+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 12:20:00 on 02-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0160 in P2(1)/c CELL 0.71073 4.9767 11.5866 7.0206 90.000 90.589 90.000 ZERR 2.00 0.0002 0.0005 0.0003 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CL RH UNIT 8 12 4 4 2 V = 404.81 F(000) = 246.0 Mu = 2.69 mm-1 Cell Wt = 511.84 Rho = 2.100 MERG 2 FMAP 2 PLAN 10 OMIT -3 55 EXTI TEMP -153 SIZE 0.4 0.12 0.1 ACTA BOND WGHT 0.03500 0.94480 L.S. 10 FVAR 1.21088 C1 1 0.422781 -0.110088 0.272925 11.00000 0.01797 0.01397 = 0.01631 -0.00125 -0.00208 -0.00021 RH1 5 0.000000 0.000000 0.000000 10.50000 0.01102 0.00923 = 0.01360 0.00209 -0.00246 -0.00068 CL1 4 -0.125859 0.122731 0.238521 11.00000 0.02170 0.01905 = 0.02157 -0.00265 -0.00196 0.00218 N1 3 0.268873 -0.070059 0.172033 11.00000 0.01831 0.01577 = 0.02186 -0.00014 -0.00134 -0.00146 C2 1 0.620029 -0.160877 0.401183 11.00000 0.01864 0.02618 = 0.02225 0.00514 -0.00108 0.00452 AFIX 33 H2A 2 0.720159 -0.218814 0.334698 11.00000 -1.50000 H2B 2 0.530200 -0.195467 0.507228 11.00000 -1.50000 H2C 2 0.740318 -0.101976 0.446538 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04src0160 in P2(1)/c C 0.770 H 0.320 N 0.700 CL 0.990 RH 1.350 C1 - N1 C2 Rh1 - N1 N1_$1 Cl1 Cl1_$1 Cl1 - Rh1 N1 - C1 Rh1 C2 - C1 Operators for generating equivalent atoms: $1 -x, -y, -z h k l Fo^2 Sigma Why rejected 3 0 3 5.53 1.38 observed but should be systematically absent 2 0 5 5.85 1.46 observed but should be systematically absent 2 0 3 27.76 1.48 observed but should be systematically absent 2 0 3 11.28 2.82 observed but should be systematically absent 2 0 1 26.79 1.50 observed but should be systematically absent 2 0 1 5.97 1.49 observed but should be systematically absent -2 0 1 12.89 1.44 observed but should be systematically absent -2 0 1 7.59 1.52 observed but should be systematically absent -2 0 3 10.62 1.52 observed but should be systematically absent -2 0 3 14.50 2.90 observed but should be systematically absent 1 0 3 18.55 1.43 observed but should be systematically absent 1 0 1 7.44 1.49 observed but should be systematically absent 0 11 0 12.32 2.74 observed but should be systematically absent 0 0 5 12.57 2.79 observed but should be systematically absent 0 0 3 12.69 1.41 observed but should be systematically absent -1 0 3 8.21 1.37 observed but should be systematically absent 1 0 3 26.79 2.82 observed but should be systematically absent 1 0 5 14.03 2.81 observed but should be systematically absent -2 0 3 14.37 2.88 observed but should be systematically absent -2 0 3 19.92 2.66 observed but should be systematically absent -2 0 1 10.97 1.37 observed but should be systematically absent 2 0 1 13.44 1.49 observed but should be systematically absent 2 0 1 9.40 1.34 observed but should be systematically absent 2 0 3 31.36 1.43 observed but should be systematically absent 2 0 3 14.93 2.99 observed but should be systematically absent 2 0 3 16.60 2.77 observed but should be systematically absent 2 0 5 11.56 2.89 observed but should be systematically absent 2 0 7 12.55 2.79 observed but should be systematically absent 3 0 1 9.01 1.50 observed but should be systematically absent 5164 Reflections read, of which 155 rejected -6 =< h =< 6, -15 =< k =< 14, -8 =< l =< 9, Max. 2-theta = 54.97 29 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -5 1 1 3223.17 31.68 9 178.97 -2 1 1 914.42 13.59 6 91.14 1 1 1 544.47 5.68 2 5542.22 2 1 1 9352.21 165.56 3 1544.93 2 5 1 981.18 12.50 7 97.78 0 8 1 20.80 0.76 8 7.18 0 0 2 30.95 0.91 4 8.56 2 0 2 8487.74 115.25 5 625.05 3 1 2 554.21 6.32 7 42.01 4 2 3 1173.65 12.99 7 93.96 -2 4 3 22.02 0.74 7 6.65 4 1 4 79.22 1.11 7 6.86 12 Inconsistent equivalents 919 Unique reflections, of which 0 suppressed R(int) = 0.0449 R(sigma) = 0.0283 Friedel opposites merged Maximum memory for data reduction = 705 / 9140 Special position constraints for Rh1 x = 0.0000 y = 0.0000 z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 827 / 70063 wR2 = 0.0785 before cycle 1 for 919 data and 44 / 44 parameters GooF = S = 1.258; Restrained GooF = 1.258 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.24504 0.00502 6.801 OSF 2 0.02946 0.00288 10.246 EXTI 12 0.01206 0.00025 4.228 U11 Rh1 13 0.01023 0.00024 4.123 U22 Rh1 14 0.01468 0.00025 4.283 U33 Rh1 Mean shift/su = 1.076 Maximum = 10.246 for EXTI Max. shift = 0.001 A for C1 Max. dU = 0.001 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0702 before cycle 2 for 919 data and 44 / 44 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.26711 0.00498 4.435 OSF 2 0.05480 0.00369 6.864 EXTI Mean shift/su = 0.682 Maximum = 6.864 for EXTI Max. shift = 0.001 A for C1 Max. dU = 0.001 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0677 before cycle 3 for 919 data and 44 / 44 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27025 0.00512 0.614 OSF 2 0.05970 0.00441 1.109 EXTI Mean shift/su = 0.096 Maximum = 1.109 for EXTI Max. shift = 0.000 A for N1 Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 4 for 919 data and 44 / 44 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27049 0.00516 0.047 OSF 2 0.06000 0.00456 0.065 EXTI Mean shift/su = 0.009 Maximum = 0.065 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 5 for 919 data and 44 / 44 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27051 0.00516 0.004 OSF 2 0.06001 0.00457 0.004 EXTI Mean shift/su = 0.001 Maximum = 0.004 for EXTI Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 6 for 919 data and 44 / 44 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27051 0.00516 0.000 OSF 2 0.06001 0.00458 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N1 Max. dU = 0.000 for C1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 7 for 919 data and 44 / 44 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27050 0.00516 -0.001 OSF 2 0.06001 0.00457 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 8 for 919 data and 44 / 44 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27050 0.00516 0.000 OSF 2 0.06001 0.00458 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N1 Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 9 for 919 data and 44 / 44 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27051 0.00516 0.000 OSF 2 0.06001 0.00458 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for U11 Rh1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for Rh1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 827 / 70063 wR2 = 0.0676 before cycle 10 for 919 data and 44 / 44 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.27051 0.00516 0.000 OSF 2 0.06001 0.00457 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for U22 Rh1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for Rh1 Largest correlation matrix elements 0.784 EXTI / OSF 0.720 U22 Rh1 / OSF 0.502 U33 Rh1 / EXTI 0.725 U33 Rh1 / OSF 0.719 U11 Rh1 / OSF 0.500 U11 Rh1 / EXTI Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.7224 -0.2201 0.3332 33 0.980 0.000 C2 C1 H2A H2B 0.5283 -0.1962 0.5092 33 0.980 0.000 C2 C1 H2A H2C 0.7430 -0.1008 0.4474 33 0.980 0.000 C2 C1 H2A 04src0160 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.42308 -0.11007 0.27274 1.00000 0.01978 0.01581 0.01833 -0.00123 -0.00149 -0.00063 0.01799 0.00483 0.00059 0.00024 0.00041 0.00000 0.00130 0.00124 0.00127 0.00099 0.00108 0.00104 0.00056 Rh1 0.00000 0.00000 0.00000 0.50000 0.01272 0.01088 0.01536 0.00209 -0.00250 -0.00067 0.01300 0.00000 0.00000 0.00000 0.00000 0.00000 0.00022 0.00022 0.00023 0.00009 0.00013 0.00009 0.00018 Cl1 -0.12580 0.12274 0.23851 1.00000 0.02349 0.02082 0.02344 -0.00264 -0.00202 0.00221 0.02260 0.00123 0.00015 0.00006 0.00010 0.00000 0.00037 0.00036 0.00037 0.00026 0.00027 0.00027 0.00022 N1 0.26890 -0.07007 0.17192 1.00000 0.01990 0.01754 0.02344 0.00015 -0.00161 -0.00152 0.02031 0.00429 0.00051 0.00021 0.00037 0.00000 0.00116 0.00113 0.00122 0.00095 0.00101 0.00097 0.00051 C2 0.62016 -0.16092 0.40104 1.00000 0.02042 0.02793 0.02413 0.00497 -0.00128 0.00441 0.02417 0.00574 0.00063 0.00028 0.00045 0.00000 0.00138 0.00148 0.00146 0.00119 0.00118 0.00121 0.00062 H2A 0.72238 -0.22007 0.33316 1.00000 0.03626 0.00000 0.00000 H2B 0.52834 -0.19625 0.50923 1.00000 0.03626 0.00000 0.00000 H2C 0.74298 -0.10083 0.44743 1.00000 0.03626 0.00000 0.00000 Final Structure Factor Calculation for 04src0160 in P2(1)/c Total number of l.s. parameters = 44 Maximum vector length = 511 Memory required = 783 / 24017 wR2 = 0.0676 before cycle 11 for 919 data and 0 / 44 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0350 * P )^2 + 0.94 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0240 for 901 Fo > 4sig(Fo) and 0.0277 for all 919 data wR2 = 0.0676, GooF = S = 1.067, Restrained GooF = 1.067 for all data Occupancy sum of asymmetric unit = 4.50 for non-hydrogen and 3.00 for hydrogen atoms Principal mean square atomic displacements U 0.0209 0.0181 0.0150 C1 0.0177 0.0113 0.0100 Rh1 0.0275 0.0213 0.0190 Cl1 0.0243 0.0199 0.0167 N1 0.0321 0.0239 0.0166 C2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.031 0.063 0.094 0.126 0.177 0.228 0.279 0.334 0.431 1.000 Number in group 92. 92. 92. 92. 94. 90. 93. 91. 91. 92. GooF 1.656 0.959 0.756 0.870 1.231 1.226 0.812 0.978 0.853 1.019 K 1.697 1.079 1.013 1.012 0.994 1.004 0.991 1.011 1.002 0.979 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.32 1.64 inf Number in group 97. 89. 92. 92. 91. 90. 92. 94. 91. 91. GooF 0.836 0.806 0.852 0.798 0.693 0.848 0.914 1.046 1.531 1.800 K 0.982 0.996 1.014 1.006 1.010 1.005 1.019 1.003 1.001 0.961 R1 0.034 0.027 0.025 0.021 0.017 0.018 0.017 0.021 0.028 0.050 Recommended weighting scheme: WGHT 0.0282 0.7426 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)/su Fc/Fc(max) Resolution(A) -2 5 3 331.75 218.65 5.37 0.130 1.38 1 4 3 13.07 0.01 5.36 0.001 1.71 1 3 1 903.72 673.54 5.10 0.228 2.79 -2 2 3 16.93 1.16 4.80 0.009 1.64 2 1 3 1340.47 1083.07 4.36 0.289 1.68 -2 9 1 430.07 314.58 4.26 0.155 1.13 -2 10 1 8.56 0.69 4.00 0.007 1.04 3 0 4 47.92 16.21 3.90 0.035 1.20 -1 7 1 1252.18 1037.47 3.89 0.282 1.53 -2 1 5 369.29 286.06 3.29 0.148 1.22 -2 2 1 14.47 4.09 3.26 0.018 2.18 -1 12 3 7.08 0.06 3.25 0.002 0.88 2 4 1 16.73 6.26 3.09 0.022 1.82 -1 1 5 1213.32 1026.52 2.94 0.281 1.35 1 0 2 649.02 544.74 2.94 0.205 2.85 0 2 3 1322.14 1520.07 2.94 0.342 2.17 2 3 2 687.49 807.00 2.76 0.249 1.79 2 4 5 6.22 1.16 2.75 0.009 1.12 -3 2 1 552.07 645.45 2.67 0.223 1.56 -1 4 4 552.82 473.94 2.57 0.191 1.44 -2 1 2 119.15 152.41 2.51 0.108 2.01 0 4 0 39.57 24.96 2.47 0.044 2.90 1 4 1 6.53 1.65 2.46 0.011 2.35 0 8 0 6044.61 5446.15 2.45 0.647 1.45 0 8 5 5.78 0.05 2.42 0.002 1.01 -6 4 1 18.24 1.23 2.42 0.010 0.79 3 1 0 120.29 152.37 2.41 0.108 1.64 2 5 1 614.74 446.29 2.40 0.185 1.65 1 5 5 398.10 339.75 2.39 0.162 1.16 0 4 2 14685.22 13011.01 2.38 1.000 2.23 2 1 0 1077.07 1210.58 2.36 0.305 2.43 -1 5 2 341.13 398.86 2.35 0.175 1.81 1 4 7 3.79 0.23 2.33 0.004 0.93 -2 1 1 574.90 422.66 2.31 0.180 2.31 0 3 2 32.74 20.79 2.29 0.040 2.60 -1 9 1 872.01 775.23 2.27 0.244 1.23 2 5 5 675.44 592.09 2.26 0.213 1.08 -2 3 4 51.43 35.55 2.26 0.052 1.35 -2 3 3 643.64 501.32 2.26 0.196 1.57 -2 9 5 236.40 195.41 2.25 0.123 0.89 -2 3 2 48.61 30.69 2.21 0.049 1.80 0 12 4 76.62 99.74 2.14 0.088 0.85 5 0 2 2080.08 1837.33 2.14 0.376 0.95 -4 4 6 39.10 55.55 2.11 0.065 0.82 2 3 5 632.57 560.29 2.10 0.208 1.16 -1 3 2 1193.70 1326.56 2.09 0.319 2.31 -4 1 6 -1.10 1.57 2.07 0.011 0.85 -4 3 6 4.29 0.54 2.07 0.006 0.84 0 0 2 19.18 5.91 2.06 0.021 3.51 2 7 3 340.57 288.58 2.04 0.149 1.18 Bond lengths and angles C1 - Distance Angles N1 1.1373 (0.0039) C2 1.4499 (0.0040) 179.86 (0.38) C1 - N1 Rh1 - Distance Angles N1 1.9682 (0.0025) N1_$1 1.9682 (0.0025) 180.00 (0.18) Cl1 2.2891 (0.0007) 89.83 (0.08) 90.17 (0.08) Cl1_$1 2.2891 (0.0007) 90.17 (0.08) 89.83 (0.08) 180.00 (0.04) Rh1 - N1 N1_$1 Cl1 Cl1 - Distance Angles Rh1 2.2891 (0.0007) Cl1 - N1 - Distance Angles C1 1.1373 (0.0039) Rh1 1.9682 (0.0025) 179.33 (0.26) N1 - C1 C2 - Distance Angles C1 1.4499 (0.0040) C2 - FMAP and GRID set by program FMAP 2 3 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0277 for 919 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.07 at 0.1228 0.1225 0.2484 [ 1.24 A from CL1 ] Deepest hole -0.88 at 0.0444 0.9410 0.0601 [ 0.83 A from RH1 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 928 / 11817 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1228 0.1225 0.2484 1.00000 0.05 1.07 1.24 CL1 2.06 H2A 2.25 H2C 2.33 RH1 Q2 1 0.1282 -0.1173 0.2430 1.00000 0.05 1.03 1.02 N1 1.48 C1 2.27 RH1 2.41 H2C Q3 1 0.1702 0.0077 0.0659 1.00000 0.05 0.53 0.97 RH1 1.26 N1 2.34 CL1 2.35 C1 Q4 1 0.2597 0.0662 0.1833 1.00000 0.05 0.53 1.58 N1 1.97 RH1 2.07 CL1 2.28 C1 Q5 1 0.9064 -0.0405 0.5962 1.00000 0.05 0.47 1.49 H2C 1.85 CL1 2.25 N1 2.41 C2 Q6 1 0.7606 -0.0009 0.5037 1.00000 0.05 0.46 1.23 H2C 2.11 C2 2.23 C1 2.42 CL1 Q7 1 0.1174 -0.0392 0.3966 1.00000 0.05 0.44 1.79 N1 1.94 C1 2.03 H2C 2.07 H2C Q8 1 0.0213 0.1031 0.3656 1.00000 0.05 0.44 1.17 CL1 1.75 H2C 2.50 C2 2.63 H2B Q9 1 0.1595 0.0225 0.1558 1.00000 0.05 0.43 1.21 N1 1.37 RH1 1.93 CL1 2.17 C1 Q10 1 0.1676 -0.0332 0.1568 1.00000 0.05 0.39 0.67 N1 1.43 RH1 1.75 C1 2.40 CL1 Shortest distances between peaks (including symmetry equivalents) 9 10 0.65 3 9 0.66 4 9 0.73 3 10 0.79 5 8 0.85 5 7 0.93 1 8 0.99 6 7 1.03 1 4 1.05 5 6 1.07 3 4 1.15 2 10 1.16 4 10 1.25 1 9 1.34 2 7 1.41 1 5 1.45 7 10 1.71 7 8 1.73 2 9 1.74 5 7 1.76 4 5 1.79 5 9 1.79 4 8 1.81 6 8 1.84 7 9 1.85 1 3 1.86 5 6 1.87 8 9 1.88 5 5 1.90 2 3 1.92 1 10 1.93 3 3 1.93 7 8 1.96 5 10 1.97 6 7 1.99 6 8 2.03 4 7 2.06 7 7 2.08 1 7 2.14 2 5 2.16 2 4 2.26 3 9 2.28 8 10 2.28 3 10 2.30 2 6 2.31 1 6 2.31 4 6 2.33 6 6 2.38 5 8 2.40 3 7 2.40 6 9 2.43 3 5 2.44 6 10 2.44 3 8 2.50 9 10 2.72 9 9 2.74 2 8 2.75 1 2 2.78 10 10 2.85 2 8 2.86 2 5 2.87 3 4 2.88 2 3 2.91 1 6 2.93 2 6 2.93 1 7 2.94 Time profile in seconds ----------------------- 0.02: 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 0.02: OSF, H-atoms from difference map 0.02: 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 0.02: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:20:01 Total CPU time: 0.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++