+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0770 started at 19:27:03 on 05-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0770 in P2(1)/n CELL 0.71073 11.4631 12.2418 17.1604 90.000 95.555 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N CL RH UNIT 108 136 8 4 4 V = 2396.79 F(000) = 1088.0 Mu = 0.84 mm-1 Cell Wt = 2099.69 Rho = 1.455 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.03 0.20 0.40 ACTA BOND WGHT 0.04960 9.00900 L.S. 4 TEMP -153.00 FVAR 0.36385 C1 1 1.092816 0.249868 0.220029 11.00000 0.01441 0.01111 = 0.01520 0.00046 0.00124 -0.00129 C2 1 1.052777 0.242384 0.354481 11.00000 0.01663 0.02422 = 0.01327 0.00013 0.00009 0.00271 C3 1 1.015973 0.339733 0.385348 11.00000 0.02406 0.02854 = 0.02170 -0.00315 0.00129 0.00270 AFIX 43 H3 2 1.044723 0.407442 0.368069 11.00000 -1.20000 AFIX 0 C4 1 0.936882 0.337646 0.441635 11.00000 0.02835 0.04096 = 0.02492 -0.00921 0.00631 0.00982 AFIX 43 H4 2 0.911050 0.404193 0.462681 11.00000 -1.20000 AFIX 0 C5 1 0.895652 0.239580 0.467139 11.00000 0.02087 0.05417 = 0.01975 0.00061 0.00670 0.00464 AFIX 43 H5 2 0.840262 0.238403 0.504884 11.00000 -1.20000 AFIX 0 C6 1 0.935352 0.142648 0.437479 11.00000 0.02374 0.03878 = 0.02239 0.00541 0.00304 -0.00256 AFIX 43 H6 2 0.907423 0.075181 0.455760 11.00000 -1.20000 AFIX 0 C7 1 1.015726 0.142157 0.381162 11.00000 0.02071 0.02668 = 0.01691 0.00129 0.00049 0.00005 C8 1 1.059348 0.035672 0.351471 11.00000 0.03469 0.02219 = 0.03561 0.00381 0.00775 0.00174 AFIX 33 H8A 2 1.114639 0.050070 0.312567 11.00000 -1.50000 H8B 2 0.992961 -0.006759 0.327254 11.00000 -1.50000 H8C 2 1.098890 -0.005738 0.395229 11.00000 -1.50000 AFIX 0 C9 1 1.259761 0.262950 0.330150 11.00000 0.01862 0.03082 = 0.01666 -0.00119 -0.00195 -0.00174 AFIX 23 H9A 2 1.298295 0.191545 0.341421 11.00000 -1.20000 H9B 2 1.258807 0.302641 0.380349 11.00000 -1.20000 AFIX 0 C10 1 1.331287 0.328230 0.275900 11.00000 0.01560 0.02191 = 0.02394 -0.00474 0.00159 -0.00367 AFIX 23 H10A 2 1.399967 0.360719 0.306912 11.00000 -1.20000 H10B 2 1.282709 0.388686 0.252140 11.00000 -1.20000 AFIX 0 C11 1 1.373485 0.257374 0.210910 11.00000 0.01645 0.02370 = 0.02380 -0.00032 0.00288 -0.00077 AFIX 23 H11A 2 1.388670 0.303969 0.165833 11.00000 -1.20000 H11B 2 1.447761 0.220829 0.230201 11.00000 -1.20000 AFIX 0 C12 1 1.282129 0.172196 0.184892 11.00000 0.01365 0.02180 = 0.02079 -0.00261 0.00076 0.00371 AFIX 23 H12A 2 1.306041 0.133713 0.138253 11.00000 -1.20000 H12B 2 1.278129 0.117642 0.227137 11.00000 -1.20000 AFIX 0 C13 1 1.130814 0.239291 0.083618 11.00000 0.01187 0.02264 = 0.01423 0.00159 0.00194 0.00001 C14 1 1.121982 0.150879 0.031468 11.00000 0.01303 0.02067 = 0.01810 0.00053 0.00310 -0.00173 C15 1 1.142951 0.033930 0.057151 11.00000 0.02640 0.02092 = 0.02326 -0.00151 0.00050 -0.00117 AFIX 33 H15A 2 1.164280 0.031704 0.113827 11.00000 -1.50000 H15B 2 1.206792 0.002977 0.030100 11.00000 -1.50000 H15C 2 1.071386 -0.008773 0.044191 11.00000 -1.50000 AFIX 0 C16 1 1.090613 0.173153 -0.047500 11.00000 0.01944 0.02760 = 0.01684 -0.00272 0.00346 -0.00311 AFIX 43 H16 2 1.085064 0.114479 -0.083902 11.00000 -1.20000 AFIX 0 C17 1 1.067353 0.278198 -0.074333 11.00000 0.02103 0.03155 = 0.01619 0.00484 0.00454 0.00080 AFIX 43 H17 2 1.045382 0.290972 -0.128368 11.00000 -1.20000 AFIX 0 C18 1 1.076237 0.364601 -0.022102 11.00000 0.02393 0.02434 = 0.02152 0.00685 0.00641 0.00435 AFIX 43 H18 2 1.059565 0.436838 -0.040101 11.00000 -1.20000 AFIX 0 C19 1 1.109691 0.345428 0.056955 11.00000 0.01832 0.02053 = 0.01988 0.00151 0.00486 0.00126 AFIX 43 H19 2 1.118074 0.404866 0.092650 11.00000 -1.20000 AFIX 0 C20 1 0.832628 0.175586 0.208611 11.00000 0.01609 0.01517 = 0.02252 -0.00152 0.00186 -0.00316 AFIX 43 H20 2 0.892096 0.154870 0.248277 11.00000 -1.20000 AFIX 0 C21 1 0.862676 0.181803 0.131084 11.00000 0.01552 0.02098 = 0.02229 -0.00647 0.00118 -0.00302 AFIX 43 H21 2 0.940097 0.160991 0.122134 11.00000 -1.20000 AFIX 0 C22 1 0.782522 0.218706 0.060795 11.00000 0.02659 0.04372 = 0.02082 -0.00736 -0.00422 -0.00381 AFIX 23 H22A 2 0.729120 0.157932 0.043629 11.00000 -1.20000 H22B 2 0.830536 0.235423 0.017348 11.00000 -1.20000 AFIX 0 C23 1 0.709437 0.318929 0.076651 11.00000 0.02229 0.04824 = 0.02585 0.00366 -0.00758 0.00169 AFIX 23 H23A 2 0.687411 0.357455 0.026663 11.00000 -1.20000 H23B 2 0.636345 0.295021 0.097921 11.00000 -1.20000 AFIX 0 C24 1 0.774115 0.397402 0.133855 11.00000 0.01426 0.02591 = 0.03125 0.00789 -0.00056 0.00307 AFIX 43 H24 2 0.823869 0.449959 0.113307 11.00000 -1.20000 AFIX 0 C25 1 0.766173 0.398235 0.213366 11.00000 0.01497 0.01684 = 0.03009 0.00119 0.00352 0.00328 AFIX 43 H25 2 0.807305 0.454480 0.242615 11.00000 -1.20000 AFIX 0 C26 1 0.698449 0.318435 0.258503 11.00000 0.01781 0.02180 = 0.02927 -0.00239 0.00888 -0.00069 AFIX 23 H26A 2 0.614416 0.338519 0.251829 11.00000 -1.20000 H26B 2 0.725593 0.324666 0.314873 11.00000 -1.20000 AFIX 0 C27 1 0.711398 0.199823 0.232976 11.00000 0.02097 0.02093 = 0.03442 -0.00076 0.01146 -0.00389 AFIX 23 H27A 2 0.695848 0.150924 0.276742 11.00000 -1.20000 H27B 2 0.652158 0.184083 0.188514 11.00000 -1.20000 AFIX 0 N1 3 1.136698 0.243961 0.296290 11.00000 0.01440 0.02226 = 0.01378 -0.00121 0.00156 0.00166 N2 3 1.164711 0.220724 0.165701 11.00000 0.01248 0.02021 = 0.01460 0.00009 0.00094 0.00182 CL1 4 1.030568 0.495086 0.214719 11.00000 0.00837 0.00605 = 0.01780 0.00003 0.00065 -0.00163 RH1 5 0.932652 0.318448 0.193664 11.00000 0.01097 0.01334 = 0.01480 0.00014 0.00081 -0.00015 HKLF 4 Covalent radii and connectivity table for 2008src0770 in P2(1)/n C 0.770 H 0.320 N 0.700 CL 0.990 RH 1.350 C1 - N2 N1 Rh1 C2 - C3 C7 N1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C7 C7 - C2 C6 C8 C8 - C7 C9 - N1 C10 C10 - C9 C11 C11 - C12 C10 C12 - N2 C11 C13 - C19 C14 N2 C14 - C16 C13 C15 C15 - C14 C16 - C17 C14 C17 - C16 C18 C18 - C17 C19 C19 - C13 C18 C20 - C21 C27 Rh1 C21 - C20 C22 Rh1 C22 - C21 C23 C23 - C24 C22 C24 - C25 C23 Rh1 C25 - C24 C26 Rh1 C26 - C25 C27 C27 - C20 C26 N1 - C1 C2 C9 N2 - C1 C13 C12 Cl1 - Rh1 Rh1 - C1 C21 C20 C25 C24 Cl1 h k l Fo^2 Sigma Why rejected 0 0 13 5.36 1.11 observed but should be systematically absent 30281 Reflections read, of which 800 rejected -14 =< h =< 14, -15 =< k =< 15, -22 =< l =< 22, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 5483 Unique reflections, of which 0 suppressed R(int) = 0.0360 R(sigma) = 0.0269 Friedel opposites merged Maximum memory for data reduction = 2966 / 54145 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 = 3822 / 350077 wR2 = 0.1103 before cycle 1 for 5483 data and 280 / 280 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0496 * P )^2 + 9.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36385 0.00059 -0.004 OSF Mean shift/esd = 0.003 Maximum = 0.034 for U12 Rh1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3822 / 350077 wR2 = 0.1103 before cycle 2 for 5483 data and 280 / 280 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0496 * P )^2 + 9.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36385 0.00059 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.013 for U12 Rh1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3822 / 350077 wR2 = 0.1103 before cycle 3 for 5483 data and 280 / 280 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0496 * P )^2 + 9.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36385 0.00059 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for C25 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3822 / 350077 wR2 = 0.1103 before cycle 4 for 5483 data and 280 / 280 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0496 * P )^2 + 9.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36385 0.00059 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C8 Largest correlation matrix elements 0.584 U11 Rh1 / OSF 0.578 U33 Rh1 / OSF 0.562 U22 Rh1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 1.0447 0.4074 0.3681 43 0.950 0.000 C3 C2 C4 H4 0.9110 0.4042 0.4627 43 0.950 0.000 C4 C5 C3 H5 0.8403 0.2384 0.5049 43 0.950 0.000 C5 C4 C6 H6 0.9074 0.0752 0.4558 43 0.950 0.000 C6 C5 C7 H8A 1.1146 0.0501 0.3126 33 0.980 0.000 C8 C7 H8A H8B 0.9930 -0.0068 0.3273 33 0.980 0.000 C8 C7 H8A H8C 1.0989 -0.0057 0.3952 33 0.980 0.000 C8 C7 H8A H9A 1.2983 0.1915 0.3414 23 0.990 0.000 C9 N1 C10 H9B 1.2588 0.3026 0.3803 23 0.990 0.000 C9 N1 C10 H10A 1.4000 0.3607 0.3069 23 0.990 0.000 C10 C9 C11 H10B 1.2827 0.3887 0.2521 23 0.990 0.000 C10 C9 C11 H11A 1.3887 0.3040 0.1658 23 0.990 0.000 C11 C12 C10 H11B 1.4478 0.2208 0.2302 23 0.990 0.000 C11 C12 C10 H12A 1.3060 0.1337 0.1383 23 0.990 0.000 C12 N2 C11 H12B 1.2781 0.1176 0.2271 23 0.990 0.000 C12 N2 C11 H15A 1.1643 0.0317 0.1138 33 0.980 0.000 C15 C14 H15A H15B 1.2068 0.0030 0.0301 33 0.980 0.000 C15 C14 H15A H15C 1.0714 -0.0088 0.0442 33 0.980 0.000 C15 C14 H15A H16 1.0851 0.1145 -0.0839 43 0.950 0.000 C16 C17 C14 H17 1.0454 0.2910 -0.1284 43 0.950 0.000 C17 C16 C18 H18 1.0596 0.4368 -0.0401 43 0.950 0.000 C18 C17 C19 H19 1.1181 0.4049 0.0926 43 0.950 0.000 C19 C13 C18 ** Bond(s) to Rh1 ignored in idealizing H-atoms attached to C20 ** H20 0.8921 0.1549 0.2483 43 0.950 0.000 C20 C21 C27 ** Bond(s) to Rh1 ignored in idealizing H-atoms attached to C21 ** H21 0.9401 0.1610 0.1221 43 0.950 0.000 C21 C20 C22 H22A 0.7291 0.1579 0.0436 23 0.990 0.000 C22 C21 C23 H22B 0.8305 0.2354 0.0173 23 0.990 0.000 C22 C21 C23 H23A 0.6874 0.3575 0.0267 23 0.990 0.000 C23 C24 C22 H23B 0.6363 0.2950 0.0979 23 0.990 0.000 C23 C24 C22 ** Bond(s) to Rh1 ignored in idealizing H-atoms attached to C24 ** H24 0.8239 0.4500 0.1133 43 0.950 0.000 C24 C25 C23 ** Bond(s) to Rh1 ignored in idealizing H-atoms attached to C25 ** H25 0.8073 0.4545 0.2426 43 0.950 0.000 C25 C24 C26 H26A 0.6144 0.3385 0.2518 23 0.990 0.000 C26 C25 C27 H26B 0.7256 0.3247 0.3149 23 0.990 0.000 C26 C25 C27 H27A 0.6958 0.1509 0.2767 23 0.990 0.000 C27 C20 C26 H27B 0.6522 0.1841 0.1885 23 0.990 0.000 C27 C20 C26 2008src0770 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.09282 0.24987 0.22003 1.00000 0.01441 0.01111 0.01520 0.00046 0.00124 -0.00129 0.01358 0.00516 0.00026 0.00023 0.00017 0.00000 0.00135 0.00131 0.00133 0.00102 0.00105 0.00102 0.00054 C2 1.05278 0.24238 0.35448 1.00000 0.01662 0.02422 0.01327 0.00013 0.00009 0.00271 0.01813 0.00568 0.00027 0.00027 0.00018 0.00000 0.00145 0.00163 0.00133 0.00114 0.00111 0.00119 0.00061 C3 1.01597 0.33973 0.38535 1.00000 0.02406 0.02855 0.02171 -0.00315 0.00129 0.00271 0.02483 0.00639 0.00031 0.00031 0.00020 0.00000 0.00169 0.00178 0.00160 0.00134 0.00130 0.00137 0.00070 H3 1.04473 0.40744 0.36807 1.00000 0.02980 0.00000 0.00000 C4 0.93688 0.33764 0.44163 1.00000 0.02834 0.04097 0.02491 -0.00921 0.00631 0.00982 0.03116 0.00724 0.00034 0.00035 0.00022 0.00000 0.00188 0.00218 0.00174 0.00156 0.00144 0.00161 0.00082 H4 0.91105 0.40419 0.46268 1.00000 0.03740 0.00000 0.00000 C5 0.89565 0.23958 0.46714 1.00000 0.02086 0.05416 0.01975 0.00060 0.00669 0.00464 0.03128 0.00724 0.00032 0.00037 0.00021 0.00000 0.00169 0.00254 0.00159 0.00158 0.00130 0.00162 0.00084 H5 0.84026 0.23841 0.50488 1.00000 0.03754 0.00000 0.00000 C6 0.93535 0.14265 0.43748 1.00000 0.02374 0.03878 0.02238 0.00540 0.00305 -0.00255 0.02825 0.00685 0.00032 0.00034 0.00021 0.00000 0.00172 0.00210 0.00163 0.00148 0.00132 0.00152 0.00075 H6 0.90743 0.07518 0.45576 1.00000 0.03390 0.00000 0.00000 C7 1.01572 0.14216 0.38116 1.00000 0.02071 0.02669 0.01690 0.00129 0.00050 0.00005 0.02152 0.00600 0.00029 0.00029 0.00019 0.00000 0.00156 0.00173 0.00143 0.00126 0.00117 0.00130 0.00065 C8 1.05935 0.03567 0.35147 1.00000 0.03470 0.02219 0.03562 0.00381 0.00776 0.00174 0.03055 0.00734 0.00035 0.00031 0.00023 0.00000 0.00199 0.00175 0.00197 0.00148 0.00157 0.00148 0.00079 H8A 1.11464 0.05007 0.31257 1.00000 0.04582 0.00000 0.00000 H8B 0.99296 -0.00676 0.32726 1.00000 0.04582 0.00000 0.00000 H8C 1.09889 -0.00574 0.39523 1.00000 0.04582 0.00000 0.00000 C9 1.25976 0.26295 0.33015 1.00000 0.01863 0.03082 0.01666 -0.00119 -0.00195 -0.00175 0.02228 0.00584 0.00028 0.00030 0.00019 0.00000 0.00155 0.00182 0.00144 0.00127 0.00118 0.00130 0.00067 H9A 1.29829 0.19154 0.34142 1.00000 0.02673 0.00000 0.00000 H9B 1.25881 0.30264 0.38035 1.00000 0.02673 0.00000 0.00000 C10 1.33129 0.32823 0.27590 1.00000 0.01561 0.02191 0.02394 -0.00474 0.00159 -0.00367 0.02051 0.00572 0.00029 0.00027 0.00020 0.00000 0.00148 0.00161 0.00159 0.00123 0.00121 0.00117 0.00065 H10A 1.39996 0.36072 0.30691 1.00000 0.02461 0.00000 0.00000 H10B 1.28271 0.38869 0.25214 1.00000 0.02461 0.00000 0.00000 C11 1.37349 0.25737 0.21091 1.00000 0.01646 0.02371 0.02380 -0.00031 0.00288 -0.00077 0.02126 0.00593 0.00028 0.00028 0.00020 0.00000 0.00149 0.00166 0.00157 0.00126 0.00120 0.00122 0.00065 H11A 1.38867 0.30397 0.16583 1.00000 0.02551 0.00000 0.00000 H11B 1.44776 0.22083 0.23020 1.00000 0.02551 0.00000 0.00000 C12 1.28213 0.17220 0.18489 1.00000 0.01365 0.02179 0.02079 -0.00261 0.00076 0.00371 0.01880 0.00572 0.00027 0.00026 0.00019 0.00000 0.00145 0.00157 0.00151 0.00119 0.00116 0.00115 0.00062 H12A 1.30604 0.13371 0.13825 1.00000 0.02256 0.00000 0.00000 H12B 1.27813 0.11764 0.22714 1.00000 0.02256 0.00000 0.00000 C13 1.13082 0.23929 0.08362 1.00000 0.01188 0.02265 0.01424 0.00159 0.00194 0.00001 0.01621 0.00550 0.00026 0.00027 0.00017 0.00000 0.00134 0.00157 0.00133 0.00113 0.00105 0.00111 0.00058 C14 1.12198 0.15088 0.03147 1.00000 0.01303 0.02067 0.01811 0.00053 0.00310 -0.00173 0.01717 0.00559 0.00026 0.00027 0.00018 0.00000 0.00136 0.00152 0.00143 0.00118 0.00109 0.00114 0.00059 C15 1.14295 0.03393 0.05715 1.00000 0.02639 0.02092 0.02327 -0.00151 0.00050 -0.00116 0.02365 0.00608 0.00031 0.00028 0.00020 0.00000 0.00171 0.00164 0.00158 0.00127 0.00129 0.00131 0.00068 H15A 1.16428 0.03170 0.11383 1.00000 0.03547 0.00000 0.00000 H15B 1.20679 0.00298 0.03010 1.00000 0.03547 0.00000 0.00000 H15C 1.07139 -0.00877 0.04419 1.00000 0.03547 0.00000 0.00000 C16 1.09061 0.17315 -0.04750 1.00000 0.01944 0.02760 0.01685 -0.00273 0.00346 -0.00312 0.02119 0.00596 0.00029 0.00029 0.00019 0.00000 0.00157 0.00175 0.00148 0.00122 0.00119 0.00125 0.00066 H16 1.08507 0.11448 -0.08390 1.00000 0.02542 0.00000 0.00000 C17 1.06735 0.27820 -0.07433 1.00000 0.02103 0.03155 0.01619 0.00483 0.00454 0.00081 0.02274 0.00637 0.00029 0.00030 0.00019 0.00000 0.00159 0.00183 0.00143 0.00132 0.00119 0.00135 0.00067 H17 1.04538 0.29097 -0.12837 1.00000 0.02729 0.00000 0.00000 C18 1.07624 0.36460 -0.02210 1.00000 0.02394 0.02435 0.02152 0.00685 0.00641 0.00435 0.02300 0.00653 0.00030 0.00029 0.00019 0.00000 0.00163 0.00170 0.00156 0.00130 0.00125 0.00132 0.00067 H18 1.05957 0.43684 -0.04010 1.00000 0.02760 0.00000 0.00000 C19 1.10969 0.34543 0.05695 1.00000 0.01833 0.02053 0.01988 0.00151 0.00487 0.00126 0.01939 0.00605 0.00028 0.00028 0.00019 0.00000 0.00148 0.00153 0.00148 0.00121 0.00117 0.00121 0.00061 H19 1.11807 0.40487 0.09265 1.00000 0.02326 0.00000 0.00000 C20 0.83263 0.17559 0.20861 1.00000 0.01610 0.01518 0.02251 -0.00152 0.00185 -0.00316 0.01793 0.00558 0.00028 0.00025 0.00019 0.00000 0.00146 0.00145 0.00154 0.00114 0.00118 0.00110 0.00061 H20 0.89210 0.15488 0.24828 1.00000 0.02151 0.00000 0.00000 C21 0.86268 0.18181 0.13108 1.00000 0.01552 0.02098 0.02228 -0.00646 0.00118 -0.00302 0.01963 0.00556 0.00029 0.00026 0.00020 0.00000 0.00147 0.00161 0.00157 0.00118 0.00120 0.00114 0.00064 H21 0.94010 0.16100 0.12213 1.00000 0.02356 0.00000 0.00000 C22 0.78252 0.21870 0.06079 1.00000 0.02661 0.04371 0.02081 -0.00736 -0.00423 -0.00381 0.03080 0.00654 0.00033 0.00036 0.00021 0.00000 0.00182 0.00224 0.00165 0.00156 0.00136 0.00164 0.00081 H22A 0.72912 0.15793 0.04363 1.00000 0.03696 0.00000 0.00000 H22B 0.83053 0.23542 0.01735 1.00000 0.03696 0.00000 0.00000 C23 0.70944 0.31893 0.07665 1.00000 0.02228 0.04822 0.02585 0.00366 -0.00758 0.00169 0.03276 0.00702 0.00034 0.00035 0.00023 0.00000 0.00180 0.00248 0.00182 0.00158 0.00143 0.00155 0.00088 H23A 0.68741 0.35745 0.02666 1.00000 0.03932 0.00000 0.00000 H23B 0.63635 0.29502 0.09792 1.00000 0.03932 0.00000 0.00000 C24 0.77412 0.39740 0.13386 1.00000 0.01426 0.02592 0.03124 0.00790 -0.00056 0.00308 0.02399 0.00644 0.00028 0.00030 0.00021 0.00000 0.00147 0.00173 0.00175 0.00139 0.00125 0.00125 0.00069 H24 0.82387 0.44996 0.11331 1.00000 0.02879 0.00000 0.00000 C25 0.76617 0.39823 0.21337 1.00000 0.01498 0.01685 0.03009 0.00118 0.00352 0.00328 0.02055 0.00614 0.00028 0.00027 0.00020 0.00000 0.00144 0.00151 0.00169 0.00125 0.00122 0.00115 0.00064 H25 0.80730 0.45448 0.24262 1.00000 0.02466 0.00000 0.00000 C26 0.69845 0.31844 0.25850 1.00000 0.01782 0.02179 0.02925 -0.00240 0.00887 -0.00068 0.02252 0.00637 0.00030 0.00027 0.00022 0.00000 0.00156 0.00170 0.00174 0.00127 0.00130 0.00119 0.00068 H26A 0.61442 0.33852 0.25183 1.00000 0.02703 0.00000 0.00000 H26B 0.72560 0.32467 0.31487 1.00000 0.02703 0.00000 0.00000 C27 0.71140 0.19982 0.23297 1.00000 0.02098 0.02093 0.03441 -0.00076 0.01146 -0.00388 0.02487 0.00667 0.00031 0.00029 0.00023 0.00000 0.00165 0.00166 0.00188 0.00138 0.00139 0.00129 0.00071 H27A 0.69585 0.15092 0.27674 1.00000 0.02984 0.00000 0.00000 H27B 0.65216 0.18408 0.18851 1.00000 0.02984 0.00000 0.00000 N1 1.13670 0.24396 0.29629 1.00000 0.01441 0.02227 0.01378 -0.00121 0.00156 0.00167 0.01681 0.00471 0.00023 0.00022 0.00015 0.00000 0.00121 0.00137 0.00118 0.00098 0.00095 0.00099 0.00052 N2 1.16471 0.22072 0.16570 1.00000 0.01247 0.02022 0.01460 0.00010 0.00095 0.00182 0.01579 0.00469 0.00022 0.00023 0.00015 0.00000 0.00118 0.00132 0.00117 0.00099 0.00092 0.00098 0.00050 Cl1 1.03057 0.49509 0.21472 1.00000 0.00837 0.00606 0.01781 0.00003 0.00065 -0.00163 0.01078 0.00112 0.00005 0.00005 0.00004 0.00000 0.00028 0.00028 0.00031 0.00022 0.00023 0.00021 0.00014 Rh1 0.93265 0.31845 0.19366 1.00000 0.01097 0.01334 0.01480 0.00014 0.00081 -0.00015 0.01306 0.00040 0.00002 0.00002 0.00001 0.00000 0.00013 0.00014 0.00013 0.00008 0.00009 0.00008 0.00009 Final Structure Factor Calculation for 2008src0770 in P2(1)/n Total number of l.s. parameters = 280 Maximum vector length = 511 Memory required = 3542 / 24017 wR2 = 0.1103 before cycle 5 for 5483 data and 0 / 280 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0496 * P )^2 + 9.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0387 for 5100 Fo > 4sig(Fo) and 0.0421 for all 5483 data wR2 = 0.1103, GooF = S = 1.056, Restrained GooF = 1.056 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0155 0.0147 0.0106 C1 0.0251 0.0164 0.0128 C2 0.0312 0.0229 0.0204 C3 0.0487 0.0301 0.0147 C4 0.0548 0.0242 0.0148 C5 0.0408 0.0240 0.0199 C6 0.0269 0.0212 0.0165 C7 0.0400 0.0305 0.0212 C8 0.0311 0.0218 0.0140 C9 0.0280 0.0200 0.0136 C10 0.0242 0.0234 0.0162 C11 0.0253 0.0189 0.0122 C12 0.0229 0.0141 0.0116 C13 0.0211 0.0184 0.0120 C14 0.0275 0.0237 0.0198 C15 0.0293 0.0186 0.0157 C16 0.0331 0.0215 0.0137 C17 0.0331 0.0202 0.0157 C18 0.0233 0.0192 0.0157 C19 0.0228 0.0186 0.0124 C20 0.0282 0.0178 0.0129 C21 0.0460 0.0315 0.0150 C22 0.0488 0.0350 0.0145 C23 0.0370 0.0223 0.0126 C24 0.0303 0.0190 0.0124 C25 0.0322 0.0213 0.0141 C26 0.0383 0.0222 0.0141 C27 0.0228 0.0143 0.0133 N1 0.0206 0.0147 0.0120 N2 0.0179 0.0092 0.0052 Cl1 0.0149 0.0133 0.0109 Rh1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.039 0.060 0.083 0.109 0.137 0.170 0.208 0.274 1.000 Number in group 570. 551. 538. 551. 537. 543. 553. 559. 535. 546. GooF 1.165 1.028 1.070 1.099 0.966 1.116 0.971 1.007 1.020 1.097 K 1.682 1.039 0.980 0.995 0.997 1.007 1.006 1.010 1.004 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 566. 553. 533. 545. 547. 548. 545. 549. 545. 552. GooF 0.911 0.852 0.749 0.769 0.662 0.613 0.768 0.954 1.396 2.040 K 0.995 0.998 1.009 1.013 1.012 1.008 1.006 1.007 0.996 1.013 R1 0.060 0.053 0.043 0.042 0.031 0.027 0.031 0.034 0.044 0.052 Recommended weighting scheme: WGHT 0.0496 9.0073 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) -3 0 3 965.64 390.49 6.91 0.076 3.31 -4 1 1 280.36 46.57 6.41 0.026 2.78 5 0 1 964.85 1892.69 6.27 0.167 2.23 -3 2 3 1858.80 1050.36 6.03 0.125 2.91 4 0 2 1523.31 2633.92 5.89 0.197 2.63 2 2 0 1787.52 1054.50 5.52 0.125 4.17 1 1 4 3083.96 2012.55 5.41 0.172 3.70 2 1 7 351.01 117.16 5.21 0.042 2.14 3 1 2 4190.35 2886.77 5.18 0.206 3.24 0 3 5 587.71 1145.96 5.16 0.130 2.62 1 1 2 2700.75 1803.97 4.90 0.163 5.77 1 3 0 2864.60 4158.49 4.76 0.248 3.84 2 5 7 831.34 448.41 4.73 0.081 1.62 3 1 4 2960.24 2045.40 4.69 0.174 2.65 2 4 0 846.63 462.46 4.68 0.083 2.70 -4 1 3 1361.03 838.02 4.64 0.111 2.59 -1 2 5 3150.31 2192.51 4.62 0.180 2.95 2 0 2 3529.32 4982.26 4.62 0.271 4.54 3 0 1 3809.45 2711.92 4.56 0.200 3.64 7 1 2 128.03 374.32 4.47 0.074 1.56 -3 4 7 2152.20 1465.10 4.37 0.147 1.76 0 4 2 7451.19 5634.46 4.36 0.288 2.88 5 1 0 420.13 190.79 4.34 0.053 2.24 0 2 2 5159.44 6962.24 4.33 0.321 4.97 -5 1 6 100.28 317.03 4.32 0.068 1.85 -1 4 3 1639.26 1077.16 4.28 0.126 2.65 -7 0 1 8.71 142.30 4.25 0.046 1.64 4 0 6 303.43 624.15 4.25 0.096 1.92 4 6 2 11.16 143.78 4.23 0.046 1.61 -2 1 1 72.44 3.95 4.18 0.008 5.07 1 3 2 1199.97 758.10 4.17 0.106 3.46 -2 2 2 104.13 306.44 4.09 0.067 3.86 5 6 1 1451.34 958.90 4.08 0.119 1.51 -5 5 6 1168.82 1753.18 3.97 0.161 1.49 2 1 9 86.77 10.81 3.92 0.013 1.73 0 4 0 4145.38 3076.98 3.88 0.213 3.06 7 0 1 2005.29 1404.49 3.87 0.144 1.61 3 1 6 228.79 478.61 3.84 0.084 2.15 1 7 0 1006.35 629.59 3.84 0.096 1.73 5 1 4 464.18 804.53 3.82 0.109 1.91 -1 7 2 173.03 54.43 3.79 0.028 1.70 -1 2 9 1890.16 1334.89 3.78 0.140 1.82 3 4 5 195.26 68.99 3.77 0.032 1.90 3 5 2 94.99 16.97 3.77 0.016 1.98 1 0 9 135.62 29.50 3.72 0.021 1.84 -6 0 4 380.94 185.73 3.70 0.052 1.80 -6 1 1 586.71 952.87 3.69 0.119 1.89 -2 3 5 8916.42 11245.04 3.66 0.408 2.45 0 1 11 52.13 188.24 3.59 0.053 1.54 -9 3 9 65.07 2.12 3.56 0.006 1.07 Bond lengths and angles C1 - Distance Angles N2 1.3507 (0.0039) N1 1.3578 (0.0038) 117.22 (0.26) Rh1 2.0297 (0.0029) 123.68 (0.21) 118.66 (0.21) C1 - N2 N1 C2 - Distance Angles C3 1.3864 (0.0048) C7 1.3903 (0.0048) 121.25 (0.31) N1 1.4522 (0.0039) 119.84 (0.30) 118.82 (0.29) C2 - C3 C7 C3 - Distance Angles C2 1.3864 (0.0048) C4 1.3875 (0.0051) 119.58 (0.36) C3 - C2 C4 - Distance Angles C5 1.3770 (0.0061) C3 1.3875 (0.0051) 120.32 (0.36) C4 - C5 C5 - Distance Angles C4 1.3770 (0.0061) C6 1.3853 (0.0058) 119.67 (0.33) C5 - C4 C6 - Distance Angles C5 1.3853 (0.0058) C7 1.3983 (0.0048) 121.30 (0.37) C6 - C5 C7 - Distance Angles C2 1.3903 (0.0048) C6 1.3983 (0.0048) 117.81 (0.33) C8 1.5027 (0.0050) 122.11 (0.30) 120.08 (0.34) C7 - C2 C6 C8 - Distance Angles C7 1.5027 (0.0050) C8 - C9 - Distance Angles N1 1.4909 (0.0040) C10 1.5249 (0.0046) 112.84 (0.26) C9 - N1 C10 - Distance Angles C9 1.5249 (0.0046) C11 1.5280 (0.0045) 112.03 (0.27) C10 - C9 C11 - Distance Angles C12 1.5142 (0.0044) C10 1.5280 (0.0045) 110.33 (0.26) C11 - C12 C12 - Distance Angles N2 1.4789 (0.0039) C11 1.5142 (0.0045) 112.19 (0.26) C12 - N2 C13 - Distance Angles C19 1.3910 (0.0045) C14 1.4018 (0.0044) 120.78 (0.29) N2 1.4425 (0.0038) 119.36 (0.28) 119.85 (0.28) C13 - C19 C14 C14 - Distance Angles C16 1.3948 (0.0044) C13 1.4018 (0.0044) 117.72 (0.30) C15 1.5103 (0.0046) 119.18 (0.29) 123.09 (0.28) C14 - C16 C13 C15 - Distance Angles C14 1.5103 (0.0046) C15 - C16 - Distance Angles C17 1.3831 (0.0049) C14 1.3948 (0.0044) 121.90 (0.31) C16 - C17 C17 - Distance Angles C16 1.3831 (0.0049) C18 1.3838 (0.0051) 119.69 (0.30) C17 - C16 C18 - Distance Angles C17 1.3838 (0.0051) C19 1.3935 (0.0045) 119.86 (0.32) C18 - C17 C19 - Distance Angles C13 1.3910 (0.0045) C18 1.3935 (0.0045) 120.02 (0.31) C19 - C13 C20 - Distance Angles C21 1.4083 (0.0046) C27 1.5187 (0.0045) 124.30 (0.31) Rh1 2.1204 (0.0030) 69.91 (0.18) 113.09 (0.21) C20 - C21 C27 C21 - Distance Angles C20 1.4083 (0.0046) C22 1.5128 (0.0048) 125.74 (0.31) Rh1 2.1043 (0.0031) 71.15 (0.18) 109.98 (0.24) C21 - C20 C22 C22 - Distance Angles C21 1.5128 (0.0048) C23 1.5249 (0.0057) 113.56 (0.29) C22 - C21 C23 - Distance Angles C24 1.5150 (0.0053) C22 1.5249 (0.0057) 112.52 (0.29) C23 - C24 C24 - Distance Angles C25 1.3763 (0.0049) C23 1.5150 (0.0053) 124.88 (0.33) Rh1 2.2201 (0.0032) 71.01 (0.19) 110.54 (0.24) C24 - C25 C23 C25 - Distance Angles C24 1.3763 (0.0049) C26 1.5078 (0.0045) 126.25 (0.32) Rh1 2.1989 (0.0031) 72.70 (0.19) 106.79 (0.21) C25 - C24 C26 C26 - Distance Angles C25 1.5078 (0.0045) C27 1.5281 (0.0047) 113.53 (0.28) C26 - C25 C27 - Distance Angles C20 1.5187 (0.0045) C26 1.5281 (0.0047) 112.42 (0.27) C27 - C20 N1 - Distance Angles C1 1.3578 (0.0038) C2 1.4522 (0.0039) 117.08 (0.25) C9 1.4909 (0.0040) 128.00 (0.26) 113.51 (0.24) N1 - C1 C2 N2 - Distance Angles C1 1.3507 (0.0039) C13 1.4425 (0.0038) 120.51 (0.25) C12 1.4789 (0.0039) 123.74 (0.26) 115.72 (0.24) N2 - C1 C13 Cl1 - Distance Angles Rh1 2.4470 (0.0007) Cl1 - Rh1 - Distance Angles C1 2.0297 (0.0030) C21 2.1043 (0.0031) 94.41 (0.12) C20 2.1204 (0.0030) 96.89 (0.12) 38.94 (0.13) C25 2.1989 (0.0031) 158.32 (0.12) 97.93 (0.13) 81.97 (0.12) C24 2.2201 (0.0032) 164.89 (0.13) 81.70 (0.13) 89.25 (0.13) 36.29 (0.13) Cl1 2.4470 (0.0007) 86.59 (0.08) 157.60 (0.10) 163.07 (0.09) 88.70 (0.09) 91.54 (0.10) Rh1 - C1 C21 C20 C25 C24 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0418 for 5483 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.07 at 0.0315 0.5062 0.2338 [ 0.35 A from CL1 ] Deepest hole -0.75 at 0.9751 0.3022 0.1977 [ 0.52 A from RH1 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3450 / 24814 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0315 0.5062 0.2338 1.00000 0.05 2.07 0.35 CL1 2.59 H3 2.61 H12B 2.63 RH1 Q2 1 1.1026 0.0189 0.1109 1.00000 0.05 0.67 0.72 H15A 1.09 C15 1.21 H15C 1.93 H15B Q3 1 1.1068 -0.0168 0.0122 1.00000 0.05 0.63 0.72 H15C 1.04 C15 1.18 H15B 1.90 H15A Q4 1 1.0178 -0.0236 0.3710 1.00000 0.05 0.61 0.80 H8B 0.95 C8 1.00 H8C 1.81 H8A Q5 1 0.8721 0.1135 0.2385 1.00000 0.05 0.58 0.57 H20 1.00 C20 2.02 C21 2.12 C27 Q6 1 1.1466 0.0358 0.3658 1.00000 0.05 0.55 0.93 H8C 0.97 H8A 1.01 C8 1.89 H8B Q7 1 0.9159 0.1189 0.1187 1.00000 0.05 0.55 0.59 H21 1.02 C21 2.01 C20 2.13 C22 Q8 1 1.2329 0.0242 0.0616 1.00000 0.05 0.51 0.65 H15B 1.03 C15 1.25 H15A 1.89 H15C Q9 1 1.0511 0.0260 0.2861 1.00000 0.05 0.50 0.87 H8A 1.09 H8B 1.12 C8 1.94 H8C Q10 1 0.9310 0.2063 0.1880 1.00000 0.05 0.49 1.23 C21 1.27 C20 1.27 H21 1.33 H20 Q11 1 1.0187 0.2957 0.3545 1.00000 0.05 0.40 0.76 C3 0.76 C2 1.41 H3 1.87 N1 Q12 1 0.8402 0.1631 0.1671 1.00000 0.05 0.39 0.73 C21 0.74 C20 1.44 H21 1.46 H20 Q13 1 0.8740 0.2339 0.1710 1.00000 0.05 0.36 0.94 C21 1.10 C20 1.27 RH1 1.48 H21 Q14 1 1.0588 0.1861 0.3784 1.00000 0.05 0.36 0.73 C7 0.80 C2 1.88 N1 1.90 C6 Q15 1 0.7823 0.4752 0.1199 1.00000 0.05 0.35 0.59 H24 0.99 C24 1.88 C25 2.11 H25 Q16 1 0.9528 0.3210 0.2533 1.00000 0.05 0.34 1.03 RH1 1.96 C1 2.15 H20 2.21 C2 Q17 1 1.0587 0.2790 0.3841 1.00000 0.05 0.34 0.68 C2 0.89 C3 1.60 H3 1.75 C7 Q18 1 0.9765 0.3182 0.1435 1.00000 0.05 0.34 1.04 RH1 1.96 C1 2.00 H21 2.12 C21 Q19 1 0.9402 0.2850 0.4724 1.00000 0.05 0.34 0.75 C5 0.83 C4 1.44 H5 1.50 H4 Q20 1 1.1456 0.2376 0.1208 1.00000 0.05 0.33 0.64 C13 0.81 N2 1.74 C19 1.86 C14 Shortest distances between peaks (including symmetry equivalents) 11 17 0.68 10 13 0.77 12 13 0.95 14 17 1.14 10 12 1.19 7 12 1.37 5 12 1.38 11 14 1.46 7 10 1.60 5 10 1.62 4 6 1.66 4 9 1.66 13 18 1.67 6 9 1.67 10 18 1.67 3 8 1.68 2 3 1.75 7 13 1.76 2 8 1.79 10 16 1.80 11 16 1.85 5 13 1.88 13 16 1.92 16 18 1.93 6 14 2.12 17 19 2.13 5 7 2.16 18 20 2.24 11 19 2.30 5 9 2.39 1 16 2.48 3 3 2.48 2 7 2.48 16 17 2.50 9 14 2.52 12 18 2.52 14 19 2.52 7 18 2.56 3 7 2.56 4 14 2.61 12 16 2.69 5 16 2.71 2 20 2.72 1 18 2.81 10 20 2.84 14 16 2.88 15 18 2.94 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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 0.03: Analyse other restraints etc. 5.58: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.75: Structure factors and derivatives 2.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.50: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0770 finished at 19:27:14 Total CPU time: 10.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++