++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + udel2 started at 12:01:59 on 26-Jan-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL UDel2 in P2(1)/c CELL 1.54178 5.4266 5.0403 21.6954 90.000 96.268 90.000 ZERR 4.00 0.0011 0.0010 0.0056 0.000 0.016 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 28 20 8 V = 589.86 F(000) = 252.0 Mu = 0.84 mm-1 Cell Wt = 484.44 Rho = 1.364 TEMP -173.150 SIZE 0.022 0.042 0.255 L.S. 4 BOND $H FMAP 2 PLAN 5 ACTA WGHT 0.1197 1.4383 FVAR 0.38894 C1 1 0.543501 1.029661 0.153403 11.00000 0.03186 0.02402 = 0.04311 0.00312 0.00832 -0.00092 H1 2 0.393481 0.930693 0.156493 11.00000 0.02343 C2 1 0.621423 1.224216 0.197072 11.00000 0.03950 0.03179 = 0.04083 -0.00089 0.00878 0.00427 H2 2 0.518089 1.258693 0.229913 11.00000 0.05524 C3 1 0.826490 1.378475 0.191035 11.00000 0.03894 0.02544 = 0.04544 -0.00178 0.00064 0.00349 H3 2 0.891813 1.516300 0.222231 11.00000 0.04860 C4 1 0.957695 1.340171 0.141812 11.00000 0.03083 0.02264 = 0.05497 0.00099 0.00699 -0.00073 H4 2 1.110239 1.450641 0.140048 11.00000 0.03003 C5 1 0.882814 1.145247 0.097901 11.00000 0.02918 0.02710 = 0.04603 0.00090 0.00886 0.00013 H5 2 0.985949 1.099185 0.063386 11.00000 0.02803 C6 1 0.676395 0.989759 0.103838 11.00000 0.02888 0.02126 = 0.03834 0.00299 0.00396 0.00199 C7 1 0.595055 0.780300 0.057255 11.00000 0.03174 0.01887 = 0.03828 0.00374 0.00605 0.00168 O1 3 0.716851 0.743737 0.013125 11.00000 0.03937 0.03166 = 0.04254 -0.00279 0.01374 -0.00491 O2 3 0.402901 0.643630 0.065524 11.00000 0.03560 0.02963 = 0.04769 -0.00287 0.01093 -0.00713 H2O 2 0.346013 0.478587 0.030467 11.00000 0.14800 HKLF 4 Covalent radii and connectivity table for UDel2 in P2(1)/c C 0.770 H 0.320 O 0.660 C1 - C6 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C1 C5 C7 C7 - O1 O2 C6 O1 - C7 O2 - C7 h k l Fo^2 Sigma Why rejected -1 0 1 4.00 0.42 observed but should be systematically absent -3 0 3 1.42 0.24 observed but should be systematically absent 0 3 0 5.64 0.85 observed but should be systematically absent 0 3 0 5.76 0.59 observed but should be systematically absent 0 5 0 5.75 1.26 observed but should be systematically absent 0 5 0 5.44 0.78 observed but should be systematically absent 0 5 0 4.95 1.14 observed but should be systematically absent -2 0 1 13.04 1.28 observed but should be systematically absent -2 0 1 16.26 1.33 observed but should be systematically absent -2 0 3 3.44 0.47 observed but should be systematically absent -2 0 3 4.92 0.57 observed but should be systematically absent -3 0 1 3.12 0.56 observed but should be systematically absent -3 0 1 3.59 0.44 observed but should be systematically absent -3 0 5 1.21 0.26 observed but should be systematically absent 3923 Reflections read, of which 220 rejected -6 =< h =< 5, -5 =< k =< 5, -25 =< l =< 25, Max. 2-theta = 137.90 14 Systematic absence violations 0 Inconsistent equivalents 1001 Unique reflections, of which 0 suppressed R(int) = 0.0545 R(sigma) = 0.0558 Friedel opposites merged Maximum memory for data reduction = 950 / 9978 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 28.00 28.00 H 20.00 24.00 O 8.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1200 / 136188 wR2 = 0.2674 before cycle 1 for 1001 data and 106 / 106 parameters GooF = S = 1.181; Restrained GooF = 1.181 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1197 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39181 0.00385 0.747 OSF Mean shift/esd = 0.199 Maximum = 0.747 for OSF Max. shift = 0.080 A for H2O Max. dU = 0.014 for H2O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1200 / 136188 wR2 = 0.2661 before cycle 2 for 1001 data and 106 / 106 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1197 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39253 0.00383 0.186 OSF Mean shift/esd = 0.081 Maximum = -0.716 for y H2O Max. shift = 0.092 A for H2O Max. dU = 0.008 for H2O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1200 / 136188 wR2 = 0.2657 before cycle 3 for 1001 data and 106 / 106 parameters GooF = S = 1.172; Restrained GooF = 1.172 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1197 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39253 0.00383 0.000 OSF Mean shift/esd = 0.024 Maximum = -0.533 for y H2O Max. shift = 0.071 A for H2O Max. dU = 0.001 for H2O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1200 / 136188 wR2 = 0.2656 before cycle 4 for 1001 data and 106 / 106 parameters GooF = S = 1.171; Restrained GooF = 1.171 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1197 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39249 0.00383 -0.010 OSF Mean shift/esd = 0.018 Maximum = -0.397 for y H2O Max. shift = 0.053 A for H2O Max. dU = 0.000 for H2O No correlation matrix elements larger than 0.500 UDel2 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.54359 1.02949 0.15336 1.00000 0.03092 0.02290 0.04511 0.00297 0.00806 -0.00171 0.03269 0.00854 0.00084 0.00090 0.00021 0.00000 0.00246 0.00241 0.00277 0.00182 0.00189 0.00185 0.00113 H1 0.39408 0.93040 0.15658 1.00000 0.02102 0.07913 0.00806 0.00917 0.00188 0.00000 0.01051 C2 0.62195 1.22442 0.19707 1.00000 0.04135 0.03111 0.04105 -0.00095 0.00877 0.00440 0.03753 0.00909 0.00091 0.00097 0.00023 0.00000 0.00280 0.00266 0.00274 0.00201 0.00208 0.00204 0.00120 H2 0.51948 1.26030 0.23032 1.00000 0.05403 0.10843 0.01094 0.01214 0.00267 0.00000 0.01656 C3 0.82657 1.37827 0.19105 1.00000 0.03967 0.02562 0.04542 -0.00266 0.00004 0.00318 0.03724 0.00925 0.00093 0.00098 0.00024 0.00000 0.00268 0.00247 0.00274 0.00205 0.00205 0.00200 0.00117 H3 0.88534 1.51057 0.22167 1.00000 0.04978 0.10550 0.01001 0.01231 0.00256 0.00000 0.01553 C4 0.95760 1.33994 0.14176 1.00000 0.03124 0.02289 0.05555 0.00105 0.00665 -0.00092 0.03642 0.00900 0.00089 0.00093 0.00024 0.00000 0.00249 0.00248 0.00306 0.00196 0.00200 0.00184 0.00120 H4 1.10725 1.45691 0.13928 1.00000 0.02710 0.08298 0.00840 0.00977 0.00195 0.00000 0.01148 C5 0.88280 1.14578 0.09791 1.00000 0.02902 0.02597 0.04801 0.00008 0.00919 -0.00035 0.03396 0.00867 0.00084 0.00092 0.00023 0.00000 0.00241 0.00244 0.00279 0.00196 0.00194 0.00182 0.00114 H5 0.98563 1.10334 0.06320 1.00000 0.02327 0.07758 0.00816 0.00898 0.00200 0.00000 0.01085 C6 0.67636 0.98973 0.10391 1.00000 0.02967 0.02197 0.03940 0.00296 0.00460 0.00173 0.03029 0.00804 0.00080 0.00086 0.00020 0.00000 0.00221 0.00233 0.00256 0.00174 0.00180 0.00176 0.00108 C7 0.59532 0.78065 0.05728 1.00000 0.03156 0.01882 0.04065 0.00329 0.00662 0.00129 0.03014 0.00815 0.00079 0.00083 0.00021 0.00000 0.00236 0.00219 0.00255 0.00179 0.00184 0.00174 0.00107 O1 0.71683 0.74401 0.01320 1.00000 0.04073 0.03068 0.04365 -0.00314 0.01424 -0.00597 0.03765 0.00606 0.00061 0.00065 0.00015 0.00000 0.00192 0.00185 0.00196 0.00140 0.00143 0.00147 0.00096 O2 0.40269 0.64380 0.06543 1.00000 0.03599 0.02972 0.04977 -0.00277 0.01155 -0.00660 0.03799 0.00588 0.00059 0.00064 0.00016 0.00000 0.00191 0.00188 0.00202 0.00142 0.00142 0.00140 0.00096 H2O 0.33684 0.42135 0.02817 1.00000 0.17148 0.21320 0.01942 0.02610 0.00484 0.00000 0.04497 Final Structure Factor Calculation for UDel2 in P2(1)/c Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1094 / 21973 wR2 = 0.2655 before cycle 5 for 1001 data and 0 / 106 parameters GooF = S = 1.171; Restrained GooF = 1.171 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1197 * P )^2 + 1.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0838 for 789 Fo > 4sig(Fo) and 0.0967 for all 1001 data wR2 = 0.2655, GooF = S = 1.171, Restrained GooF = 1.171 for all data Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0460 0.0303 0.0218 C1 0.0455 0.0383 0.0287 C2 0.0493 0.0377 0.0247 C3 0.0556 0.0309 0.0227 C4 0.0488 0.0273 0.0259 C5 0.0399 0.0297 0.0213 C6 0.0416 0.0305 0.0183 C7 0.0526 0.0329 0.0275 O1 0.0530 0.0358 0.0253 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.020 0.031 0.044 0.056 0.075 0.097 0.126 0.192 1.000 Number in group 100. 110. 93. 108. 89. 103. 102. 97. 98. 101. GooF 1.081 1.715 1.285 0.943 1.066 1.205 1.145 0.946 1.114 0.942 K 10.413 3.541 1.425 1.115 1.128 1.128 1.056 0.988 1.011 1.016 Resolution(A) 0.83 0.88 0.91 0.95 1.00 1.06 1.15 1.26 1.45 1.80 inf Number in group 106. 96. 99. 100. 102. 98. 100. 99. 100. 101. GooF 1.060 1.003 0.940 1.267 1.292 1.322 1.045 1.073 1.299 1.317 K 1.154 1.116 1.150 1.077 0.982 1.015 0.940 0.916 0.970 1.058 R1 0.161 0.129 0.143 0.141 0.118 0.107 0.100 0.103 0.075 0.056 Recommended weighting scheme: WGHT 0.1016 1.7911 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 5 1 81.73 0.97 6.86 0.012 0.99 -6 2 3 47.98 1.56 6.04 0.016 0.85 -4 3 4 76.41 2.35 5.57 0.019 1.05 -2 4 1 56.10 0.58 5.28 0.010 1.14 -2 3 1 40.53 5.82 5.23 0.031 1.43 -1 3 3 52.57 6.67 5.22 0.033 1.58 -6 1 2 65.76 12.83 5.07 0.045 0.89 1 4 1 55.80 0.01 4.90 0.001 1.22 -4 3 1 35.43 1.77 4.61 0.017 1.05 2 2 0 128.39 49.70 4.51 0.089 1.84 -5 2 2 28.20 4.90 4.24 0.028 1.00 -3 1 2 29.28 3.69 4.17 0.024 1.70 -3 4 2 37.00 3.40 4.17 0.023 1.03 2 4 1 408.78 137.70 4.15 0.148 1.14 -2 1 3 63.05 21.83 4.11 0.059 2.33 1 2 0 71.22 24.67 4.05 0.063 2.28 -2 4 3 45.90 0.18 4.02 0.005 1.14 -5 1 2 89.72 33.95 3.76 0.074 1.06 -1 3 1 317.87 182.51 3.29 0.171 1.60 2 4 0 114.45 53.39 3.16 0.092 1.14 -3 2 2 50.32 18.66 3.13 0.055 1.47 -1 2 2 132.38 63.97 3.12 0.101 2.25 1 3 1 107.62 52.70 3.11 0.092 1.60 -5 2 3 15.08 1.63 3.02 0.016 1.00 -3 5 3 13.98 2.25 3.00 0.019 0.88 -2 5 4 75.22 38.74 2.89 0.079 0.94 -2 5 3 123.02 70.36 2.87 0.106 0.94 0 5 2 49.42 23.13 2.78 0.061 1.00 0 4 1 7.33 0.04 2.68 0.002 1.26 -2 2 2 305.36 203.54 2.59 0.180 1.84 -3 1 1 101.10 57.75 2.45 0.096 1.70 -3 5 1 8.80 1.02 2.43 0.013 0.88 -5 1 5 116.73 55.56 2.39 0.094 1.05 -6 2 2 124.13 75.80 2.35 0.110 0.85 2 1 0 256.20 174.15 2.34 0.167 2.38 0 2 0 1160.23 827.45 2.33 0.364 2.52 -4 2 2 24.75 10.79 2.32 0.042 1.19 -5 1 3 79.02 48.09 2.27 0.088 1.06 4 4 0 34.06 15.43 2.26 0.050 0.92 -5 0 6 12.72 2.14 2.23 0.018 1.07 -2 3 3 57.56 31.39 2.22 0.071 1.41 -1 5 1 334.90 229.73 2.21 0.192 0.99 -2 1 1 590.96 426.70 2.20 0.261 2.39 -4 3 5 29.81 13.87 2.16 0.047 1.04 -3 3 2 41.18 20.69 2.06 0.058 1.23 -3 3 4 25.70 0.53 1.96 0.009 1.22 2 5 1 38.21 16.23 1.96 0.051 0.94 -3 3 6 77.14 115.34 1.89 0.136 1.19 -6 2 1 135.36 92.50 1.88 0.122 0.85 -4 4 3 14.03 0.34 1.87 0.007 0.92 Bond lengths and angles C1 - Distance Angles C6 1.3708 (0.0062) C2 1.3991 (0.0067) 119.10 (0.43) H1 0.9617 (0.0448) 120.04 (2.58) 120.78 (2.57) C1 - C6 C2 C2 - Distance Angles C3 1.3722 (0.0069) C1 1.3991 (0.0067) 121.43 (0.45) H2 0.9746 (0.0559) 119.91 (3.64) 118.44 (3.66) C2 - C3 C1 C3 - Distance Angles C4 1.3610 (0.0070) C2 1.3722 (0.0069) 119.49 (0.48) H3 0.9704 (0.0593) 118.34 (3.39) 122.14 (3.38) C3 - C4 C2 C4 - Distance Angles C3 1.3610 (0.0070) C5 1.3941 (0.0069) 119.85 (0.45) H4 1.0097 (0.0477) 116.82 (2.53) 123.34 (2.53) C4 - C3 C5 C5 - Distance Angles C6 1.3865 (0.0062) C4 1.3941 (0.0069) 120.81 (0.43) H5 1.0078 (0.0443) 117.95 (2.56) 121.00 (2.57) C5 - C6 C4 C6 - Distance Angles C1 1.3708 (0.0062) C5 1.3865 (0.0062) 119.32 (0.43) C7 1.4934 (0.0062) 119.49 (0.40) 121.19 (0.41) C6 - C1 C5 C7 - Distance Angles O1 1.2333 (0.0051) O2 1.2807 (0.0051) 122.68 (0.42) C6 1.4934 (0.0062) 119.21 (0.39) 118.09 (0.39) C7 - O1 O2 O1 - Distance Angles C7 1.2333 (0.0051) O1 - O2 - Distance Angles C7 1.2807 (0.0051) H2O 1.4053 (0.1238) 120.69 (4.01) O2 - C7 FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 -2 -1 4.545 2 1 R1 = 0.0966 for 1001 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.41 at 0.2513 0.2364 0.4394 [ 0.86 A from C7 ] Deepest hole -0.29 at 0.2281 0.4344 0.0390 [ 0.66 A from H2O ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1265 / 14800 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7487 0.7364 0.0606 1.00000 0.05 0.41 0.86 C7 1.02 O1 1.66 C6 1.95 O2 Q2 1 0.5605 0.7800 -0.0017 1.00000 0.05 0.32 0.89 O1 1.27 C7 1.32 H2O 1.90 O2 Q3 1 0.2605 0.7277 0.0599 1.00000 0.05 0.32 0.88 O2 1.76 H2O 1.84 C7 2.37 H1 Q4 1 0.2844 0.2681 0.0359 1.00000 0.05 0.31 0.85 H2O 1.07 O1 1.97 H5 2.08 O2 Q5 1 0.5216 1.0419 0.1008 1.00000 0.05 0.30 0.88 C6 1.13 C1 1.56 H1 1.69 C7 Shortest distances between peaks (including symmetry equivalents) 2 4 1.21 1 2 1.62 1 4 2.08 4 5 2.13 1 5 2.21 2 3 2.23 3 5 2.24 2 2 2.32 2 5 2.33 3 4 2.38 2 5 2.61 1 3 2.65 2 3 2.99 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. 0.02: 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 0.00: 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 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + udel2 finished at 12:01:59 Total CPU time: 0.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++