+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0408 started at 12:52:03 on 03-Aug-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0408 in P2(1)/c CELL 0.71073 15.2671 14.7379 10.5379 90.000 95.004 90.000 ZERR 2.00 0.0003 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O P S HG UNIT 72 96 16 8 16 4 V = 2362.04 F(000) = 1352.0 Mu = 7.03 mm-1 Cell Wt = 2780.57 Rho = 1.955 MERG 2 OMIT -3.00 55.00 OMIT 0 2 1 FMAP 2 PLAN 5 SIZE 0.25 0.09 0.15 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.009600 3.494100 EXTI 0.001004 FVAR 0.22640 C1 1 0.811346 0.346316 0.523211 11.00000 0.01346 0.01837 = 0.01975 -0.00042 -0.00175 -0.00264 AFIX 23 H1A 2 0.854047 0.344322 0.457754 11.00000 -1.20000 H1B 2 0.840550 0.323088 0.604324 11.00000 -1.20000 AFIX 0 C2 1 0.780218 0.441876 0.540142 11.00000 0.02013 0.01683 = 0.03438 -0.00282 -0.00348 -0.00311 AFIX 137 H2A 2 0.756157 0.466029 0.457719 11.00000 -1.50000 H2B 2 0.829725 0.479617 0.573918 11.00000 -1.50000 H2C 2 0.734462 0.442333 0.599837 11.00000 -1.50000 AFIX 0 C3 1 0.634001 0.161681 0.403611 11.00000 0.01346 0.01329 = 0.01709 -0.00219 -0.00169 -0.00064 C4 1 0.617280 0.188339 0.276275 11.00000 0.01411 0.02273 = 0.01587 0.00134 0.00124 -0.00634 AFIX 43 H4 2 0.663872 0.210933 0.231105 11.00000 -1.20000 AFIX 0 C5 1 0.533304 0.181993 0.215754 11.00000 0.01838 0.02397 = 0.01447 0.00267 -0.00226 -0.00387 AFIX 43 H5 2 0.522335 0.200079 0.129299 11.00000 -1.20000 AFIX 0 C6 1 0.464851 0.148965 0.282098 11.00000 0.01364 0.01471 = 0.02053 -0.00390 -0.00251 -0.00109 C7 1 0.480889 0.120207 0.406773 11.00000 0.01612 0.02329 = 0.01912 0.00126 0.00282 -0.00402 AFIX 43 H7 2 0.434469 0.095973 0.450806 11.00000 -1.20000 AFIX 0 C8 1 0.565499 0.126894 0.467743 11.00000 0.01736 0.02201 = 0.01620 0.00382 0.00174 -0.00184 AFIX 43 H8 2 0.576431 0.107560 0.553665 11.00000 -1.20000 AFIX 0 C9 1 0.312286 0.110844 0.274254 11.00000 0.01365 0.02743 = 0.03810 0.00271 -0.00094 -0.00694 AFIX 137 H9A 2 0.322816 0.046418 0.292875 11.00000 -1.50000 H9B 2 0.258368 0.117465 0.217369 11.00000 -1.50000 H9C 2 0.305904 0.143638 0.353822 11.00000 -1.50000 AFIX 0 C10 1 1.030537 0.293307 0.603949 11.00000 0.01589 0.01788 = 0.04812 0.00333 -0.00708 0.00535 AFIX 23 H10A 2 0.990460 0.283437 0.671616 11.00000 -1.20000 H10B 2 1.002547 0.268173 0.523221 11.00000 -1.20000 AFIX 0 C11 1 1.047803 0.391914 0.589394 11.00000 0.02957 0.01618 = 0.02385 -0.00037 -0.00608 0.00559 AFIX 137 H11A 2 1.078245 0.415436 0.668314 11.00000 -1.50000 H11B 2 0.991913 0.424074 0.571428 11.00000 -1.50000 H11C 2 1.084629 0.401205 0.518848 11.00000 -1.50000 AFIX 0 C12 1 1.229881 0.127867 0.712187 11.00000 0.01176 0.01251 = 0.01655 0.00182 -0.00391 -0.00136 C13 1 1.297474 0.079259 0.663890 11.00000 0.01474 0.01867 = 0.01488 -0.00168 -0.00046 -0.00078 AFIX 43 H13 2 1.287893 0.050216 0.583394 11.00000 -1.20000 AFIX 0 C14 1 1.379255 0.072935 0.733033 11.00000 0.01247 0.02067 = 0.01796 -0.00172 0.00017 0.00287 AFIX 43 H14 2 1.425441 0.039657 0.699912 11.00000 -1.20000 AFIX 0 C15 1 1.392901 0.115434 0.850388 11.00000 0.01217 0.01800 = 0.01855 0.00289 -0.00479 -0.00167 C16 1 1.324277 0.162230 0.901313 11.00000 0.01871 0.01824 = 0.01774 -0.00476 -0.00294 0.00034 AFIX 43 H16 2 1.333343 0.189805 0.982886 11.00000 -1.20000 AFIX 0 C17 1 1.243593 0.168066 0.832536 11.00000 0.01602 0.01574 = 0.02071 -0.00085 -0.00027 0.00173 AFIX 43 H17 2 1.196875 0.199622 0.867044 11.00000 -1.20000 AFIX 0 C18 1 1.545390 0.075182 0.875400 11.00000 0.01388 0.03096 = 0.03246 -0.00567 -0.00577 0.00420 AFIX 137 H18A 2 1.534776 0.009945 0.864596 11.00000 -1.50000 H18B 2 1.597283 0.084819 0.935416 11.00000 -1.50000 H18C 2 1.555398 0.102249 0.792957 11.00000 -1.50000 AFIX 0 O1 3 0.734873 0.291284 0.483634 11.00000 0.01234 0.01325 = 0.01944 -0.00172 -0.00397 -0.00066 O2 3 0.385209 0.147487 0.213735 11.00000 0.01326 0.03058 = 0.02270 0.00128 -0.00268 -0.00553 O3 3 1.114320 0.248648 0.637501 11.00000 0.01164 0.01328 = 0.02862 -0.00218 -0.00451 0.00138 O4 3 1.470417 0.116894 0.923981 11.00000 0.01263 0.02965 = 0.02368 -0.00548 -0.00668 0.00358 P1 4 0.740462 0.183194 0.482737 11.00000 0.01228 0.01331 = 0.01267 -0.00070 -0.00151 0.00082 P2 4 1.124908 0.141876 0.625283 11.00000 0.00987 0.01183 = 0.01583 -0.00027 -0.00282 -0.00024 S1 5 0.838070 0.144221 0.374185 11.00000 0.01595 0.02224 = 0.01297 0.00120 0.00169 0.00493 S2 5 0.757908 0.129980 0.656314 11.00000 0.01698 0.02040 = 0.01258 0.00217 0.00151 0.00448 S3 5 0.878922 -0.109957 0.558999 11.00000 0.01748 0.01657 = 0.01393 0.00130 -0.00205 -0.00248 S4 5 1.034997 0.076303 0.723056 11.00000 0.01314 0.02329 = 0.01456 0.00268 -0.00195 -0.00384 HG1 6 0.909890 0.064740 0.561314 11.00000 0.01275 0.01915 = 0.01850 0.00016 -0.00338 0.00216 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 2005slh0408 in P2(1)/c C 0.770 H 0.320 O 0.660 P 1.100 S 1.030 HG 1.500 C1 - O1 C2 C2 - C1 C3 - C8 C4 P1 C4 - C5 C3 C5 - C4 C6 C6 - O2 C7 C5 C7 - C6 C8 C8 - C3 C7 C9 - O2 C10 - O3 C11 C11 - C10 C12 - C13 C17 P2 C13 - C12 C14 C14 - C15 C13 C15 - O4 C14 C16 C16 - C17 C15 C17 - C16 C12 C18 - O4 O1 - C1 P1 O2 - C6 C9 O3 - C10 P2 O4 - C15 C18 P1 - O1 C3 S2 S1 P2 - O3 C12 S3_$1 S4 S1 - P1 Hg1 S2 - P1 Hg1 S3 - P2_$1 Hg1 S4 - P2 Hg1 Hg1 - S4 S1 S3 S2 Operators for generating equivalent atoms: $1 -x+2, -y, -z+1 h k l Fo^2 Sigma Why rejected 0 5 0 2.52 0.62 observed but should be systematically absent 0 11 0 7.98 1.60 observed but should be systematically absent -1 0 5 11.21 2.13 observed but should be systematically absent 26739 Reflections read, of which 622 rejected -19 =< h =< 19, -17 =< k =< 19, -13 =< l =< 13, Max. 2-theta = 55.00 3 Systematic absence violations 0 Inconsistent equivalents 5402 Unique reflections, of which 0 suppressed R(int) = 0.0347 R(sigma) = 0.0289 Friedel opposites merged Maximum memory for data reduction = 2725 / 53608 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 = 3481 / 334225 wR2 = 0.0447 before cycle 1 for 5402 data and 267 / 267 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 -0.018 OSF 2 0.00100 0.00008 0.002 EXTI Mean shift/esd = 0.004 Maximum = 0.094 for U12 Hg1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C18 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0447 before cycle 2 for 5402 data and 267 / 267 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 -0.004 OSF 2 0.00100 0.00008 0.003 EXTI Mean shift/esd = 0.001 Maximum = 0.032 for U12 Hg1 Max. shift = 0.000 A for H2C Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0447 before cycle 3 for 5402 data and 267 / 267 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 0.002 OSF 2 0.00100 0.00008 0.003 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for x Hg1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0446 before cycle 4 for 5402 data and 267 / 267 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 0.001 OSF 2 0.00100 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for x Hg1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for C6 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0447 before cycle 5 for 5402 data and 267 / 267 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 0.000 OSF 2 0.00100 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for x Hg1 Max. shift = 0.000 A for H18A Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0447 before cycle 6 for 5402 data and 267 / 267 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22640 0.00020 -0.001 OSF 2 0.00100 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for x Hg1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C17 Largest correlation matrix elements 0.694 EXTI / OSF 0.636 U22 Hg1 / OSF 0.658 U11 Hg1 / OSF 0.623 U33 Hg1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.8540 0.3443 0.4578 23 0.990 0.000 C1 O1 C2 H1B 0.8406 0.3231 0.6043 23 0.990 0.000 C1 O1 C2 H2A 0.7562 0.4660 0.4577 137 0.980 0.000 C2 C1 H2A H2B 0.8297 0.4796 0.5739 137 0.980 0.000 C2 C1 H2A H2C 0.7345 0.4423 0.5998 137 0.980 0.000 C2 C1 H2A H4 0.6639 0.2109 0.2311 43 0.950 0.000 C4 C5 C3 H5 0.5223 0.2001 0.1293 43 0.950 0.000 C5 C4 C6 H7 0.4345 0.0960 0.4508 43 0.950 0.000 C7 C6 C8 H8 0.5764 0.1076 0.5537 43 0.950 0.000 C8 C3 C7 H9A 0.3228 0.0464 0.2929 137 0.980 0.000 C9 O2 H9A H9B 0.2584 0.1175 0.2174 137 0.980 0.000 C9 O2 H9A H9C 0.3059 0.1436 0.3538 137 0.980 0.000 C9 O2 H9A H10A 0.9905 0.2834 0.6716 23 0.990 0.000 C10 O3 C11 H10B 1.0025 0.2682 0.5232 23 0.990 0.000 C10 O3 C11 H11A 1.0782 0.4154 0.6683 137 0.980 0.000 C11 C10 H11A H11B 0.9919 0.4241 0.5714 137 0.980 0.000 C11 C10 H11A H11C 1.0846 0.4012 0.5188 137 0.980 0.000 C11 C10 H11A H13 1.2879 0.0502 0.5834 43 0.950 0.000 C13 C12 C14 H14 1.4254 0.0397 0.6999 43 0.950 0.000 C14 C15 C13 H16 1.3333 0.1898 0.9829 43 0.950 0.000 C16 C17 C15 H17 1.1969 0.1996 0.8670 43 0.950 0.000 C17 C16 C12 H18A 1.5348 0.0099 0.8646 137 0.980 0.000 C18 O4 H18A H18B 1.5973 0.0848 0.9354 137 0.980 0.000 C18 O4 H18A H18C 1.5554 0.1022 0.7930 137 0.980 0.000 C18 O4 H18A 2005slh0408 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.81135 0.34632 0.52321 1.00000 0.01346 0.01837 0.01975 -0.00042 -0.00175 -0.00264 0.01738 0.00439 0.00016 0.00017 0.00026 0.00000 0.00121 0.00129 0.00130 0.00103 0.00099 0.00097 0.00052 H1A 0.85405 0.34432 0.45775 1.00000 0.02086 0.00000 0.00000 H1B 0.84055 0.32309 0.60432 1.00000 0.02086 0.00000 0.00000 C2 0.78022 0.44188 0.54014 1.00000 0.02013 0.01683 0.03438 -0.00282 -0.00348 -0.00311 0.02412 0.00496 0.00019 0.00018 0.00031 0.00000 0.00142 0.00136 0.00168 0.00115 0.00122 0.00104 0.00063 H2A 0.75616 0.46603 0.45772 1.00000 0.03618 0.00000 0.00000 H2B 0.82973 0.47962 0.57392 1.00000 0.03618 0.00000 0.00000 H2C 0.73446 0.44233 0.59984 1.00000 0.03618 0.00000 0.00000 C3 0.63400 0.16168 0.40361 1.00000 0.01346 0.01329 0.01709 -0.00219 -0.00169 -0.00064 0.01479 0.00427 0.00016 0.00017 0.00024 0.00000 0.00118 0.00118 0.00124 0.00096 0.00095 0.00092 0.00050 C4 0.61728 0.18834 0.27628 1.00000 0.01411 0.02273 0.01587 0.00134 0.00124 -0.00634 0.01757 0.00446 0.00016 0.00018 0.00025 0.00000 0.00122 0.00136 0.00123 0.00106 0.00096 0.00102 0.00053 H4 0.66387 0.21093 0.23111 1.00000 0.02109 0.00000 0.00000 C5 0.53330 0.18199 0.21575 1.00000 0.01838 0.02397 0.01447 0.00267 -0.00226 -0.00387 0.01916 0.00452 0.00017 0.00018 0.00025 0.00000 0.00129 0.00140 0.00124 0.00106 0.00099 0.00105 0.00054 H5 0.52234 0.20008 0.12930 1.00000 0.02299 0.00000 0.00000 C6 0.46485 0.14896 0.28210 1.00000 0.01364 0.01471 0.02053 -0.00390 -0.00251 -0.00109 0.01653 0.00432 0.00016 0.00017 0.00025 0.00000 0.00120 0.00123 0.00133 0.00101 0.00098 0.00094 0.00052 C7 0.48089 0.12021 0.40677 1.00000 0.01612 0.02329 0.01912 0.00126 0.00282 -0.00402 0.01944 0.00468 0.00017 0.00019 0.00026 0.00000 0.00128 0.00138 0.00132 0.00108 0.00103 0.00103 0.00054 H7 0.43447 0.09597 0.45081 1.00000 0.02332 0.00000 0.00000 C8 0.56550 0.12689 0.46774 1.00000 0.01736 0.02201 0.01620 0.00382 0.00174 -0.00184 0.01851 0.00466 0.00017 0.00018 0.00025 0.00000 0.00127 0.00135 0.00126 0.00105 0.00102 0.00104 0.00053 H8 0.57643 0.10756 0.55366 1.00000 0.02221 0.00000 0.00000 C9 0.31229 0.11084 0.27425 1.00000 0.01365 0.02743 0.03810 0.00271 -0.00094 -0.00694 0.02658 0.00514 0.00017 0.00020 0.00031 0.00000 0.00131 0.00153 0.00172 0.00131 0.00118 0.00112 0.00064 H9A 0.32282 0.04642 0.29288 1.00000 0.03987 0.00000 0.00000 H9B 0.25837 0.11747 0.21737 1.00000 0.03987 0.00000 0.00000 H9C 0.30590 0.14364 0.35382 1.00000 0.03987 0.00000 0.00000 C10 1.03054 0.29331 0.60395 1.00000 0.01589 0.01788 0.04812 0.00333 -0.00708 0.00535 0.02787 0.00531 0.00018 0.00019 0.00033 0.00000 0.00134 0.00139 0.00192 0.00129 0.00125 0.00106 0.00067 H10A 0.99046 0.28344 0.67162 1.00000 0.03345 0.00000 0.00000 H10B 1.00255 0.26817 0.52322 1.00000 0.03345 0.00000 0.00000 C11 1.04780 0.39191 0.58939 1.00000 0.02957 0.01618 0.02385 -0.00037 -0.00608 0.00559 0.02369 0.00492 0.00019 0.00018 0.00028 0.00000 0.00152 0.00135 0.00145 0.00111 0.00117 0.00111 0.00060 H11A 1.07825 0.41544 0.66831 1.00000 0.03554 0.00000 0.00000 H11B 0.99191 0.42407 0.57143 1.00000 0.03554 0.00000 0.00000 H11C 1.08463 0.40121 0.51885 1.00000 0.03554 0.00000 0.00000 C12 1.22988 0.12787 0.71219 1.00000 0.01176 0.01251 0.01655 0.00182 -0.00391 -0.00136 0.01391 0.00420 0.00016 0.00016 0.00024 0.00000 0.00114 0.00115 0.00122 0.00096 0.00093 0.00091 0.00049 C13 1.29747 0.07926 0.66389 1.00000 0.01474 0.01867 0.01488 -0.00168 -0.00046 -0.00078 0.01620 0.00453 0.00017 0.00017 0.00025 0.00000 0.00124 0.00126 0.00124 0.00100 0.00098 0.00098 0.00051 H13 1.28789 0.05022 0.58339 1.00000 0.01944 0.00000 0.00000 C14 1.37925 0.07293 0.73303 1.00000 0.01247 0.02067 0.01796 -0.00172 0.00017 0.00287 0.01710 0.00457 0.00017 0.00017 0.00026 0.00000 0.00124 0.00134 0.00131 0.00102 0.00100 0.00096 0.00054 H14 1.42544 0.03966 0.69991 1.00000 0.02052 0.00000 0.00000 C15 1.39290 0.11543 0.85039 1.00000 0.01217 0.01800 0.01855 0.00289 -0.00479 -0.00167 0.01660 0.00442 0.00016 0.00017 0.00025 0.00000 0.00118 0.00128 0.00127 0.00102 0.00097 0.00096 0.00052 C16 1.32428 0.16223 0.90131 1.00000 0.01871 0.01824 0.01774 -0.00476 -0.00294 0.00034 0.01850 0.00451 0.00017 0.00018 0.00025 0.00000 0.00129 0.00129 0.00130 0.00103 0.00102 0.00101 0.00054 H16 1.33334 0.18981 0.98289 1.00000 0.02220 0.00000 0.00000 C17 1.24359 0.16807 0.83254 1.00000 0.01602 0.01574 0.02071 -0.00085 -0.00027 0.00173 0.01760 0.00452 0.00017 0.00017 0.00025 0.00000 0.00125 0.00125 0.00132 0.00103 0.00101 0.00097 0.00053 H17 1.19687 0.19962 0.86704 1.00000 0.02112 0.00000 0.00000 C18 1.54539 0.07518 0.87540 1.00000 0.01388 0.03096 0.03246 -0.00567 -0.00577 0.00420 0.02622 0.00517 0.00018 0.00020 0.00031 0.00000 0.00132 0.00160 0.00166 0.00126 0.00118 0.00111 0.00065 H18A 1.53478 0.00995 0.86460 1.00000 0.03933 0.00000 0.00000 H18B 1.59728 0.08482 0.93542 1.00000 0.03933 0.00000 0.00000 H18C 1.55540 0.10225 0.79296 1.00000 0.03933 0.00000 0.00000 O1 0.73487 0.29128 0.48363 1.00000 0.01234 0.01325 0.01944 -0.00172 -0.00397 -0.00066 0.01533 0.00292 0.00011 0.00011 0.00017 0.00000 0.00083 0.00085 0.00091 0.00070 0.00069 0.00066 0.00036 O2 0.38521 0.14749 0.21373 1.00000 0.01326 0.03058 0.02270 0.00128 -0.00268 -0.00553 0.02243 0.00324 0.00012 0.00013 0.00018 0.00000 0.00090 0.00109 0.00101 0.00083 0.00075 0.00077 0.00042 O3 1.11432 0.24865 0.63750 1.00000 0.01164 0.01328 0.02862 -0.00218 -0.00451 0.00138 0.01821 0.00306 0.00011 0.00012 0.00018 0.00000 0.00085 0.00088 0.00103 0.00076 0.00074 0.00067 0.00039 O4 1.47042 0.11689 0.92398 1.00000 0.01263 0.02965 0.02368 -0.00548 -0.00668 0.00358 0.02247 0.00322 0.00011 0.00013 0.00018 0.00000 0.00088 0.00108 0.00101 0.00083 0.00074 0.00076 0.00042 P1 0.74046 0.18319 0.48274 1.00000 0.01228 0.01331 0.01267 -0.00070 -0.00151 0.00082 0.01291 0.00109 0.00004 0.00004 0.00006 0.00000 0.00029 0.00030 0.00029 0.00024 0.00023 0.00023 0.00013 P2 1.12491 0.14188 0.62528 1.00000 0.00987 0.01184 0.01583 -0.00027 -0.00282 -0.00024 0.01274 0.00108 0.00004 0.00004 0.00006 0.00000 0.00029 0.00030 0.00031 0.00024 0.00023 0.00023 0.00013 S1 0.83807 0.14422 0.37418 1.00000 0.01595 0.02224 0.01297 0.00120 0.00169 0.00493 0.01703 0.00115 0.00004 0.00004 0.00006 0.00000 0.00031 0.00033 0.00029 0.00024 0.00023 0.00024 0.00013 S2 0.75791 0.12998 0.65631 1.00000 0.01698 0.02040 0.01258 0.00217 0.00151 0.00448 0.01664 0.00116 0.00004 0.00004 0.00006 0.00000 0.00031 0.00032 0.00029 0.00024 0.00023 0.00024 0.00013 S3 0.87892 -0.10996 0.55900 1.00000 0.01748 0.01657 0.01393 0.00130 -0.00205 -0.00248 0.01620 0.00109 0.00004 0.00004 0.00006 0.00000 0.00031 0.00031 0.00029 0.00024 0.00023 0.00024 0.00013 S4 1.03500 0.07630 0.72306 1.00000 0.01314 0.02329 0.01456 0.00268 -0.00195 -0.00384 0.01718 0.00111 0.00004 0.00004 0.00006 0.00000 0.00030 0.00033 0.00030 0.00025 0.00024 0.00024 0.00013 Hg1 0.90989 0.06474 0.56131 1.00000 0.01275 0.01915 0.01850 0.00016 -0.00338 0.00216 0.01708 0.00017 0.00001 0.00001 0.00001 0.00000 0.00007 0.00007 0.00007 0.00004 0.00004 0.00003 0.00005 Final Structure Factor Calculation for 2005slh0408 in P2(1)/c Total number of l.s. parameters = 267 Maximum vector length = 511 Memory required = 3214 / 25039 wR2 = 0.0446 before cycle 7 for 5402 data and 0 / 267 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0096 * P )^2 + 3.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0207 for 5077 Fo > 4sig(Fo) and 0.0231 for all 5402 data wR2 = 0.0446, GooF = S = 1.054, Restrained GooF = 1.054 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0216 0.0191 0.0114 C1 0.0372 0.0214 0.0138 C2 0.0195 0.0140 0.0109 C3 0.0264 0.0158 0.0106 C4 0.0276 0.0173 0.0125 C5 0.0239 0.0153 0.0104 C6 0.0252 0.0195 0.0136 C7 0.0244 0.0173 0.0138 C8 0.0402 0.0288 0.0107 C9 0.0519 0.0220 0.0097 C10 0.0375 0.0200 0.0136 C11 0.0210 0.0119 0.0089 C12 0.0193 0.0166 0.0127 C13 0.0226 0.0171 0.0116 C14 0.0247 0.0162 0.0089 C15 0.0253 0.0181 0.0120 C16 0.0219 0.0168 0.0141 C17 0.0410 0.0262 0.0114 C18 0.0230 0.0136 0.0094 O1 0.0330 0.0234 0.0108 O2 0.0317 0.0131 0.0099 O3 0.0361 0.0225 0.0089 O4 0.0158 0.0128 0.0101 P1 0.0182 0.0119 0.0082 P2 0.0250 0.0133 0.0128 S1 0.0237 0.0144 0.0119 S2 0.0216 0.0149 0.0121 S3 0.0260 0.0149 0.0107 S4 0.0220 0.0192 0.0100 Hg1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.044 0.067 0.090 0.119 0.150 0.187 0.230 0.296 1.000 Number in group 553. 530. 549. 527. 550. 543. 534. 532. 540. 544. GooF 1.092 1.070 1.074 1.099 1.066 1.040 0.951 0.981 1.019 1.149 K 1.229 1.005 0.977 0.966 0.980 0.986 1.000 1.006 1.010 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 548. 542. 539. 549. 521. 545. 542. 539. 536. 541. GooF 1.117 1.046 1.064 1.039 1.005 0.957 0.958 0.954 1.034 1.330 K 0.977 1.002 1.017 1.006 1.012 1.010 1.011 1.009 1.003 1.001 R1 0.049 0.042 0.035 0.031 0.024 0.021 0.016 0.014 0.013 0.015 Recommended weighting scheme: WGHT 0.0088 3.5455 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) -5 2 13 3347.81 4432.14 4.56 0.150 0.79 -7 2 3 8254.35 9207.80 4.07 0.216 1.86 0 1 4 693.95 483.90 3.91 0.050 2.58 -6 1 1 21988.21 23810.43 3.85 0.348 2.48 3 0 2 3464.26 2971.67 3.61 0.123 3.50 -6 12 7 126.10 273.66 3.58 0.037 0.91 18 2 1 3034.50 2472.51 3.54 0.112 0.83 -6 4 13 1209.06 1724.61 3.45 0.094 0.77 4 1 3 12554.63 13618.39 3.40 0.263 2.44 13 2 6 2447.63 2908.32 3.34 0.121 0.93 1 19 0 1023.37 1472.06 3.31 0.086 0.77 2 8 1 35.95 4.90 3.28 0.005 1.76 0 15 3 280.24 132.55 3.26 0.026 0.95 13 14 1 715.82 1160.66 3.21 0.077 0.78 4 6 11 11893.97 10519.98 3.21 0.231 0.85 -18 4 1 9777.16 8351.29 3.18 0.206 0.83 -13 5 7 599.17 907.12 3.16 0.068 0.92 0 12 0 174.77 89.74 3.14 0.021 1.23 -1 2 3 828.17 640.67 3.12 0.057 3.14 -7 3 12 2951.27 3459.95 3.08 0.133 0.83 -17 5 4 13766.76 11737.96 3.05 0.244 0.83 7 1 2 954.99 767.72 3.02 0.062 1.93 13 10 6 379.93 599.37 3.00 0.055 0.79 1 2 5 36928.94 33750.88 2.98 0.414 1.98 0 2 7 2662.83 2292.24 2.97 0.108 1.47 -6 4 2 1849.79 1591.19 2.96 0.090 1.99 -1 3 7 2369.35 2014.01 2.95 0.101 1.44 3 2 0 59.38 20.69 2.93 0.010 4.18 9 8 0 222.22 131.88 2.91 0.026 1.25 1 5 11 7140.40 6376.16 2.90 0.180 0.90 9 4 8 108.57 0.15 2.90 0.001 0.96 -4 14 8 -74.33 78.66 2.90 0.020 0.81 -12 3 3 93.29 25.08 2.90 0.011 1.19 -8 8 11 1012.91 1470.71 2.89 0.086 0.80 0 13 6 7698.33 6948.59 2.88 0.188 0.95 -5 2 2 10244.01 11019.36 2.87 0.236 2.57 -7 15 2 2006.20 2388.18 2.86 0.110 0.89 11 14 1 780.57 1008.91 2.83 0.072 0.83 1 4 0 408.81 304.93 2.82 0.039 3.58 -4 18 2 1634.05 2150.10 2.80 0.104 0.79 -1 2 2 602.14 468.56 2.80 0.049 4.19 -2 8 7 143.67 50.33 2.79 0.016 1.16 3 7 11 21652.33 19569.64 2.78 0.315 0.85 3 4 4 8966.82 9673.31 2.78 0.222 1.92 7 5 2 50.96 7.29 2.76 0.006 1.63 -8 16 5 -99.51 336.21 2.75 0.041 0.78 7 0 2 39811.82 42472.96 2.75 0.464 1.95 7 14 1 297.75 416.21 2.73 0.046 0.94 17 5 5 369.75 556.98 2.72 0.053 0.77 6 2 5 1095.37 911.04 2.72 0.068 1.52 Bond lengths and angles C1 - Distance Angles O1 1.4526 (0.0029) C2 1.5020 (0.0036) 107.63 (0.20) H1A 0.9900 110.18 110.18 H1B 0.9900 110.18 110.18 108.48 C1 - O1 C2 H1A C2 - Distance Angles C1 1.5020 (0.0036) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C8 1.3916 (0.0037) C4 1.4001 (0.0036) 119.14 (0.23) P1 1.7892 (0.0024) 121.98 (0.20) 118.63 (0.19) C3 - C8 C4 C4 - Distance Angles C5 1.3844 (0.0035) C3 1.4001 (0.0036) 120.44 (0.24) H4 0.9500 119.78 119.78 C4 - C5 C3 C5 - Distance Angles C4 1.3844 (0.0035) C6 1.3948 (0.0037) 119.80 (0.24) H5 0.9500 120.10 120.10 C5 - C4 C6 C6 - Distance Angles O2 1.3583 (0.0030) C7 1.3819 (0.0037) 125.13 (0.24) C5 1.3948 (0.0038) 114.52 (0.23) 120.35 (0.23) C6 - O2 C7 C7 - Distance Angles C6 1.3819 (0.0037) C8 1.3951 (0.0035) 119.76 (0.24) H7 0.9500 120.12 120.12 C7 - C6 C8 C8 - Distance Angles C3 1.3916 (0.0037) C7 1.3951 (0.0035) 120.48 (0.25) H8 0.9500 119.76 119.76 C8 - C3 C7 C9 - Distance Angles O2 1.4359 (0.0033) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - O2 H9A H9B C10 - Distance Angles O3 1.4545 (0.0030) C11 1.4873 (0.0038) 107.89 (0.22) H10A 0.9900 110.13 110.13 H10B 0.9900 110.13 110.13 108.44 C10 - O3 C11 H10A C11 - Distance Angles C10 1.4873 (0.0038) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C13 1.3888 (0.0036) C17 1.3989 (0.0036) 119.57 (0.22) P2 1.7871 (0.0024) 122.25 (0.19) 118.18 (0.19) C12 - C13 C17 C13 - Distance Angles C12 1.3888 (0.0036) C14 1.3927 (0.0036) 120.24 (0.24) H13 0.9500 119.88 119.88 C13 - C12 C14 C14 - Distance Angles C15 1.3857 (0.0037) C13 1.3927 (0.0036) 119.65 (0.24) H14 0.9500 120.17 120.17 C14 - C15 C13 C15 - Distance Angles O4 1.3573 (0.0029) C14 1.3857 (0.0037) 124.95 (0.24) C16 1.3998 (0.0037) 114.68 (0.23) 120.37 (0.23) C15 - O4 C14 C16 - Distance Angles C17 1.3763 (0.0035) C15 1.3998 (0.0038) 119.63 (0.24) H16 0.9500 120.19 120.19 C16 - C17 C15 C17 - Distance Angles C16 1.3763 (0.0035) C12 1.3989 (0.0036) 120.48 (0.24) H17 0.9500 119.76 119.76 C17 - C16 C12 C18 - Distance Angles O4 1.4326 (0.0034) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - O4 H18A H18B O1 - Distance Angles C1 1.4526 (0.0029) P1 1.5954 (0.0018) 121.14 (0.15) O1 - C1 O2 - Distance Angles C6 1.3583 (0.0030) C9 1.4359 (0.0033) 117.60 (0.22) O2 - C6 O3 - Distance Angles C10 1.4545 (0.0030) P2 1.5883 (0.0018) 121.48 (0.16) O3 - C10 O4 - Distance Angles C15 1.3573 (0.0029) C18 1.4326 (0.0034) 118.23 (0.22) O4 - C15 P1 - Distance Angles O1 1.5954 (0.0018) C3 1.7892 (0.0025) 97.63 (0.10) S2 1.9866 (0.0009) 113.06 (0.07) 113.74 (0.09) S1 2.0388 (0.0009) 109.07 (0.07) 111.55 (0.09) 111.07 (0.04) P1 - O1 C3 S2 P2 - Distance Angles O3 1.5883 (0.0018) C12 1.7871 (0.0024) 99.55 (0.10) S3_$1 1.9940 (0.0009) 108.55 (0.08) 114.87 (0.09) S4 2.0314 (0.0009) 110.62 (0.08) 107.49 (0.09) 114.71 (0.04) P2 - O3 C12 S3_$1 S1 - Distance Angles P1 2.0388 (0.0009) Hg1 2.4669 (0.0006) 88.91 (0.03) S1 - P1 S2 - Distance Angles P1 1.9866 (0.0009) Hg1 2.7777 (0.0006) 81.60 (0.03) S2 - P1 S3 - Distance Angles P2_$1 1.9940 (0.0009) Hg1 2.6174 (0.0006) 103.36 (0.03) S3 - P2_$1 S4 - Distance Angles P2 2.0314 (0.0009) Hg1 2.4524 (0.0006) 101.56 (0.03) S4 - P2 Hg1 - Distance Angles S4 2.4524 (0.0006) S1 2.4669 (0.0006) 141.95 (0.02) S3 2.6174 (0.0006) 101.77 (0.02) 113.10 (0.02) S2 2.7777 (0.0006) 110.48 (0.02) 78.27 (0.02) 100.83 (0.02) Hg1 - S4 S1 S3 FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0221 for 5402 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.93 at 0.9779 0.0647 0.5557 [ 1.04 A from HG1 ] Deepest hole -1.34 at 0.9375 0.0640 0.4984 [ 0.82 A from HG1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 3283 / 24774 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9779 0.0647 0.5557 1.00000 0.05 0.93 1.04 HG1 1.91 S4 2.57 P2 2.67 S3 Q2 1 0.9084 -0.1912 0.5606 1.00000 0.05 0.88 1.28 S3 2.03 H10B 2.11 P2 2.25 O3 Q3 1 0.8535 0.0531 0.5747 1.00000 0.05 0.88 0.90 HG1 2.09 S2 2.44 S3 2.50 S1 Q4 1 0.2719 0.0646 0.3221 1.00000 0.05 0.84 0.90 H9A 1.07 C9 1.31 H9C 1.35 H9B Q5 1 0.9392 -0.1226 0.5469 1.00000 0.05 0.62 0.96 S3 2.01 P2 2.46 H10B 2.76 O3 Shortest distances between peaks (including symmetry equivalents) 2 5 1.13 1 5 1.93 1 3 1.93 1 1 2.37 1 5 2.82 3 4 2.87 1 2 2.89 3 5 2.93 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 0.01: 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. 2.18: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.68: Structure factors and derivatives 7.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0408 finished at 12:52:19 Total CPU time: 15.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++