+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0949_295 started at 10:59:24 on 15-Dec-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0949_295 R-3m CELL 0.71073 7.3353 7.3353 16.9570 90.000 90.000 120.000 ZERR 3.00 0.0010 0.0010 0.0030 0.000 0.000 0.000 LATT 3 SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM Y, X, - Z SYMM - X, - X + Y, - Z SYMM X - Y, - Y, - Z SFAC H FE O S UNIT 18 9 45 6 V = 790.16 F(000) = 708.0 Mu = 4.57 mm-1 Cell Wt = 1433.15 Rho = 3.012 MERG 2 OMIT -3.00 55.00 EXTI 0.00898 FMAP 2 PLAN 10 SIZE 0.08 0.08 0.08 ACTA WGHT 0.02860 3.40830 L.S. 6 TEMP 22.00 FVAR 0.38252 FE1 2 0.333333 0.166667 0.166667 10.25000 0.01000 0.01314 = 0.01320 0.00090 0.00180 0.00500 S1 4 0.666667 0.333333 0.025362 10.16670 0.01075 0.01075 = 0.00680 0.00000 0.00000 0.00537 O1 3 0.447876 0.223938 0.054817 10.50000 0.00990 0.01948 = 0.01192 0.00031 0.00062 0.00495 O2 3 0.666667 0.333333 -0.060163 10.16670 0.01993 0.01993 = 0.00577 0.00000 0.00000 0.00996 O3 3 0.127506 -0.127506 0.135013 10.50000 0.00976 0.00976 = 0.02652 -0.00350 0.00350 0.00401 AFIX 3 H3 1 0.174816 -0.174781 0.114613 10.50000 0.00992 AFIX 0 O4 3 0.000000 0.000000 0.000000 10.08330 0.04146 0.04146 = 0.02572 0.00000 0.00000 0.02073 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 04src0949_295 R-3m H 0.320 FE 1.240 O 0.660 S 1.030 Fe1 - O3_$6 O3_$5 O3 O3_$2 O1 O1_$2 S1 - O2 O1_$3 O1_$4 O1 O1 - S1 Fe1 O2 - S1 O3 - Fe1_$1 Fe1 O4 - no bonds found Operators for generating equivalent atoms: $1 -x+y, -x, z $2 -x+2/3, -y+1/3, -z+1/3 $3 -y+1, x-y, z $4 -x+y+1, -x+1, z $5 -y, x-y, z $6 y+2/3, -x+y+1/3, -z+1/3 6992 Reflections read, of which 4681 rejected -9 =< h =< 8, -9 =< k =< 9, -21 =< l =< 20, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 1 1 243.33 2.32 3 99.70 1 Inconsistent equivalents 253 Unique reflections, of which 0 suppressed R(int) = 0.0281 R(sigma) = 0.0243 Friedel opposites merged Maximum memory for data reduction = 870 / 3940 Special position constraints for Fe1 x = 0.3333 y = 0.1667 z = 0.1667 U13 = 2.0 * U23 U12 = 0.5 * U11 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for S1 x = 0.6667 y = 0.3333 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.16667 Input constraints retained (at least in part) for sof Special position constraints for O1 y = 0.5 * x + 0.0000 U13 = 2.0 * U23 U12 = 0.5 * U11 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O2 x = 0.6667 y = 0.3333 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.16667 Input constraints retained (at least in part) for sof Special position constraints for O3 y = -1.0 * x + 0.0000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for H3 y = -1.0 * x + 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O4 x = 0.0000 y = 0.0000 z = 0.0000 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.08333 Input constraints retained (at least in part) for sof Least-squares cycle 1 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0611 before cycle 1 for 253 data and 27 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38218 0.00239 -0.140 OSF 2 0.00896 0.00092 -0.025 EXTI Mean shift/esd = 0.149 Maximum = -0.451 for U33 Fe1 Max. shift = 0.001 A for O2 Max. dU = 0.002 for H3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0610 before cycle 2 for 253 data and 27 / 27 parameters GooF = S = 1.122; Restrained GooF = 1.122 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38196 0.00239 -0.095 OSF 2 0.00894 0.00092 -0.018 EXTI Mean shift/esd = 0.052 Maximum = -0.151 for U33 Fe1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for H3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0610 before cycle 3 for 253 data and 27 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38195 0.00239 -0.002 OSF 2 0.00894 0.00092 -0.003 EXTI Mean shift/esd = 0.001 Maximum = 0.004 for U11 O4 Max. shift = 0.000 A for O3 Max. dU = 0.000 for H3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0610 before cycle 4 for 253 data and 27 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38195 0.00239 0.000 OSF 2 0.00894 0.00092 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U11 H3 Max. shift = 0.000 A for O2 Max. dU = 0.000 for H3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0610 before cycle 5 for 253 data and 27 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38195 0.00239 0.000 OSF 2 0.00894 0.00092 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 H3 Max. shift = 0.000 A for O3 Max. dU = 0.000 for H3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 975 / 51021 wR2 = 0.0610 before cycle 6 for 253 data and 27 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38195 0.00239 0.000 OSF 2 0.00894 0.00092 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 H3 Max. shift = 0.000 A for O3 Max. dU = 0.000 for H3 Largest correlation matrix elements 0.774 U12 O3 / U11 O3 0.684 U22 Fe1 / U11 Fe1 0.530 U22 Fe1 / EXTI 0.771 U22 Fe1 / OSF 0.664 U33 Fe1 / OSF 0.521 U11 S1 / U11 Fe1 0.761 EXTI / OSF 0.612 U11 S1 / OSF 0.502 U33 S1 / U33 Fe1 0.695 U11 Fe1 / OSF 0.592 U11 S1 / U22 Fe1 04src0949_295 R-3m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.33333 0.16667 0.16667 0.25000 0.00991 0.01307 0.01295 0.00090 0.00180 0.00496 0.01233 0.00000 0.00000 0.00000 0.00000 0.00000 0.00040 0.00035 0.00042 0.00010 0.00019 0.00020 0.00031 S1 0.66667 0.33333 0.02537 0.16670 0.01066 0.01066 0.00655 0.00000 0.00000 0.00533 0.00929 0.00108 0.00000 0.00000 0.00006 0.00000 0.00043 0.00043 0.00056 0.00000 0.00000 0.00021 0.00034 O1 0.44789 0.22394 0.05482 0.50000 0.00981 0.01922 0.01163 0.00037 0.00074 0.00491 0.01460 0.00410 0.00033 0.00017 0.00011 0.00000 0.00105 0.00082 0.00091 0.00036 0.00073 0.00052 0.00050 O2 0.66667 0.33333 -0.06010 0.16670 0.01999 0.01999 0.00505 0.00000 0.00000 0.01000 0.01501 0.00327 0.00000 0.00000 0.00019 0.00000 0.00118 0.00118 0.00154 0.00000 0.00000 0.00059 0.00077 O3 0.12747 -0.12747 0.13505 0.50000 0.00972 0.00972 0.02603 -0.00348 0.00348 0.00410 0.01550 0.00211 0.00017 0.00017 0.00012 0.00000 0.00075 0.00075 0.00114 0.00045 0.00045 0.00086 0.00049 H3 0.17478 -0.17482 0.11465 0.50000 0.01199 0.00000 0.01019 O4 0.00000 0.00000 0.00000 0.08330 0.04183 0.04183 0.02554 0.00000 0.00000 0.02092 0.03640 0.00000 0.00000 0.00000 0.00000 0.00000 0.00254 0.00254 0.00312 0.00000 0.00000 0.00127 0.00161 Final Structure Factor Calculation for 04src0949_295 R-3m Total number of l.s. parameters = 27 Maximum vector length = 511 Memory required = 948 / 22995 wR2 = 0.0610 before cycle 7 for 253 data and 0 / 27 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0286 * P )^2 + 3.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0224 for 244 Fo > 4sig(Fo) and 0.0236 for all 253 data wR2 = 0.0610, GooF = S = 1.123, Restrained GooF = 1.123 for all data Occupancy sum of asymmetric unit = 1.67 for non-hydrogen and 0.50 for hydrogen atoms Principal mean square atomic displacements U 0.0141 0.0138 0.0091 Fe1 0.0107 0.0107 0.0066 S1 0.0224 0.0119 0.0095 O1 0.0200 0.0200 0.0051 O2 0.0288 0.0092 0.0085 O3 0.0418 0.0418 0.0255 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.048 0.096 0.122 0.162 0.198 0.250 0.339 0.430 1.000 Number in group 26. 25. 25. 27. 25. 25. 24. 26. 25. 25. GooF 1.181 1.355 0.969 0.988 1.304 0.963 0.909 1.011 0.975 1.429 K 1.106 0.985 0.960 1.004 0.984 0.985 0.985 1.014 1.008 1.009 Resolution(A) 0.77 0.79 0.84 0.88 0.92 1.00 1.09 1.19 1.40 1.83 inf Number in group 26. 26. 27. 24. 24. 27. 23. 26. 25. 25. GooF 1.024 0.767 0.711 0.772 0.810 0.786 0.753 1.051 1.457 2.201 K 0.971 0.979 1.000 1.008 1.024 1.033 1.029 1.022 1.021 0.985 R1 0.032 0.031 0.019 0.019 0.019 0.019 0.017 0.018 0.022 0.033 Recommended weighting scheme: WGHT 0.0282 3.4076 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 3 3 1499.08 1931.54 4.21 0.162 1.98 -1 3 2 268.16 159.45 3.81 0.046 2.31 -2 2 2 5562.73 6425.28 3.31 0.295 2.97 -2 2 5 3939.42 4586.25 3.30 0.249 2.32 0 3 6 62.41 123.09 2.96 0.041 1.69 -1 4 1 -4.51 16.23 2.88 0.015 1.75 -6 6 15 7676.01 8905.22 2.75 0.347 0.77 0 2 10 80152.45 72946.94 2.65 0.994 1.50 -2 3 7 1771.90 2047.85 2.57 0.167 1.71 0 5 4 59.83 23.97 2.52 0.018 1.22 0 0 9 50534.14 45852.80 2.46 0.788 1.88 0 2 4 19772.04 21690.96 2.44 0.542 2.54 -2 3 1 248.94 333.62 2.36 0.067 2.38 -1 2 6 1163.81 1007.26 2.15 0.117 2.24 0 3 0 1751.44 1537.36 2.15 0.144 2.12 0 2 1 56844.41 61200.27 1.93 0.910 3.12 -1 2 12 2239.80 2024.02 1.91 0.166 1.32 -3 6 9 25.82 9.75 1.85 0.011 1.03 -4 5 18 976.30 1127.86 1.81 0.124 0.78 -2 4 0 69057.88 73867.39 1.81 1.000 1.83 -2 7 6 793.04 916.02 1.80 0.111 0.96 0 1 20 73.09 125.13 1.78 0.041 0.84 -7 7 1 108.43 68.81 1.73 0.031 0.91 -1 1 7 41429.50 39006.87 1.70 0.727 2.26 0 2 16 17878.57 16666.83 1.67 0.475 1.01 -1 2 21 48.32 90.11 1.58 0.035 0.79 -2 7 12 754.48 855.57 1.49 0.108 0.83 0 6 6 10878.19 10085.37 1.48 0.370 0.99 -1 5 0 779.84 694.53 1.46 0.097 1.39 -1 5 9 318.39 267.38 1.46 0.060 1.12 -1 5 6 15.03 4.97 1.44 0.008 1.24 -5 7 12 264.42 317.49 1.40 0.066 0.83 -1 2 9 1327.35 1446.87 1.39 0.140 1.68 -2 4 3 11257.58 11850.63 1.35 0.401 1.74 0 7 11 409.19 476.96 1.33 0.080 0.78 -2 6 1 13464.93 12816.22 1.30 0.417 1.20 -2 4 15 7439.15 7038.51 1.23 0.309 0.96 -1 4 7 4823.94 5089.89 1.22 0.262 1.42 -2 6 10 15741.59 14964.62 1.20 0.450 0.98 0 4 11 18646.93 17773.78 1.19 0.491 1.11 -3 7 11 191.31 228.12 1.17 0.056 0.86 -1 1 1 1725.49 2609.26 1.16 0.188 5.95 0 7 8 259.79 311.06 1.12 0.065 0.83 -1 1 19 890.57 752.79 1.05 0.101 0.88 0 2 13 2476.94 2343.24 1.04 0.178 1.21 -2 7 3 7074.64 6758.25 1.02 0.302 1.00 -2 7 9 1036.49 960.52 1.02 0.114 0.90 -4 4 4 21219.15 22050.06 1.01 0.546 1.49 -4 4 1 17776.01 18507.83 1.00 0.501 1.58 -1 5 18 1454.53 1566.88 1.00 0.146 0.78 Bond lengths and angles Fe1 - Distance Angles O3_$6 1.9912 (0.0009) O3_$5 1.9912 (0.0009) 180.00 O3 1.9912 (0.0009) 90.44 (0.13) 89.56 (0.13) O3_$2 1.9912 (0.0009) 89.56 (0.13) 90.44 (0.13) 180.00 O1 2.0314 (0.0019) 90.93 (0.07) 89.08 (0.07) 89.08 (0.07) 90.93 (0.07) O1_$2 2.0314 (0.0019) 89.07 (0.07) 90.92 (0.07) 90.92 (0.07) 89.07 (0.07) 180.00 Fe1 - O3_$6 O3_$5 O3 O3_$2 O1 S1 - Distance Angles O2 1.4493 (0.0035) O1_$3 1.4768 (0.0021) 109.76 (0.08) O1_$4 1.4768 (0.0021) 109.76 (0.08) 109.18 (0.08) O1 1.4768 (0.0021) 109.76 (0.08) 109.18 (0.08) 109.18 (0.08) S1 - O2 O1_$3 O1_$4 O1 - Distance Angles S1 1.4768 (0.0021) Fe1 2.0314 (0.0019) 130.76 (0.13) O1 - S1 O2 - Distance Angles S1 1.4493 (0.0035) O2 - O3 - Distance Angles Fe1_$1 1.9912 (0.0009) Fe1 1.9912 (0.0009) 134.14 (0.11) O3 - Fe1_$1 FMAP and GRID set by program FMAP 2 3 19 GRID -1.042 -2 -2 1.042 2 2 R1 = 0.0230 for 253 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.42 at 0.3333 0.6667 0.1667 [ 1.81 A from O2 ] Deepest hole -0.53 at 0.8455 0.6909 0.1184 [ 0.83 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 1066 / 13046 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6667 0.3333 -0.1667 0.08333 0.05 0.42 1.81 O2 2.20 H3 2.67 O3 3.26 S1 Q2 1 0.5492 0.2746 0.0438 0.50000 0.05 0.41 0.67 O1 0.81 S1 1.89 O1 1.91 O2 Q3 1 0.4956 0.3126 0.0620 1.00000 0.05 0.31 0.58 O1 1.34 S1 1.93 O1 2.11 FE1 Q4 1 0.6232 0.2465 -0.0543 0.50000 0.05 0.28 0.56 O2 1.46 S1 2.07 H3 2.21 O1 Q5 1 0.1617 -0.1617 0.0256 0.50000 0.05 0.27 1.52 H3 1.58 O1 1.91 O3 2.10 O4 Q6 1 0.0238 -0.2102 0.1570 1.00000 0.05 0.25 0.79 O3 1.23 H3 1.24 FE1 2.25 O3 Q7 1 -0.1585 0.0000 0.0000 0.50000 0.05 0.22 1.16 O4 2.14 O1 2.36 H3 2.44 O3 Q8 1 0.2318 -0.2318 0.1653 0.50000 0.05 0.20 1.12 H3 1.42 O3 1.99 H3 2.20 O2 Q9 1 0.3395 -0.0086 0.1370 1.00000 0.05 0.19 1.27 H3 1.35 O3 1.40 FE1 1.64 O3 Q10 1 0.5675 0.1350 -0.0871 0.50000 0.05 0.19 1.34 O2 1.82 H3 2.29 S1 2.32 O3 Shortest distances between peaks (including symmetry equivalents) 2 3 0.66 4 10 0.90 3 3 0.95 4 4 0.96 6 9 0.96 9 9 1.01 6 9 1.06 7 7 1.16 5 7 1.27 1 8 1.29 8 8 1.29 2 2 1.29 6 6 1.37 8 10 1.37 3 3 1.41 8 9 1.48 8 9 1.50 2 3 1.50 6 6 1.60 6 8 1.62 9 10 1.63 4 10 1.70 2 4 1.79 3 9 1.82 8 10 1.84 1 10 1.85 2 5 1.85 2 3 1.87 6 6 1.89 3 5 1.90 1 4 1.98 3 6 2.01 7 7 2.01 4 5 2.02 3 3 2.05 6 9 2.06 6 9 2.06 4 8 2.07 2 4 2.11 3 4 2.13 6 8 2.16 5 10 2.16 3 10 2.18 10 10 2.18 4 8 2.19 5 5 2.23 6 10 2.23 8 8 2.24 5 9 2.25 9 9 2.29 7 7 2.33 3 4 2.34 9 10 2.34 3 3 2.36 4 9 2.36 3 7 2.39 5 6 2.40 5 7 2.40 3 9 2.40 1 9 2.41 3 6 2.42 6 9 2.42 9 9 2.43 3 6 2.44 2 9 2.45 6 10 2.46 6 9 2.47 3 6 2.47 2 10 2.48 6 6 2.48 2 6 2.51 4 8 2.53 5 8 2.53 3 9 2.55 3 5 2.56 9 9 2.56 8 8 2.58 8 10 2.60 3 4 2.61 3 7 2.61 9 9 2.62 4 8 2.63 3 10 2.64 3 9 2.65 2 7 2.65 7 9 2.69 6 7 2.71 8 9 2.71 8 9 2.76 3 8 2.77 6 8 2.78 4 5 2.78 2 10 2.78 9 9 2.80 4 9 2.81 3 6 2.81 3 4 2.82 9 10 2.82 6 6 2.83 1 6 2.84 2 6 2.84 6 6 2.85 8 10 2.87 2 5 2.88 10 10 2.98 6 7 2.99 3 5 2.99 2 9 2.99 2 10 2.99 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. 0.42: 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 0.00: Generate idealized H-atoms 0.05: Structure factors and derivatives 0.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0949_295 finished at 10:59:25 Total CPU time: 0.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++