 0.102 0.93 -4 0 6 209.77 257.46 2.13 0.115 1.02 0 6 0 787.33 943.47 2.12 0.221 2.37 5 7 1 161.92 208.24 2.10 0.104 0.89 5 11 0 177.34 140.20 2.09 0.085 0.79 1 5 2 481.48 405.94 2.09 0.145 2.16 0 4 12 103.97 136.47 2.07 0.084 0.77 -3 15 2 14.81 28.68 2.06 0.039 0.82 3 7 2 8.37 13.85 2.05 0.027 1.22 3 7 1 146.28 120.93 2.02 0.079 1.26 -3 13 5 16.30 27.95 2.01 0.038 0.84 -1 11 3 26.51 18.44 2.01 0.031 1.17 2 0 10 32.13 50.53 2.01 0.051 0.87 -3 3 4 166.26 137.99 2.01 0.084 1.35 -1 7 9 516.84 434.17 1.99 0.150 0.93 1 1 1 2062.96 2419.31 1.98 0.354 4.10 5 7 2 29.24 13.15 1.98 0.026 0.87 -5 3 4 6.10 11.06 1.95 0.024 0.93 4 2 8 94.85 121.59 1.93 0.079 0.82 -4 12 5 439.61 355.80 1.92 0.136 0.80 0 8 5 230.59 194.97 1.91 0.100 1.30 0 12 2 -2.91 0.92 1.90 0.007 1.15 -1 1 6 499.81 428.59 1.90 0.149 1.53 -2 0 8 86.94 108.17 1.89 0.075 1.10 -1 15 2 21.98 11.26 1.88 0.024 0.92 0 16 3 76.67 101.11 1.88 0.072 0.86 0 4 0 1445.64 1689.54 1.87 0.295 3.55 1 3 2 980.50 1141.82 1.87 0.243 2.72 1 1 0 3042.91 3528.13 1.85 0.427 4.71 0 14 8 3.53 22.58 1.85 0.034 0.77 Bond lengths and angles O1 - Distance Angles C1 1.3202 (0.0018) H1 0.9345 (0.0302) 108.03 (1.67) O1 - C1 O2 - Distance Angles C1 1.2221 (0.0018) O2 - C2 - Distance Angles C3 1.3921 (0.0020) C2_$2 1.4044 (0.0030) 119.35 (0.09) C1 1.4923 (0.0020) 117.83 (0.13) 122.34 (0.08) C2 - C3 C2_$2 C4 - Distance Angles C4_$2 1.3830 (0.0032) C3 1.3961 (0.0022) 119.76 (0.09) H4 0.9623 (0.0202) 120.66 (1.17) 119.53 (1.19) C4 - C4_$2 C3 C1 - Distance Angles O2 1.2221 (0.0018) O1 1.3202 (0.0018) 123.30 (0.13) C2 1.4923 (0.0020) 122.99 (0.13) 113.53 (0.12) C1 - O2 O1 C3 - Distance Angles C2 1.3921 (0.0020) C4 1.3961 (0.0022) 120.78 (0.14) H3 0.9604 (0.0209) 119.26 (1.10) 119.89 (1.10) C3 - C2 C4 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.93(3) 1.74(3) 2.6710(15) 174(3) O1-H1...O2_$1 FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -1 -2 4.167 1 2 R1 = 0.0534 for 774 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.1250 0.3991 0.1603 [ 0.70 A from C2 ] Deepest hole -0.26 at 0.1696 0.3984 0.0762 [ 0.81 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1285 / 14844 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3750 0.1009 0.8397 1.00000 0.05 0.21 0.70 C2 0.80 C1 1.78 O2 1.80 O1 Q2 1 0.3832 0.2300 0.7926 1.00000 0.05 0.19 1.13 O2 1.44 C1 2.01 O2 2.10 H4 Q3 1 -0.2553 0.0922 0.8970 1.00000 0.05 0.19 1.87 O1 1.92 C2 2.02 C2 2.04 H3 Q4 1 0.6412 0.2921 0.9311 1.00000 0.05 0.18 1.38 O2 1.40 H1 1.51 H4 2.08 O1 Q5 1 0.6984 0.2249 0.9095 1.00000 0.05 0.18 1.08 O2 1.85 H4 1.95 H1 2.08 H1 Shortest distances between peaks (including symmetry equivalents) 4 5 1.02 2 2 1.47 4 5 1.68 2 5 1.86 1 2 1.89 1 3 1.89 5 5 1.90 3 5 1.90 2 5 1.94 2 4 1.98 4 4 2.03 1 1 2.19 1 3 2.29 2 4 2.30 3 4 2.36 1 5 2.45 1 2 2.58 2 3 2.71 2 3 2.80 3 4 2.91 1 5 2.95 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 0.00: Analyse other restraints etc. 0.25: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.02: Generate idealized H-atoms 0.16: Structure factors and derivatives 0.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 05mbh1006 finished at 11:41:25 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++