+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0951_295 started at 17:27:51 on 15-Dec-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0951_295 in R-3m CELL 0.71073 7.3003 7.3003 17.2160 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 K O S UNIT 18 9 3 42 6 V = 794.59 F(000) = 741.0 Mu = 4.92 mm-1 Cell Wt = 1502.45 Rho = 3.140 MERG 2 OMIT -3.00 55.00 OMIT -2 2 5 EXTI 0.00202 FMAP 2 PLAN 10 SIZE 0.05 0.05 0.05 ACTA WGHT 0.02450 3.99690 L.S. 6 TEMP 22.00 FVAR 0.33421 FE1 2 0.333333 0.166667 0.166667 10.25000 0.00541 0.00712 = 0.00984 -0.00002 -0.00003 0.00271 S1 5 0.666667 0.333333 0.025160 10.16670 0.00704 0.00704 = 0.00609 0.00000 0.00000 0.00352 O1 4 0.127191 -0.127191 0.135591 10.50000 0.00824 0.00824 = 0.01384 -0.00224 0.00224 0.00455 AFIX 3 H1 1 0.173791 -0.174135 0.120381 10.50000 0.00001 AFIX 0 O2 4 0.446078 0.223039 0.054363 10.50000 0.00734 0.01426 = 0.01019 0.00111 0.00221 0.00367 O3 4 0.666667 0.333333 -0.059570 10.16670 0.01589 0.01589 = 0.00349 0.00000 0.00000 0.00794 K1 3 0.000000 0.000000 0.000000 10.08330 0.02161 0.02161 = 0.00998 0.00000 0.00000 0.01080 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 04src0951_295 in R-3m H 0.320 FE 1.240 K 2.270 O 0.660 S 1.030 Fe1 - O1_$9 O1_$2 O1 O1_$7 O2 O2_$7 K1 K1_$13 S1 - O3 O2_$11 O2_$12 O2 O1 - Fe1_$4 Fe1 K1 O2 - S1 Fe1 K1 O3 - S1 K1 - O1_$2 O1_$8 O1_$4 O1 O1_$6 O1_$10 O2 O2_$6 O2_$10 O2_$2 O2_$4 O2_$8 Operators for generating equivalent atoms: $1 x-2/3, y-1/3, z-1/3 $2 -y, x-y, z $3 -y+1/3, x-y-1/3, z-1/3 $4 -x+y, -x, z $5 -x+y+1/3, -x+2/3, z-1/3 $6 -x, -y, -z $7 -x+2/3, -y+1/3, -z+1/3 $8 y, -x+y, -z $9 y+2/3, -x+y+1/3, -z+1/3 $10 x-y, x, -z $11 -y+1, x-y, z $12 -x+y+1, -x+1, z $13 x+2/3, y+1/3, z+1/3 h k l Fo^2 Sigma Why rejected 2 -4 8 17.30 4.28 observed but should be systematically absent 6618 Reflections read, of which 4428 rejected -9 =< h =< 9, -9 =< k =< 8, -22 =< l =< 19, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 252 Unique reflections, of which 0 suppressed R(int) = 0.0320 R(sigma) = 0.0327 Friedel opposites merged Maximum memory for data reduction = 1401 / 4013 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 = -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 H1 y = -1.0 * x + 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O2 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 O3 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 K1 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 = 1503 / 52043 wR2 = 0.0615 before cycle 1 for 252 data and 27 / 27 parameters GooF = S = 1.099; Restrained GooF = 1.099 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33472 0.00201 0.254 OSF 2 0.00206 0.00057 0.066 EXTI Mean shift/esd = 0.245 Maximum = -0.937 for x O1 Max. shift = 0.002 A for O2 Max. dU = 0.004 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.0609 before cycle 2 for 252 data and 27 / 27 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33462 0.00199 -0.050 OSF 2 0.00207 0.00057 0.023 EXTI Mean shift/esd = 0.081 Maximum = -0.307 for x O1 Max. shift = 0.001 A for O2 Max. dU = 0.002 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.0609 before cycle 3 for 252 data and 27 / 27 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33462 0.00199 0.001 OSF 2 0.00207 0.00057 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.012 for U11 H1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.0609 before cycle 4 for 252 data and 27 / 27 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33462 0.00199 0.000 OSF 2 0.00207 0.00057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for U11 O2 Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.0609 before cycle 5 for 252 data and 27 / 27 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33463 0.00199 0.000 OSF 2 0.00207 0.00057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O2 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.0609 before cycle 6 for 252 data and 27 / 27 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33462 0.00199 0.000 OSF 2 0.00207 0.00057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O2 Max. dU = 0.000 for H1 Largest correlation matrix elements 0.775 U12 O1 / U11 O1 0.691 U11 Fe1 / OSF 0.576 U11 S1 / OSF 0.763 U22 Fe1 / OSF 0.681 U22 Fe1 / U11 Fe1 0.546 U11 S1 / U22 Fe1 0.719 EXTI / OSF 0.641 U33 Fe1 / OSF 04src0951_295 in R-3m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.33333 0.16667 0.16667 0.25000 0.00531 0.00704 0.00975 0.00000 -0.00001 0.00266 0.00756 0.00000 0.00000 0.00000 0.00000 0.00000 0.00040 0.00036 0.00045 0.00011 0.00022 0.00020 0.00031 S1 0.66667 0.33333 0.02515 0.16670 0.00697 0.00697 0.00594 0.00000 0.00000 0.00348 0.00663 0.00123 0.00000 0.00000 0.00007 0.00000 0.00046 0.00046 0.00065 0.00000 0.00000 0.00023 0.00036 O1 0.12695 -0.12695 0.13560 0.50000 0.00813 0.00813 0.01430 -0.00206 0.00206 0.00444 0.01002 0.00218 0.00019 0.00019 0.00013 0.00000 0.00080 0.00080 0.00116 0.00045 0.00045 0.00093 0.00051 H1 0.17355 -0.17379 0.12039 0.50000 0.00603 0.00000 0.01121 O2 0.44640 0.22320 0.05429 0.50000 0.00658 0.01407 0.01054 0.00111 0.00222 0.00329 0.01123 0.00427 0.00034 0.00017 0.00012 0.00000 0.00114 0.00086 0.00105 0.00040 0.00080 0.00057 0.00054 O3 0.66667 0.33333 -0.05948 0.16670 0.01556 0.01556 0.00419 0.00000 0.00000 0.00778 0.01177 0.00361 0.00000 0.00000 0.00021 0.00000 0.00123 0.00123 0.00175 0.00000 0.00000 0.00061 0.00083 K1 0.00000 0.00000 0.00000 0.08330 0.02158 0.02158 0.01016 0.00000 0.00000 0.01079 0.01777 0.00000 0.00000 0.00000 0.00000 0.00000 0.00063 0.00063 0.00084 0.00000 0.00000 0.00031 0.00045 Final Structure Factor Calculation for 04src0951_295 in R-3m Total number of l.s. parameters = 27 Maximum vector length = 511 Memory required = 1476 / 24017 wR2 = 0.0609 before cycle 7 for 252 data and 0 / 27 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0245 * P )^2 + 4.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0230 for 237 Fo > 4sig(Fo) and 0.0241 for all 252 data wR2 = 0.0609, GooF = S = 1.090, Restrained GooF = 1.090 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 0.0097 0.0076 0.0053 Fe1 0.0070 0.0070 0.0059 S1 0.0162 0.0084 0.0055 O1 0.0166 0.0115 0.0056 O2 0.0156 0.0156 0.0042 O3 0.0216 0.0216 0.0102 K1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.029 0.062 0.085 0.120 0.162 0.204 0.255 0.329 0.420 1.000 Number in group 26. 25. 25. 27. 23. 28. 23. 26. 24. 25. GooF 1.136 0.815 1.464 1.276 0.901 0.838 1.122 0.743 1.316 1.072 K 1.214 0.988 0.923 0.990 0.993 0.969 0.995 1.005 1.010 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.99 1.07 1.19 1.38 1.74 inf Number in group 26. 25. 25. 26. 24. 26. 26. 24. 25. 25. GooF 1.196 0.763 0.914 0.818 0.764 0.796 0.845 0.941 1.400 1.900 K 0.933 0.994 1.025 1.006 1.025 1.031 1.030 1.019 1.011 0.986 R1 0.051 0.036 0.026 0.019 0.020 0.024 0.017 0.017 0.017 0.027 Recommended weighting scheme: WGHT 0.0170 3.2587 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) -1 3 2 1634.60 1291.94 3.82 0.119 2.30 -5 6 16 213.58 460.77 3.32 0.071 0.78 0 1 2 13296.75 15678.82 3.30 0.416 5.10 -2 2 2 10253.56 11636.15 3.23 0.358 2.97 -2 3 10 61.91 11.14 3.21 0.011 1.40 0 2 4 26226.92 29000.37 2.78 0.566 2.55 0 3 6 75.13 30.52 2.60 0.018 1.70 -1 4 1 455.94 586.01 2.55 0.080 1.74 0 1 8 342.54 457.33 2.43 0.071 2.04 -1 1 10 841.61 685.80 2.39 0.087 1.66 -2 3 7 3932.86 4359.65 2.31 0.219 1.71 -4 8 12 4492.07 5366.57 2.28 0.243 0.77 0 0 15 2240.64 1852.83 2.12 0.143 1.15 0 7 5 486.95 625.87 2.09 0.083 0.87 -3 3 3 4142.96 4551.34 2.09 0.224 1.98 0 5 4 33.06 68.74 2.02 0.028 1.21 -7 7 1 546.68 429.07 1.98 0.069 0.90 -1 5 0 2136.83 1933.21 1.83 0.146 1.38 -2 4 3 7777.54 8316.81 1.79 0.303 1.74 -4 6 17 2162.19 2807.39 1.74 0.176 0.77 0 4 11 17138.35 15987.35 1.69 0.420 1.11 0 3 3 69758.02 66241.88 1.66 0.855 1.98 -4 7 10 397.05 489.05 1.66 0.073 0.89 -2 5 17 839.12 998.19 1.63 0.105 0.83 -3 6 9 297.51 237.31 1.63 0.051 1.03 0 6 0 20900.93 19473.20 1.59 0.463 1.05 -2 5 8 457.60 385.95 1.56 0.065 1.20 -1 1 4 1359.65 1499.29 1.49 0.129 3.56 -1 5 18 775.26 901.69 1.40 0.100 0.79 -1 2 12 849.44 760.76 1.37 0.092 1.34 -1 3 17 5643.65 5239.25 1.36 0.240 0.93 -1 4 4 6095.74 5782.17 1.36 0.253 1.62 -1 5 6 256.19 211.48 1.36 0.048 1.24 -2 7 3 11194.35 10593.85 1.35 0.342 1.00 -5 7 9 263.25 317.70 1.32 0.059 0.89 -3 4 5 9159.62 8741.07 1.30 0.310 1.56 -3 8 7 1163.11 1295.78 1.28 0.120 0.85 -2 6 10 22309.39 21223.15 1.28 0.484 0.98 -3 6 0 14678.73 13984.15 1.28 0.393 1.22 -3 7 11 609.47 695.61 1.28 0.088 0.87 -1 5 9 1060.38 968.85 1.23 0.103 1.12 -6 6 12 4009.87 3604.99 1.22 0.199 0.85 -4 5 18 619.32 729.89 1.22 0.090 0.79 -2 3 1 1690.30 1812.53 1.21 0.141 2.37 -1 7 10 60.24 95.36 1.21 0.032 0.84 -2 7 12 530.85 607.95 1.18 0.082 0.83 -4 6 14 8521.45 7870.27 1.17 0.295 0.86 -2 3 16 296.70 349.87 1.17 0.062 0.98 0 6 6 15716.69 14870.00 1.16 0.405 0.99 -6 7 8 3203.93 3460.29 1.14 0.195 0.88 Bond lengths and angles Fe1 - Distance Angles O1_$9 1.9802 (0.0009) O1_$2 1.9802 (0.0009) 180.00 O1 1.9802 (0.0009) 90.82 (0.14) 89.18 (0.14) O1_$7 1.9802 (0.0009) 89.18 (0.14) 90.82 (0.14) 180.00 O2 2.0625 (0.0021) 91.43 (0.07) 88.57 (0.07) 88.57 (0.07) 91.43 (0.07) O2_$7 2.0625 (0.0021) 88.57 (0.07) 91.43 (0.07) 91.43 (0.07) 88.57 (0.07) 180.00 K1 3.5601 (0.0004) 127.43 (0.07) 52.57 (0.07) 52.57 (0.07) 127.43 (0.07) 56.57 (0.06) 123.43 (0.06) K1_$13 3.5601 (0.0004) 52.57 (0.07) 127.43 (0.07) 127.43 (0.07) 52.57 (0.07) 123.43 (0.06) 56.57 (0.06) 180.00 Fe1 - O1_$9 O1_$2 O1 O1_$7 O2 O2_$7 K1 S1 - Distance Angles O3 1.4569 (0.0039) O2_$11 1.4802 (0.0022) 109.81 (0.09) O2_$12 1.4802 (0.0022) 109.81 (0.09) 109.13 (0.09) O2 1.4802 (0.0022) 109.81 (0.09) 109.13 (0.09) 109.13 (0.09) S1 - O3 O2_$11 O2_$12 O1 - Distance Angles Fe1_$4 1.9802 (0.0009) Fe1 1.9802 (0.0009) 134.34 (0.12) K1 2.8331 (0.0023) 93.71 (0.07) 93.71 (0.07) O1 - Fe1_$4 Fe1 O2 - Distance Angles S1 1.4802 (0.0022) Fe1 2.0625 (0.0021) 130.09 (0.13) K1 2.9730 (0.0022) 141.86 (0.12) 88.05 (0.07) O2 - S1 Fe1 O3 - Distance Angles S1 1.4569 (0.0039) O3 - K1 - Distance Angles O1_$2 2.8331 (0.0023) O1_$8 2.8331 (0.0023) 180.00 (0.11) O1_$4 2.8331 (0.0023) 58.77 (0.08) 121.23 (0.08) O1 2.8331 (0.0023) 58.77 (0.08) 121.23 (0.08) 58.77 (0.08) O1_$6 2.8331 (0.0023) 121.23 (0.08) 58.77 (0.08) 121.23 (0.08) 180.00 (0.07) O1_$10 2.8331 (0.0023) 121.23 (0.08) 58.77 (0.08) 180.00 (0.17) 121.23 (0.08) 58.77 (0.08) O2 2.9730 (0.0022) 58.13 (0.03) 121.87 (0.03) 106.19 (0.06) 58.13 (0.03) 121.87 (0.03) 73.81 (0.06) O2_$6 2.9730 (0.0022) 121.87 (0.03) 58.13 (0.03) 73.81 (0.06) 121.87 (0.03) 58.13 (0.03) 106.19 (0.06) 180.00 (0.09) O2_$10 2.9730 (0.0022) 73.81 (0.06) 106.19 (0.06) 121.87 (0.03) 121.87 (0.03) 58.13 (0.03) 58.13 (0.03) 69.41 (0.04) O2_$2 2.9730 (0.0022) 58.13 (0.03) 121.87 (0.03) 58.13 (0.03) 106.19 (0.06) 73.81 (0.06) 121.87 (0.03) 110.59 (0.04) O2_$4 2.9730 (0.0022) 106.19 (0.06) 73.81 (0.06) 58.13 (0.03) 58.13 (0.03) 121.87 (0.03) 121.87 (0.03) 110.59 (0.04) O2_$8 2.9730 (0.0022) 121.87 (0.03) 58.13 (0.03) 121.87 (0.03) 73.81 (0.06) 106.19 (0.06) 58.13 (0.03) 69.41 (0.04) K1 - O1_$2 O1_$8 O1_$4 O1 O1_$6 O1_$10 O2 FMAP and GRID set by program FMAP 2 3 20 GRID -0.980 -2 -2 0.980 2 2 R1 = 0.0238 for 252 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.6714 0.8357 0.0328 [ 1.51 A from H1 ] Deepest hole -0.52 at 0.6667 0.3333 0.1440 [ 1.85 A from O1 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 1594 / 13288 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1643 -0.1643 0.0328 0.50000 0.05 0.50 1.51 H1 1.67 O2 1.83 O1 2.15 K1 Q2 1 0.6667 0.3333 -0.1667 0.08333 0.05 0.45 1.85 O3 2.17 H1 2.66 O1 3.30 S1 Q3 1 0.7186 0.4372 0.0334 0.50000 0.05 0.44 0.67 S1 0.82 O2 1.73 O3 1.85 O2 Q4 1 0.6667 0.3333 -0.0186 0.16667 0.05 0.40 0.70 O3 0.75 S1 1.87 O2 2.67 H1 Q5 1 0.1680 -0.1680 0.2067 0.50000 0.05 0.39 1.33 O1 1.49 H1 2.06 H1 2.06 H1 Q6 1 0.6667 0.3333 0.1072 0.16667 0.05 0.38 1.41 S1 1.66 O2 2.24 O1 2.34 FE1 Q7 1 0.0000 0.0000 0.1524 0.16667 0.05 0.34 1.63 O1 2.12 FE1 2.26 H1 2.59 O2 Q8 1 0.4348 0.3136 0.1167 1.00000 0.05 0.32 1.28 FE1 1.29 O2 1.69 O1 2.04 H1 Q9 1 0.1249 -0.1249 0.0961 0.50000 0.05 0.30 0.68 O1 0.75 H1 2.25 FE1 2.29 K1 Q10 1 0.5902 0.1805 -0.1237 0.50000 0.05 0.29 1.47 O3 1.75 H1 1.75 H1 1.86 H1 Shortest distances between peaks (including symmetry equivalents) 3 4 1.11 5 10 1.13 3 3 1.14 1 9 1.20 2 10 1.22 5 8 1.22 6 7 1.27 8 8 1.40 3 6 1.43 6 8 1.63 10 10 1.67 10 10 1.77 3 8 1.79 8 8 1.84 7 9 1.85 1 3 1.87 7 8 1.97 5 9 1.98 4 10 2.05 8 9 2.10 8 10 2.12 8 8 2.15 5 6 2.15 1 4 2.15 4 6 2.17 2 5 2.20 8 9 2.28 3 8 2.30 5 10 2.31 5 7 2.32 9 10 2.36 1 1 2.36 1 10 2.43 10 10 2.43 5 9 2.47 3 5 2.47 1 8 2.49 5 5 2.50 2 4 2.55 5 8 2.56 8 8 2.57 9 10 2.57 5 8 2.58 3 7 2.62 3 8 2.62 1 5 2.66 5 10 2.71 9 9 2.73 6 9 2.74 1 8 2.75 1 3 2.78 4 5 2.80 8 8 2.82 3 10 2.84 4 8 2.84 8 9 2.87 8 10 2.88 2 9 2.90 7 8 2.90 1 9 2.91 1 7 2.92 4 9 2.95 3 9 2.98 1 5 2.99 Time profile in seconds ----------------------- 0.09: 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. 0.47: 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 0.03: Structure factors and derivatives 0.02: 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 0.02: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0951_295 finished at 17:27:51 Total CPU time: 0.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++