+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0059p21c started at 13:24:16 on 07-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 0059 in P2(1)/c CELL 0.71073 17.1242 7.4638 7.6228 90.000 91.048 90.000 ZERR 2.00 0.0011 0.0005 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O LA W S UNIT 20 20 32 4 4 4 V = 974.12 F(000) = 984.0 Mu = 16.36 mm-1 Cell Wt = 2191.64 Rho = 3.736 MERG 2 OMIT -3.00 55.00 DFIX 0.85 O1W H1W O1W H2W DANG 1.37 H1W H2W SHEL 7 0.77 EQIV_$1 x, -y+1/2, z-1/2 HTAB O1w O21_$1 EQIV_$2 x, -y+1/2, z-1/2 HTAB O1W S1_$2 EQIV_$3 x, y-1, z HTAB O1W S1_$3 HTAB O1W O21_$3 ISOR 0.01 C1 C2 C3 C4 C5 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.10 ACTA BOND $H WGHT 0.00000 73.80040 L.S. 4 TEMP -153.00 FVAR 0.20626 C1 1 0.096264 0.392626 0.061836 11.00000 0.01788 0.01774 = 0.01782 -0.00637 -0.00058 -0.00338 C2 1 0.074094 0.226762 0.114277 11.00000 0.01165 0.01386 = 0.02078 -0.00532 -0.00045 0.00703 AFIX 43 H2 2 0.112447 0.141402 0.149402 11.00000 -1.20000 AFIX 0 C3 1 -0.005802 0.180878 0.116720 11.00000 0.02456 0.01728 = 0.00530 -0.00656 0.00077 0.00017 AFIX 43 H3 2 -0.021124 0.065427 0.155696 11.00000 -1.20000 AFIX 0 C4 1 0.040095 0.524278 -0.002678 11.00000 0.01864 0.01927 = 0.01630 -0.00061 -0.00282 0.00587 C5 1 0.061812 0.697009 -0.062730 11.00000 0.01464 0.01109 = 0.01473 -0.00021 0.00077 -0.00324 AFIX 43 H5 2 0.115479 0.728889 -0.065784 11.00000 -1.20000 AFIX 0 O3 3 0.391866 0.444029 0.049217 11.00000 0.03038 0.02657 = 0.02104 0.00093 0.01047 0.00374 O4 3 0.373414 0.405828 0.410314 11.00000 0.02816 0.00716 = 0.03269 0.00310 -0.00397 0.00391 O21 3 0.197302 0.605026 0.210683 11.00000 0.03758 0.01519 = 0.01505 0.00252 -0.00078 -0.00560 O22 3 0.224630 0.502082 -0.084984 11.00000 0.02053 0.03099 = 0.02440 0.00352 -0.00042 0.00380 O23 3 0.234761 0.295099 0.159772 11.00000 0.01626 0.02431 = 0.03067 0.00755 -0.00687 0.00577 O1W 3 0.240270 -0.072550 0.064872 11.00000 0.03161 0.01961 = 0.01702 0.00585 -0.00628 -0.01735 H2W 2 0.225736 -0.077745 -0.042306 11.00000 0.05125 H1W 2 0.222288 -0.164525 0.116246 11.00000 0.01269 MOLE 1 O1 3 0.514517 0.580838 0.282814 11.00000 0.03031 0.01779 = 0.01052 0.00394 0.00675 -0.00268 O2 3 0.368528 0.768637 0.256501 11.00000 0.01821 0.01475 = 0.02651 0.00119 -0.00528 -0.00060 LA1 4 0.344503 0.091709 0.237683 11.00000 0.01680 0.01076 = 0.01372 0.00018 0.00009 0.00049 W1 5 0.413408 0.555152 0.250771 11.00000 0.01675 0.00959 = 0.01447 -0.00009 0.00006 -0.00006 S1 6 0.195573 0.453749 0.087462 11.00000 0.01898 0.01413 = 0.01774 0.00195 0.00048 -0.00058 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 0059 in P2(1)/c C 0.770 H 0.320 O 0.660 LA 1.870 W 1.370 S 1.030 C1 - C2 C4 S1 C2 - C1 C3 C3 - C5_$4 C2 C4 - C5 C4_$4 C1 C5 - C3_$4 C4 O3 - W1 La1_$1 O4 - W1 La1_$5 La1 O21 - S1 O22 - S1 La1_$1 O23 - S1 La1 O1W - La1 O1 - W1 La1_$8 O2 - W1 La1_$7 La1 - O1_$6 O2_$3 O23 O3_$5 O1W O4_$1 O22_$5 O4 W1 W1 - O1 O2 O3 O4 La1 S1 - O22 O23 O21 C1 Operators for generating equivalent atoms: $1 x, -y+1/2, z-1/2 $2 x, -y+1/2, z-1/2 $3 x, y-1, z $4 -x, -y+1, -z $5 x, -y+1/2, z+1/2 $6 -x+1, y-1/2, -z+1/2 $7 x, y+1, z $8 -x+1, y+1/2, -z+1/2 11175 Reflections read, of which 605 rejected -22 =< h =< 22, -9 =< k =< 9, -9 =< l =< 9, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2214 Unique reflections, of which 0 suppressed R(int) = 0.0782 R(sigma) = 0.0627 Friedel opposites merged Maximum memory for data reduction = 1868 / 21965 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 = 2243 / 193492 wR2 = 0.1255 before cycle 1 for 2214 data and 153 / 153 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.001 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.121; Restrained GooF = 1.113 for 33 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 73.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.20626 0.00054 -0.005 OSF Mean shift/su = 0.001 Maximum = 0.012 for U23 W1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2243 / 193492 wR2 = 0.1255 before cycle 2 for 2214 data and 153 / 153 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.001 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.121; Restrained GooF = 1.113 for 33 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 73.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.20626 0.00054 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.004 for U23 W1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2243 / 193492 wR2 = 0.1255 before cycle 3 for 2214 data and 153 / 153 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.001 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.121; Restrained GooF = 1.113 for 33 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 73.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.20626 0.00054 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x W1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2243 / 193492 wR2 = 0.1255 before cycle 4 for 2214 data and 153 / 153 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.001 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.121; Restrained GooF = 1.113 for 33 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 73.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.20626 0.00054 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x W1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Largest correlation matrix elements -0.913 z H2W / x H2W -0.612 z H1W / y H2W 0.667 z H1W / y H1W -0.605 y H1W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1124 0.1414 0.1494 43 0.950 0.000 C2 C1 C3 H3 -0.0211 0.0654 0.1557 43 0.950 0.000 C3 C5_$4 C2 H5 0.1155 0.7289 -0.0658 43 0.950 0.000 C5 C3_$4 C4 0059 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09626 0.39263 0.06184 1.00000 0.01788 0.01774 0.01781 -0.00638 -0.00058 -0.00338 0.01782 0.02571 0.00091 0.00214 0.00198 0.00000 0.00638 0.00635 0.00605 0.00519 0.00517 0.00534 0.00317 C2 0.07409 0.22676 0.11428 1.00000 0.01165 0.01386 0.02078 -0.00532 -0.00044 0.00704 0.01544 0.02583 0.00086 0.00203 0.00196 0.00000 0.00597 0.00608 0.00620 0.00511 0.00499 0.00504 0.00303 H2 0.11245 0.14140 0.14940 1.00000 0.01853 0.00000 0.00000 C3 -0.00580 0.18088 0.11672 1.00000 0.02455 0.01728 0.00530 -0.00657 0.00077 0.00017 0.01571 0.02535 0.00092 0.00211 0.00179 0.00000 0.00660 0.00621 0.00525 0.00477 0.00489 0.00535 0.00302 H3 -0.02112 0.06543 0.15570 1.00000 0.01885 0.00000 0.00000 C4 0.04009 0.52428 -0.00268 1.00000 0.01864 0.01927 0.01630 -0.00061 -0.00282 0.00587 0.01811 0.02722 0.00090 0.00219 0.00196 0.00000 0.00634 0.00644 0.00588 0.00517 0.00504 0.00541 0.00315 C5 0.06181 0.69701 -0.06273 1.00000 0.01464 0.01109 0.01472 -0.00021 0.00077 -0.00324 0.01348 0.02494 0.00088 0.00196 0.00186 0.00000 0.00607 0.00584 0.00583 0.00482 0.00486 0.00501 0.00290 H5 0.11548 0.72889 -0.06578 1.00000 0.01617 0.00000 0.00000 O3 0.39187 0.44403 0.04922 1.00000 0.03038 0.02656 0.02104 0.00093 0.01047 0.00374 0.02587 0.02177 0.00071 0.00164 0.00148 0.00000 0.00673 0.00661 0.00582 0.00491 0.00495 0.00534 0.00265 O4 0.37341 0.40583 0.41031 1.00000 0.02815 0.00716 0.03269 0.00310 -0.00396 0.00391 0.02272 0.01984 0.00068 0.00141 0.00154 0.00000 0.00653 0.00524 0.00651 0.00450 0.00509 0.00456 0.00253 O21 0.19730 0.60503 0.21068 1.00000 0.03758 0.01519 0.01505 0.00252 -0.00078 -0.00560 0.02262 0.01954 0.00072 0.00149 0.00140 0.00000 0.00707 0.00563 0.00527 0.00440 0.00473 0.00500 0.00251 O22 0.22463 0.50208 -0.08498 1.00000 0.02053 0.03099 0.02440 0.00352 -0.00042 0.00380 0.02532 0.02122 0.00067 0.00171 0.00149 0.00000 0.00603 0.00692 0.00600 0.00507 0.00472 0.00513 0.00262 O23 0.23476 0.29510 0.15977 1.00000 0.01626 0.02431 0.03068 0.00755 -0.00687 0.00577 0.02384 0.02077 0.00065 0.00162 0.00154 0.00000 0.00581 0.00632 0.00647 0.00506 0.00475 0.00481 0.00257 O1W 0.24027 -0.07255 0.06487 1.00000 0.03161 0.01961 0.01702 0.00585 -0.00628 -0.01735 0.02283 0.01833 0.00071 0.00155 0.00145 0.00000 0.00674 0.00618 0.00565 0.00450 0.00487 0.00515 0.00259 H2W 0.22573 -0.07776 -0.04230 1.00000 0.05129 0.18040 0.01211 0.02320 0.00778 0.00000 0.07102 H1W 0.22230 -0.16452 0.11626 1.00000 0.01262 0.22498 0.00887 0.01301 0.01637 0.00000 0.04239 O1 0.51452 0.58084 0.28281 1.00000 0.03031 0.01779 0.01052 0.00394 0.00676 -0.00268 0.01946 0.01927 0.00067 0.00147 0.00131 0.00000 0.00642 0.00588 0.00497 0.00411 0.00439 0.00481 0.00239 O2 0.36853 0.76864 0.25650 1.00000 0.01820 0.01475 0.02651 0.00119 -0.00528 -0.00060 0.01989 0.01861 0.00064 0.00146 0.00144 0.00000 0.00574 0.00558 0.00616 0.00454 0.00458 0.00449 0.00239 La1 0.34450 0.09171 0.23768 1.00000 0.01680 0.01076 0.01372 0.00018 0.00009 0.00049 0.01376 0.00148 0.00005 0.00011 0.00011 0.00000 0.00045 0.00041 0.00041 0.00030 0.00031 0.00032 0.00021 W1 0.41341 0.55515 0.25077 1.00000 0.01675 0.00959 0.01447 -0.00009 0.00006 -0.00006 0.01361 0.00103 0.00004 0.00008 0.00008 0.00000 0.00032 0.00029 0.00029 0.00022 0.00021 0.00023 0.00018 S1 0.19557 0.45375 0.08746 1.00000 0.01898 0.01413 0.01774 0.00195 0.00048 -0.00058 0.01695 0.00667 0.00023 0.00052 0.00048 0.00000 0.00190 0.00181 0.00178 0.00144 0.00144 0.00149 0.00076 Final Structure Factor Calculation for 0059 in P2(1)/c Total number of l.s. parameters = 153 Maximum vector length = 511 Memory required = 2090 / 25039 wR2 = 0.1255 before cycle 5 for 2214 data and 0 / 153 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 30. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.001 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.121; Restrained GooF = 1.113 for 33 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 73.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0595 for 1871 Fo > 4sig(Fo) and 0.0770 for all 2214 data wR2 = 0.1255, GooF = S = 1.121, Restrained GooF = 1.113 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0246 0.0186 0.0102 C1 0.0252 0.0161 0.0050 C2 0.0246 0.0202 0.0024 C3 0.0256 0.0165 0.0122 C4 0.0167 0.0146 0.0092 C5 0.0378 0.0255 0.0144 O3 0.0356 0.0267 0.0059 O4 0.0391 0.0167 0.0121 O21 0.0333 0.0240 0.0186 O22 0.0363 0.0264 0.0088 O23 0.0468 0.0146 0.0071 O1W 0.0322 0.0195 0.0066 O1 0.0296 0.0154 0.0146 O2 0.0169 0.0137 0.0107 La1 0.0168 0.0145 0.0096 W1 0.0191 0.0186 0.0132 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.029 0.051 0.074 0.097 0.121 0.149 0.188 0.232 0.297 1.000 Number in group 227. 218. 225. 219. 218. 225. 221. 221. 217. 223. GooF 1.452 1.256 1.164 1.170 1.077 0.961 1.019 0.955 1.066 0.982 K 4.440 1.254 1.080 1.086 0.999 0.996 0.981 1.008 1.002 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.67 inf Number in group 232. 215. 225. 219. 219. 223. 218. 219. 224. 220. GooF 1.359 1.226 1.193 1.091 1.199 1.150 0.987 1.005 0.921 0.986 K 0.926 1.042 1.041 1.017 1.050 1.025 1.028 1.015 1.007 0.990 R1 0.159 0.130 0.124 0.092 0.082 0.076 0.059 0.050 0.037 0.031 Recommended weighting scheme: WGHT 0.0000 73.7821 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) 0 4 9 10593.39 19669.13 3.89 0.283 0.77 -19 1 2 1454.54 203.17 3.73 0.029 0.87 -1 3 7 3608.08 1585.99 3.66 0.080 1.00 -2 2 6 1536.42 350.90 3.60 0.038 1.19 5 9 2 389.70 2192.57 3.44 0.094 0.79 7 7 4 1866.46 503.41 3.40 0.045 0.87 -2 7 6 9416.97 14261.88 3.27 0.241 0.81 -10 5 3 929.81 203.23 3.11 0.029 1.03 2 1 0 723.87 89.22 3.10 0.019 5.63 -17 1 2 3464.65 1214.95 3.10 0.070 0.97 -11 4 5 11047.85 7239.17 3.07 0.172 0.95 -10 0 8 1320.96 58.30 3.01 0.015 0.84 0 7 2 1442.30 430.11 3.00 0.042 1.03 16 2 6 3535.49 5823.35 3.00 0.154 0.79 -10 4 3 1738.36 3217.11 2.96 0.114 1.14 -9 4 1 436.50 1.62 2.95 0.003 1.32 -1 6 7 4341.09 1948.03 2.95 0.089 0.82 -1 0 2 220980.02 245711.42 2.93 1.000 3.73 9 3 8 5785.54 8846.07 2.93 0.190 0.80 10 0 2 841.67 70.41 2.89 0.017 1.55 2 4 7 878.63 30.66 2.86 0.011 0.93 4 6 1 1283.12 461.35 2.85 0.043 1.18 19 1 1 8613.23 5845.76 2.83 0.154 0.89 -15 3 2 1167.61 94.52 2.80 0.020 1.01 10 1 1 3276.47 1916.60 2.79 0.088 1.62 -9 4 6 -20.93 1030.97 2.77 0.065 0.93 20 1 1 17253.91 13146.85 2.77 0.231 0.84 14 0 2 6014.90 3777.02 2.69 0.124 1.16 2 3 0 2087.01 953.75 2.68 0.062 2.39 1 1 1 1323.40 570.51 2.66 0.048 5.07 16 0 2 37168.57 29467.64 2.66 0.346 1.03 -8 2 3 459.64 12.35 2.65 0.007 1.51 -12 5 4 4449.37 2423.28 2.62 0.099 0.91 -8 0 4 642.82 56.26 2.62 0.015 1.44 -1 7 6 5887.94 3425.53 2.62 0.118 0.82 0 1 8 2099.85 978.65 2.61 0.063 0.95 6 6 6 1385.70 471.20 2.56 0.044 0.85 12 7 1 5685.38 2056.38 2.54 0.091 0.85 1 4 7 25717.08 21193.55 2.53 0.294 0.94 -9 8 2 1691.98 61.78 2.51 0.016 0.82 18 5 2 852.11 27.53 2.48 0.011 0.78 -19 2 4 2659.85 41.28 2.46 0.013 0.80 4 8 1 2868.11 1162.13 2.44 0.069 0.90 4 8 4 731.50 2044.93 2.42 0.091 0.82 -3 1 6 1241.63 112.83 2.41 0.021 1.23 8 8 3 1253.45 221.44 2.39 0.030 0.81 -11 4 7 2581.94 4354.94 2.37 0.133 0.81 -17 3 5 1754.34 61.47 2.36 0.016 0.80 14 7 2 10925.50 14961.81 2.35 0.247 0.78 8 1 9 13555.94 18137.30 2.33 0.272 0.78 Bond lengths and angles C1 - Distance Angles C2 1.3572 (0.0220) C4 1.4544 (0.0216) 121.94 (1.44) S1 1.7681 (0.0157) 118.45 (1.23) 119.46 (1.19) C1 - C2 C4 C2 - Distance Angles C1 1.3572 (0.0220) C3 1.4108 (0.0213) 120.12 (1.41) H2 0.9500 119.94 119.94 C2 - C1 C3 C3 - Distance Angles C5_$4 1.3804 (0.0213) C2 1.4108 (0.0213) 120.30 (1.45) H3 0.9500 119.85 119.85 C3 - C5_$4 C2 C4 - Distance Angles C5 1.4199 (0.0215) C4_$4 1.4215 (0.0316) 119.97 (1.76) C1 1.4544 (0.0217) 123.16 (1.42) 116.83 (1.82) C4 - C5 C4_$4 C5 - Distance Angles C3_$4 1.3804 (0.0213) C4 1.4199 (0.0215) 120.73 (1.40) H5 0.9500 119.64 119.64 C5 - C3_$4 C4 O3 - Distance Angles W1 1.7787 (0.0119) La1_$1 2.5096 (0.0118) 157.71 (0.66) O3 - W1 O4 - Distance Angles W1 1.7946 (0.0115) La1_$5 2.5530 (0.0119) 137.83 (0.56) La1 2.7294 (0.0111) 105.95 (0.51) 116.15 (0.41) O4 - W1 La1_$5 O21 - Distance Angles S1 1.4687 (0.0115) O21 - O22 - Distance Angles S1 1.4593 (0.0119) La1_$1 2.5754 (0.0116) 133.93 (0.68) O22 - S1 O23 - Distance Angles S1 1.4638 (0.0116) La1 2.4795 (0.0109) 157.77 (0.75) O23 - S1 O1W - Distance Angles La1 2.5176 (0.0106) H2W 0.8506 (0.0205) 135.81 (9.99) H1W 0.8508 (0.0204) 114.27 (9.70) 107.66 (5.21) O1W - La1 H2W O1 - Distance Angles W1 1.7546 (0.0115) La1_$8 2.4234 (0.0115) 167.50 (0.58) O1 - W1 O2 - Distance Angles W1 1.7699 (0.0110) La1_$7 2.4500 (0.0109) 163.17 (0.62) O2 - W1 La1 - Distance Angles O1_$6 2.4234 (0.0115) O2_$3 2.4500 (0.0109) 78.72 (0.36) O23 2.4795 (0.0109) 139.17 (0.39) 137.93 (0.38) O3_$5 2.5096 (0.0118) 75.66 (0.36) 77.82 (0.38) 121.48 (0.39) O1W 2.5176 (0.0106) 130.36 (0.38) 70.61 (0.38) 69.26 (0.41) 131.08 (0.37) O4_$1 2.5530 (0.0120) 74.10 (0.35) 91.66 (0.35) 85.48 (0.38) 149.39 (0.37) 68.92 (0.36) O22_$5 2.5754 (0.0116) 146.02 (0.37) 80.58 (0.39) 71.59 (0.40) 73.82 (0.37) 65.04 (0.37) 133.29 (0.36) O4 2.7294 (0.0111) 83.55 (0.35) 142.04 (0.34) 73.71 (0.37) 65.32 (0.37) 142.30 (0.38) 115.36 (0.29) 96.88 (0.37) W1 3.6555 (0.0010) 73.26 (0.26) 151.16 (0.26) 70.73 (0.28) 88.63 (0.28) 134.47 (0.27) 87.23 (0.24) 120.19 (0.28) La1 - O1_$6 O2_$3 O23 O3_$5 O1W O4_$1 O22_$5 W1 - Distance Angles O1 1.7546 (0.0116) O2 1.7699 (0.0110) 109.03 (0.50) O3 1.7787 (0.0119) 111.08 (0.51) 110.97 (0.52) O4 1.7946 (0.0115) 111.18 (0.49) 111.78 (0.51) 102.71 (0.53) La1 3.6555 (0.0010) 115.11 (0.36) 135.44 (0.36) 58.23 (0.39) 45.88 (0.36) W1 - O1 O2 O3 O4 S1 - Distance Angles O22 1.4593 (0.0119) O23 1.4638 (0.0116) 112.19 (0.72) O21 1.4687 (0.0115) 112.51 (0.70) 112.17 (0.69) C1 1.7681 (0.0157) 107.90 (0.71) 105.44 (0.74) 106.09 (0.73) S1 - O22 O23 O21 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.85(2) 1.95(3) 2.796(15) 176(22) O1W-H2W...O21_$1 0.85(2) 3.01(6) 3.810(12) 158(13) O1W-H2W...S1_$2 0.85(2) 2.89(9) 3.622(12) 145(13) O1W-H1W...S1_$3 0.85(2) 1.92(4) 2.756(15) 169(16) O1W-H1W...O21_$3 FMAP and GRID set by program FMAP 2 2 19 GRID 21.875 -2 -1 3.125 2 1 R1 = 0.0737 for 2214 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.08 at 0.3382 0.4086 0.8436 [ 0.82 A from LA1 ] Deepest hole -2.51 at 0.4521 0.5639 0.1816 [ 0.86 A from W1 ] Mean = 0.00, Rms deviation from mean = 0.47 e/A^3, Highest memory used = 2330 / 21448 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3382 0.0914 0.3436 1.00000 0.05 2.08 0.82 LA1 1.82 O3 2.15 O22 2.47 O4 Q2 1 0.1978 0.0417 -0.1277 1.00000 0.05 1.95 1.20 H2W 1.65 O21 1.84 O1W 2.13 O23 Q3 1 0.4563 0.4596 0.0228 1.00000 0.05 1.84 1.13 O3 2.03 W1 2.38 O1 2.41 O1 Q4 1 0.1916 0.0853 -0.0398 1.00000 0.05 1.82 1.35 H2W 1.64 O1W 2.04 H2 2.27 H1W Q5 1 0.4184 0.5784 0.1232 1.00000 0.05 1.77 0.99 W1 1.23 O3 1.95 O2 2.03 O1 Q6 1 0.3455 0.5694 0.2833 1.00000 0.05 1.74 1.20 W1 1.55 O2 1.62 O4 2.18 O3 Q7 1 0.4094 0.4434 0.3534 1.00000 0.05 1.73 0.81 O4 1.15 W1 2.15 O1 2.33 O3 Q8 1 0.1895 -0.0821 0.2161 1.00000 0.05 1.71 1.14 H1W 1.46 O1W 1.73 O22 2.08 H2W Q9 1 0.4113 0.4370 0.1396 1.00000 0.05 1.71 0.76 O3 1.22 W1 2.19 O4 2.32 O1 Q10 1 0.1060 0.0410 0.3169 1.00000 0.05 1.65 1.49 H2 1.86 C4 1.94 C1 2.14 C2 Shortest distances between peaks (including symmetry equivalents) 2 4 0.75 5 9 1.07 3 9 1.20 3 5 1.34 6 7 1.53 7 9 1.63 3 3 1.66 5 6 1.76 6 9 1.87 8 10 1.88 5 7 2.03 4 8 2.32 1 3 2.45 3 5 2.45 1 9 2.57 3 7 2.66 3 9 2.71 2 6 2.76 2 8 2.78 1 5 2.82 3 6 2.89 1 7 2.90 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.50: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.28: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0059p21c finished at 13:24:18 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++