+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0553 started at 16:40:24 on 09-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0553 in Pbca CELL 0.71073 16.8121 19.2293 22.9684 90.000 90.000 90.000 ZERR 8.00 0.0012 0.0024 0.0027 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O P CL FE RH UNIT 296 480 32 16 8 8 8 V = 7425.34 F(000) = 3456.0 Mu = 1.03 mm-1 Cell Wt = 6600.00 Rho = 1.476 MERG 2 OMIT -3.00 55.00 OMIT 4 0 0 OMIT 0 0 8 OMIT 2 0 2 OMIT 0 2 3 OMIT 1 3 1 OMIT 2 2 0 OMIT 11 4 6 OMIT 2 1 3 EXTI 0.00221 FMAP 2 PLAN 10 SIZE 0.25 0.30 0.35 ACTA BOND $H WGHT 0.05770 5.22450 L.S. 4 TEMP -153.00 FVAR 0.22809 C31 1 0.541290 0.161806 0.503101 11.00000 0.02529 0.07445 = 0.01718 -0.00121 0.00624 -0.00302 C32 1 0.581435 0.222863 0.512304 11.00000 0.03905 0.04398 = 0.01932 -0.00386 0.00773 0.01156 C33 1 0.632464 0.212281 0.566305 11.00000 0.04410 0.05289 = 0.01904 -0.01115 0.00060 0.00136 AFIX 13 H33 2 0.652728 0.254892 0.586378 11.00000 -1.20000 AFIX 0 C34 1 0.693755 0.161708 0.542775 11.00000 0.03770 0.06079 = 0.01877 -0.00435 -0.00668 0.00910 C35 1 0.656102 0.100137 0.534092 11.00000 0.07322 0.04685 = 0.01461 0.00903 0.00439 0.02184 C36 1 0.568070 0.111985 0.550699 11.00000 0.06467 0.05335 = 0.02303 0.00468 0.01233 -0.01383 AFIX 13 H36 2 0.534587 0.069823 0.557695 11.00000 -1.20000 AFIX 0 C37 1 0.579219 0.162786 0.601995 11.00000 0.05677 0.07012 = 0.01836 0.00321 0.00670 0.00801 AFIX 23 H37A 2 0.528856 0.184658 0.614786 11.00000 -1.20000 H37B 2 0.607162 0.141620 0.635543 11.00000 -1.20000 AFIX 0 O1 3 0.362403 0.132545 0.477468 11.00000 0.03826 0.11931 = 0.03359 0.01912 -0.01449 -0.02298 O2 3 0.293202 0.172603 0.397561 11.00000 0.04451 0.20314 = 0.08868 0.10709 -0.01297 -0.01993 O3 3 0.290531 0.060417 0.419178 11.00000 0.08253 0.10596 = 0.20531 -0.11405 -0.01478 0.00959 O4 3 0.224026 0.132711 0.478658 11.00000 0.03778 0.13279 = 0.05033 0.00469 0.01916 0.00977 H31 2 0.494761 0.153709 0.482079 11.00000 0.04311 H32 2 0.564071 0.267909 0.495972 11.00000 0.04638 H34 2 0.751167 0.170002 0.546435 11.00000 0.03518 H35 2 0.672573 0.059661 0.528835 11.00000 0.03802 MOLE 1 C1 1 0.588151 0.135490 0.303921 11.00000 0.01420 0.01278 = 0.01768 0.00035 0.00047 0.00219 C2 1 0.540753 0.073148 0.309999 11.00000 0.01172 0.01865 = 0.02326 -0.00341 0.00169 0.00034 C3 1 0.494130 0.049941 0.361931 11.00000 0.02056 0.01844 = 0.03223 0.00006 0.00811 -0.00408 AFIX 137 H3A 2 0.440303 0.069359 0.359953 11.00000 -1.50000 H3B 2 0.520409 0.066209 0.397498 11.00000 -1.50000 H3C 2 0.491123 -0.000952 0.362375 11.00000 -1.50000 AFIX 0 C4 1 0.542663 0.037163 0.255141 11.00000 0.01336 0.02505 = 0.03017 -0.01029 -0.00318 0.00222 C5 1 0.499030 -0.028997 0.241583 11.00000 0.02063 0.03115 = 0.05473 -0.02236 -0.00693 -0.00090 AFIX 137 H5A 2 0.447585 -0.017909 0.223797 11.00000 -1.50000 H5B 2 0.490400 -0.055227 0.277616 11.00000 -1.50000 H5C 2 0.530623 -0.057046 0.214485 11.00000 -1.50000 AFIX 0 C6 1 0.590074 0.075751 0.215816 11.00000 0.01541 0.03440 = 0.01845 -0.00619 -0.00418 0.00747 C7 1 0.605473 0.057323 0.153180 11.00000 0.02769 0.06142 = 0.02002 -0.01178 -0.00517 0.01617 AFIX 137 H7A 2 0.593394 0.008036 0.146883 11.00000 -1.50000 H7B 2 0.661471 0.066094 0.143878 11.00000 -1.50000 H7C 2 0.571588 0.085832 0.127968 11.00000 -1.50000 AFIX 0 C8 1 0.618715 0.136376 0.244565 11.00000 0.01697 0.02577 = 0.01469 0.00296 -0.00002 0.00558 C9 1 0.667994 0.189898 0.213475 11.00000 0.03091 0.03358 = 0.02147 0.01035 0.00697 0.00633 AFIX 137 H9A 2 0.701370 0.166965 0.184234 11.00000 -1.50000 H9B 2 0.701892 0.214158 0.241623 11.00000 -1.50000 H9C 2 0.632874 0.223497 0.194280 11.00000 -1.50000 AFIX 0 C10 1 0.747513 0.051626 0.346221 11.00000 0.01373 0.01659 = 0.01979 -0.00022 -0.00114 0.00153 C11 1 0.776888 0.049439 0.286684 11.00000 0.01385 0.02458 = 0.02165 0.00298 0.00220 0.00417 C12 1 0.827516 0.100250 0.254097 11.00000 0.01534 0.04116 = 0.02952 0.00875 0.00375 -0.00044 AFIX 137 H12A 2 0.883007 0.084669 0.254824 11.00000 -1.50000 H12B 2 0.823506 0.146121 0.272456 11.00000 -1.50000 H12C 2 0.809190 0.103236 0.213670 11.00000 -1.50000 AFIX 0 C13 1 0.747589 -0.012858 0.260298 11.00000 0.01880 0.02478 = 0.02115 -0.00322 -0.00019 0.00859 C14 1 0.767194 -0.037637 0.199998 11.00000 0.03301 0.04315 = 0.02668 -0.00686 0.00190 0.01916 AFIX 137 H14A 2 0.817406 -0.063507 0.200779 11.00000 -1.50000 H14B 2 0.772421 0.002461 0.173942 11.00000 -1.50000 H14C 2 0.724554 -0.068040 0.185910 11.00000 -1.50000 AFIX 0 C15 1 0.700123 -0.049446 0.301955 11.00000 0.02312 0.01571 = 0.02394 -0.00383 -0.00288 0.00420 C16 1 0.660680 -0.118536 0.292621 11.00000 0.03971 0.01873 = 0.03742 -0.00764 -0.00848 0.00167 AFIX 137 H16A 2 0.696307 -0.155770 0.305611 11.00000 -1.50000 H16B 2 0.648867 -0.124569 0.251145 11.00000 -1.50000 H16C 2 0.611103 -0.120400 0.315008 11.00000 -1.50000 AFIX 0 C17 1 0.699275 -0.009998 0.354831 11.00000 0.01789 0.01546 = 0.01853 0.00026 -0.00072 0.00093 C18 1 0.658764 -0.032822 0.409474 11.00000 0.02855 0.02349 = 0.02261 0.00452 -0.00037 -0.00312 AFIX 137 H18A 2 0.611374 -0.060057 0.399606 11.00000 -1.50000 H18B 2 0.643076 0.008109 0.432154 11.00000 -1.50000 H18C 2 0.695266 -0.061490 0.432509 11.00000 -1.50000 AFIX 0 C19 1 0.483502 0.222612 0.365800 11.00000 0.01908 0.02004 = 0.02381 -0.00075 0.00161 0.00290 AFIX 13 H19 2 0.456042 0.182646 0.385087 11.00000 -1.20000 AFIX 0 C20 1 0.444168 0.229168 0.305844 11.00000 0.02132 0.03079 = 0.03084 -0.00291 -0.00425 0.00620 AFIX 137 H20A 2 0.386208 0.229209 0.310389 11.00000 -1.50000 H20B 2 0.460095 0.189789 0.281397 11.00000 -1.50000 H20C 2 0.461053 0.272697 0.287415 11.00000 -1.50000 AFIX 0 C21 1 0.461136 0.286516 0.402105 11.00000 0.03099 0.03264 = 0.03454 -0.01318 -0.00047 0.01222 AFIX 137 H21A 2 0.481776 0.328512 0.383234 11.00000 -1.50000 H21B 2 0.484215 0.282244 0.441122 11.00000 -1.50000 H21C 2 0.403109 0.289674 0.405184 11.00000 -1.50000 AFIX 0 C22 1 0.647424 0.276030 0.340390 11.00000 0.02084 0.01546 = 0.03167 0.00333 0.00001 -0.00270 AFIX 13 H22 2 0.699722 0.259474 0.324961 11.00000 -1.20000 AFIX 0 C23 1 0.610257 0.321251 0.292957 11.00000 0.03072 0.02180 = 0.04729 0.01672 0.00328 0.00175 AFIX 137 H23A 2 0.565114 0.347017 0.309185 11.00000 -1.50000 H23B 2 0.591774 0.291629 0.260981 11.00000 -1.50000 H23C 2 0.650037 0.354116 0.278276 11.00000 -1.50000 AFIX 0 C24 1 0.665627 0.321526 0.393377 11.00000 0.04100 0.01669 = 0.04887 -0.00595 -0.00605 -0.00652 AFIX 137 H24A 2 0.702901 0.358373 0.382219 11.00000 -1.50000 H24B 2 0.689407 0.292914 0.424097 11.00000 -1.50000 H24C 2 0.616234 0.342438 0.407760 11.00000 -1.50000 AFIX 0 C25 1 0.824872 0.045491 0.455306 11.00000 0.03278 0.02508 = 0.03082 0.00088 -0.01256 0.00198 AFIX 13 H25 2 0.784281 0.014037 0.473175 11.00000 -1.20000 AFIX 0 C26 1 0.870030 0.077871 0.506727 11.00000 0.05072 0.05298 = 0.04356 -0.01616 -0.02999 0.02037 AFIX 137 H26A 2 0.887252 0.041032 0.533379 11.00000 -1.50000 H26B 2 0.834981 0.110222 0.527435 11.00000 -1.50000 H26C 2 0.916669 0.103021 0.492177 11.00000 -1.50000 AFIX 0 C27 1 0.881631 -0.002319 0.422105 11.00000 0.03643 0.02317 = 0.05236 -0.00597 -0.02093 0.01090 AFIX 137 H27A 2 0.928270 0.024270 0.409473 11.00000 -1.50000 H27B 2 0.854378 -0.021477 0.387968 11.00000 -1.50000 H27C 2 0.898627 -0.040396 0.447591 11.00000 -1.50000 AFIX 0 C28 1 0.836862 0.178178 0.386837 11.00000 0.01674 0.01957 = 0.04483 -0.00398 -0.00394 -0.00096 AFIX 13 H28 2 0.812544 0.201727 0.352340 11.00000 -1.20000 AFIX 0 C29 1 0.921189 0.156558 0.368494 11.00000 0.01633 0.03646 = 0.06029 -0.00905 -0.00129 -0.00049 AFIX 137 H29A 2 0.946527 0.194898 0.347370 11.00000 -1.50000 H29B 2 0.918237 0.115590 0.343208 11.00000 -1.50000 H29C 2 0.952593 0.145397 0.403204 11.00000 -1.50000 AFIX 0 C30 1 0.843105 0.233771 0.435020 11.00000 0.02458 0.02216 = 0.06787 -0.01433 -0.00252 -0.00424 AFIX 137 H30A 2 0.877166 0.216467 0.466469 11.00000 -1.50000 H30B 2 0.789968 0.243794 0.450423 11.00000 -1.50000 H30C 2 0.866150 0.276377 0.418784 11.00000 -1.50000 AFIX 0 P1 4 0.591707 0.197702 0.363701 11.00000 0.01543 0.01239 = 0.01657 -0.00027 0.00092 0.00046 P2 4 0.766826 0.108196 0.408628 11.00000 0.01704 0.01654 = 0.02325 -0.00216 -0.00506 0.00045 FE1 6 0.655432 0.049550 0.288680 11.00000 0.01255 0.01461 = 0.01529 -0.00204 0.00027 0.00064 RH1 7 0.650107 0.156827 0.452342 11.00000 0.01954 0.02026 = 0.01377 -0.00024 -0.00050 -0.00005 MOLE 2 CL1 5 0.292625 0.125720 0.444012 11.00000 0.02189 0.03258 = 0.01714 -0.00244 0.00148 -0.00168 HKLF 4 Covalent radii and connectivity table for 04src0553 in Pbca C 0.770 H 0.320 O 0.660 P 1.100 CL 0.990 FE 1.240 RH 1.350 C31 - C32 C36 Rh1 C32 - C31 C33 Rh1 C33 - C34 C32 C37 C34 - C35 C33 Rh1 C35 - C34 C36 Rh1 C36 - C31 C37 C35 C37 - C36 C33 O1 - Cl1 O2 - Cl1 O3 - Cl1 O4 - Cl1 C1 - C2 C8 P1 Fe1 C2 - C4 C1 C3 Fe1 C3 - C2 C4 - C6 C2 C5 Fe1 C5 - C4 C6 - C4 C8 C7 Fe1 C7 - C6 C8 - C6 C1 C9 Fe1 C9 - C8 C10 - C17 C11 P2 Fe1 C11 - C13 C10 C12 Fe1 C12 - C11 C13 - C11 C15 C14 Fe1 C14 - C13 C15 - C13 C17 C16 Fe1 C16 - C15 C17 - C15 C10 C18 Fe1 C18 - C17 C19 - C21 C20 P1 C20 - C19 C21 - C19 C22 - C23 C24 P1 C23 - C22 C24 - C22 C25 - C27 C26 P2 C26 - C25 C27 - C25 C28 - C29 C30 P2 C29 - C28 C30 - C28 P1 - C1 C22 C19 Rh1 P2 - C10 C28 C25 Rh1 Fe1 - C1 C10 C2 C17 C11 C8 C4 C6 C13 C15 Rh1 - C31 C35 C32 C34 P1 P2 Cl1 - O3 O2 O4 O1 45408 Reflections read, of which 2149 rejected -21 =< h =< 20, -24 =< k =< 20, -29 =< l =< 29, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 0 10 37.58 0.83 3 4.32 10 1 19 -0.97 0.22 5 3.81 2 Inconsistent equivalents 8466 Unique reflections, of which 0 suppressed R(int) = 0.0377 R(sigma) = 0.0332 Friedel opposites merged Maximum memory for data reduction = 5265 / 83791 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 = 6601 / 585389 wR2 = 0.1020 before cycle 1 for 8466 data and 448 / 448 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0577 * P )^2 + 5.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22654 0.00035 -4.417 OSF 2 0.00054 0.00015 -11.087 EXTI Mean shift/esd = 0.199 Maximum = -11.087 for EXTI Max. shift = 0.021 A for H32 Max. dU = 0.002 for H31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6601 / 585389 wR2 = 0.1007 before cycle 2 for 8466 data and 448 / 448 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0577 * P )^2 + 5.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22628 0.00033 -0.784 OSF 2 0.00039 0.00011 -1.323 EXTI Mean shift/esd = 0.047 Maximum = -1.323 for EXTI Max. shift = 0.009 A for H32 Max. dU = 0.000 for H32 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6601 / 585389 wR2 = 0.1007 before cycle 3 for 8466 data and 448 / 448 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0577 * P )^2 + 5.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22628 0.00033 0.006 OSF 2 0.00039 0.00011 0.032 EXTI Mean shift/esd = 0.004 Maximum = 0.080 for z H32 Max. shift = 0.003 A for H32 Max. dU =-0.001 for H32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6601 / 585389 wR2 = 0.1007 before cycle 4 for 8466 data and 448 / 448 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0577 * P )^2 + 5.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22629 0.00033 0.010 OSF 2 0.00039 0.00011 0.030 EXTI Mean shift/esd = 0.001 Maximum = 0.030 for EXTI Max. shift = 0.001 A for H32 Max. dU = 0.000 for H32 Largest correlation matrix elements -0.638 U23 O3 / U22 O3 -0.578 U12 O3 / U13 O3 0.551 z O2 / y O2 0.634 U23 O2 / U33 O2 0.573 U33 Rh1 / OSF -0.544 z O3 / y O3 0.633 U23 O2 / U22 O2 0.565 U12 O2 / U13 O2 0.542 U22 Rh1 / OSF -0.630 U23 O3 / U33 O3 0.556 U11 Rh1 / OSF 0.537 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H33 0.6527 0.2549 0.5864 13 1.000 0.000 C33 C34 C32 C37 H36 0.5348 0.0698 0.5578 13 1.000 0.000 C36 C31 C37 C35 H37A 0.6072 0.1417 0.6356 23 0.990 0.000 C37 C36 C33 H37B 0.5289 0.1846 0.6148 23 0.990 0.000 C37 C36 C33 H3A 0.4404 0.0696 0.3600 137 0.980 0.000 C3 C2 H3A H3B 0.5205 0.0660 0.3975 137 0.980 0.000 C3 C2 H3A H3C 0.4908 -0.0009 0.3622 137 0.980 0.000 C3 C2 H3A H5A 0.4479 -0.0179 0.2233 137 0.980 0.000 C5 C4 H5A H5B 0.4898 -0.0550 0.2776 137 0.980 0.000 C5 C4 H5A H5C 0.5309 -0.0573 0.2148 137 0.980 0.000 C5 C4 H5A H7A 0.5940 0.0079 0.1471 137 0.980 0.000 C7 C6 H7A H7B 0.6614 0.0666 0.1438 137 0.980 0.000 C7 C6 H7A H7C 0.5712 0.0854 0.1280 137 0.980 0.000 C7 C6 H7A H9A 0.7014 0.1670 0.1843 137 0.980 0.000 C9 C8 H9A H9B 0.7017 0.2143 0.2416 137 0.980 0.000 C9 C8 H9A H9C 0.6327 0.2234 0.1941 137 0.980 0.000 C9 C8 H9A H12A 0.8831 0.0846 0.2548 137 0.980 0.000 C12 C11 H12A H12B 0.8236 0.1461 0.2725 137 0.980 0.000 C12 C11 H12A H12C 0.8092 0.1033 0.2137 137 0.980 0.000 C12 C11 H12A H14A 0.8173 -0.0637 0.2007 137 0.980 0.000 C14 C13 H14A H14B 0.7726 0.0025 0.1739 137 0.980 0.000 C14 C13 H14A H14C 0.7244 -0.0679 0.1858 137 0.980 0.000 C14 C13 H14A H16A 0.6961 -0.1558 0.3058 137 0.980 0.000 C16 C15 H16A H16B 0.6490 -0.1246 0.2512 137 0.980 0.000 C16 C15 H16A H16C 0.6109 -0.1203 0.3149 137 0.980 0.000 C16 C15 H16A H18A 0.6116 -0.0603 0.3997 137 0.980 0.000 C18 C17 H18A H18B 0.6427 0.0082 0.4320 137 0.980 0.000 C18 C17 H18A H18C 0.6954 -0.0611 0.4327 137 0.980 0.000 C18 C17 H18A H19 0.4560 0.1826 0.3851 13 1.000 0.000 C19 C21 C20 P1 H20A 0.3861 0.2292 0.3105 137 0.980 0.000 C20 C19 H20A H20B 0.4599 0.1898 0.2814 137 0.980 0.000 C20 C19 H20A H20C 0.4610 0.2727 0.2874 137 0.980 0.000 C20 C19 H20A H21A 0.4814 0.3285 0.3831 137 0.980 0.000 C21 C19 H21A H21B 0.4846 0.2824 0.4410 137 0.980 0.000 C21 C19 H21A H21C 0.4031 0.2894 0.4055 137 0.980 0.000 C21 C19 H21A H22 0.6997 0.2595 0.3249 13 1.000 0.000 C22 C23 C24 P1 H23A 0.5650 0.3469 0.3092 137 0.980 0.000 C23 C22 H23A H23B 0.5919 0.2917 0.2610 137 0.980 0.000 C23 C22 H23A H23C 0.6500 0.3542 0.2784 137 0.980 0.000 C23 C22 H23A H24A 0.7028 0.3584 0.3823 137 0.980 0.000 C24 C22 H24A H24B 0.6893 0.2929 0.4241 137 0.980 0.000 C24 C22 H24A H24C 0.6161 0.3424 0.4078 137 0.980 0.000 C24 C22 H24A H25 0.7842 0.0141 0.4731 13 1.000 0.000 C25 C27 C26 P2 H26A 0.8871 0.0409 0.5334 137 0.980 0.000 C26 C25 H26A H26B 0.8350 0.1102 0.5274 137 0.980 0.000 C26 C25 H26A H26C 0.9167 0.1029 0.4922 137 0.980 0.000 C26 C25 H26A H27A 0.9284 0.0242 0.4097 137 0.980 0.000 C27 C25 H27A H27B 0.8544 -0.0213 0.3879 137 0.980 0.000 C27 C25 H27A H27C 0.8983 -0.0405 0.4476 137 0.980 0.000 C27 C25 H27A H28 0.8125 0.2017 0.3524 13 1.000 0.000 C28 C29 C30 P2 H29A 0.9464 0.1949 0.3472 137 0.980 0.000 C29 C28 H29A H29B 0.9181 0.1155 0.3432 137 0.980 0.000 C29 C28 H29A H29C 0.9526 0.1455 0.4031 137 0.980 0.000 C29 C28 H29A H30A 0.8773 0.2165 0.4664 137 0.980 0.000 C30 C28 H30A H30B 0.7900 0.2437 0.4504 137 0.980 0.000 C30 C28 H30A H30C 0.8661 0.2764 0.4187 137 0.980 0.000 C30 C28 H30A 04src0553 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C31 0.54132 0.16182 0.50311 1.00000 0.02534 0.07404 0.01702 -0.00107 0.00629 -0.00276 0.03880 0.00579 0.00018 0.00019 0.00012 0.00000 0.00149 0.00250 0.00134 0.00137 0.00119 0.00145 0.00078 C32 0.58149 0.22284 0.51233 1.00000 0.03875 0.04310 0.01926 -0.00356 0.00767 0.01147 0.03370 0.00556 0.00018 0.00018 0.00012 0.00000 0.00166 0.00191 0.00133 0.00124 0.00118 0.00138 0.00068 C33 0.63246 0.21230 0.56630 1.00000 0.04363 0.05277 0.01854 -0.01114 0.00048 0.00141 0.03831 0.00556 0.00019 0.00019 0.00013 0.00000 0.00178 0.00210 0.00133 0.00134 0.00127 0.00146 0.00074 H33 0.65274 0.25491 0.58636 1.00000 0.04598 0.00000 0.00000 C34 0.69369 0.16168 0.54279 1.00000 0.03731 0.06066 0.01831 -0.00449 -0.00680 0.00896 0.03876 0.00591 0.00021 0.00019 0.00012 0.00000 0.00185 0.00237 0.00140 0.00132 0.00124 0.00153 0.00079 C35 0.65609 0.10018 0.53413 1.00000 0.07331 0.04650 0.01427 0.00914 0.00451 0.02179 0.04469 0.00713 0.00023 0.00021 0.00013 0.00000 0.00262 0.00230 0.00134 0.00136 0.00142 0.00190 0.00093 C36 0.56821 0.11198 0.55076 1.00000 0.06545 0.05288 0.02255 0.00466 0.01245 -0.01428 0.04696 0.00618 0.00023 0.00020 0.00013 0.00000 0.00239 0.00226 0.00152 0.00137 0.00146 0.00180 0.00089 H36 0.53476 0.06981 0.55778 1.00000 0.05636 0.00000 0.00000 C37 0.57929 0.16281 0.60199 1.00000 0.05596 0.07009 0.01827 0.00323 0.00656 0.00805 0.04810 0.00640 0.00023 0.00019 0.00013 0.00000 0.00216 0.00257 0.00142 0.00145 0.00144 0.00175 0.00090 H37A 0.60725 0.14169 0.63555 1.00000 0.05773 0.00000 0.00000 H37B 0.52889 0.18464 0.61476 1.00000 0.05773 0.00000 0.00000 O1 0.36248 0.13251 0.47742 1.00000 0.03746 0.11987 0.03360 0.01935 -0.01476 -0.02315 0.06364 0.00463 0.00014 0.00018 0.00011 0.00000 0.00133 0.00252 0.00132 0.00150 0.00106 0.00144 0.00083 O2 0.29329 0.17270 0.39765 1.00000 0.04489 0.20277 0.08935 0.10808 -0.01303 -0.01989 0.11234 0.00751 0.00017 0.00024 0.00016 0.00000 0.00166 0.00431 0.00243 0.00276 0.00163 0.00207 0.00165 O3 0.29063 0.06032 0.41929 1.00000 0.08396 0.10468 0.20332 -0.11303 -0.01517 0.00986 0.13065 0.00591 0.00023 0.00021 0.00023 0.00000 0.00264 0.00311 0.00477 0.00333 0.00286 0.00217 0.00191 O4 0.22394 0.13269 0.47859 1.00000 0.03740 0.13295 0.05039 0.00484 0.01957 0.01021 0.07358 0.00576 0.00015 0.00019 0.00013 0.00000 0.00141 0.00279 0.00163 0.00178 0.00124 0.00158 0.00090 H31 0.49397 0.15397 0.48107 1.00000 0.04525 0.06291 0.00222 0.00166 0.00159 0.00000 0.00975 H32 0.56574 0.26723 0.49623 1.00000 0.04716 0.05975 0.00209 0.00186 0.00152 0.00000 0.00983 H34 0.75122 0.17067 0.54645 1.00000 0.03570 0.05710 0.00217 0.00163 0.00129 0.00000 0.00909 H35 0.67186 0.05980 0.52934 1.00000 0.03772 0.06169 0.00211 0.00186 0.00154 0.00000 0.00960 C1 0.58814 0.13548 0.30392 1.00000 0.01379 0.01254 0.01738 0.00040 0.00052 0.00225 0.01457 0.00397 0.00013 0.00012 0.00010 0.00000 0.00106 0.00112 0.00111 0.00087 0.00087 0.00084 0.00045 C2 0.54080 0.07317 0.31002 1.00000 0.01165 0.01839 0.02271 -0.00339 0.00170 0.00039 0.01758 0.00400 0.00013 0.00012 0.00011 0.00000 0.00107 0.00124 0.00121 0.00096 0.00093 0.00086 0.00048 C3 0.49408 0.04995 0.36190 1.00000 0.02041 0.01807 0.03218 -0.00002 0.00817 -0.00400 0.02355 0.00457 0.00015 0.00013 0.00012 0.00000 0.00124 0.00131 0.00141 0.00103 0.00106 0.00096 0.00055 H3A 0.44036 0.06959 0.35999 1.00000 0.03533 0.00000 0.00000 H3B 0.52047 0.06597 0.39750 1.00000 0.03533 0.00000 0.00000 H3C 0.49081 -0.00093 0.36221 1.00000 0.03533 0.00000 0.00000 C4 0.54269 0.03714 0.25515 1.00000 0.01324 0.02468 0.02989 -0.01037 -0.00333 0.00227 0.02260 0.00418 0.00014 0.00014 0.00012 0.00000 0.00115 0.00137 0.00138 0.00105 0.00101 0.00096 0.00054 C5 0.49903 -0.02901 0.24156 1.00000 0.02035 0.03086 0.05484 -0.02246 -0.00671 -0.00105 0.03535 0.00450 0.00016 0.00015 0.00015 0.00000 0.00135 0.00161 0.00195 0.00139 0.00130 0.00114 0.00072 H5A 0.44789 -0.01790 0.22332 1.00000 0.05302 0.00000 0.00000 H5B 0.48979 -0.05498 0.27764 1.00000 0.05302 0.00000 0.00000 H5C 0.53092 -0.05731 0.21484 1.00000 0.05302 0.00000 0.00000 C6 0.59012 0.07578 0.21579 1.00000 0.01494 0.03419 0.01821 -0.00623 -0.00423 0.00754 0.02245 0.00438 0.00014 0.00014 0.00011 0.00000 0.00116 0.00153 0.00119 0.00103 0.00095 0.00101 0.00054 C7 0.60551 0.05732 0.15324 1.00000 0.02712 0.06123 0.01973 -0.01179 -0.00514 0.01602 0.03603 0.00526 0.00017 0.00018 0.00012 0.00000 0.00146 0.00214 0.00133 0.00132 0.00115 0.00136 0.00073 H7A 0.59400 0.00791 0.14707 1.00000 0.05404 0.00000 0.00000 H7B 0.66136 0.06657 0.14382 1.00000 0.05404 0.00000 0.00000 H7C 0.57120 0.08544 0.12803 1.00000 0.05404 0.00000 0.00000 C8 0.61871 0.13638 0.24455 1.00000 0.01637 0.02544 0.01473 0.00303 0.00009 0.00556 0.01885 0.00434 0.00014 0.00014 0.00010 0.00000 0.00113 0.00136 0.00112 0.00095 0.00092 0.00098 0.00049 C9 0.66790 0.18992 0.21342 1.00000 0.03056 0.03330 0.02116 0.01033 0.00696 0.00630 0.02834 0.00536 0.00017 0.00015 0.00012 0.00000 0.00142 0.00164 0.00130 0.00113 0.00110 0.00118 0.00061 H9A 0.70141 0.16698 0.18426 1.00000 0.04251 0.00000 0.00000 H9B 0.70166 0.21433 0.24157 1.00000 0.04251 0.00000 0.00000 H9C 0.63273 0.22339 0.19412 1.00000 0.04251 0.00000 0.00000 C10 0.74750 0.05162 0.34621 1.00000 0.01355 0.01621 0.01954 -0.00026 -0.00114 0.00149 0.01643 0.00398 0.00013 0.00012 0.00010 0.00000 0.00107 0.00124 0.00115 0.00091 0.00092 0.00086 0.00048 C11 0.77693 0.04941 0.28672 1.00000 0.01359 0.02431 0.02140 0.00296 0.00226 0.00395 0.01977 0.00440 0.00014 0.00013 0.00011 0.00000 0.00111 0.00138 0.00123 0.00098 0.00094 0.00092 0.00051 C12 0.82758 0.10024 0.25410 1.00000 0.01503 0.04068 0.02956 0.00876 0.00396 -0.00056 0.02842 0.00508 0.00015 0.00016 0.00012 0.00000 0.00120 0.00173 0.00142 0.00122 0.00107 0.00112 0.00061 H12A 0.88306 0.08464 0.25479 1.00000 0.04263 0.00000 0.00000 H12B 0.82362 0.14611 0.27248 1.00000 0.04263 0.00000 0.00000 H12C 0.80921 0.10326 0.21369 1.00000 0.04263 0.00000 0.00000 C13 0.74758 -0.01287 0.26030 1.00000 0.01863 0.02426 0.02105 -0.00322 -0.00021 0.00857 0.02131 0.00439 0.00015 0.00013 0.00011 0.00000 0.00118 0.00134 0.00120 0.00101 0.00099 0.00096 0.00052 C14 0.76717 -0.03763 0.19995 1.00000 0.03298 0.04279 0.02623 -0.00694 0.00177 0.01913 0.03400 0.00552 0.00018 0.00017 0.00012 0.00000 0.00154 0.00181 0.00142 0.00125 0.00121 0.00130 0.00068 H14A 0.81725 -0.06369 0.20074 1.00000 0.05100 0.00000 0.00000 H14B 0.77262 0.00249 0.17395 1.00000 0.05100 0.00000 0.00000 H14C 0.72440 -0.06786 0.18579 1.00000 0.05100 0.00000 0.00000 C15 0.70009 -0.04944 0.30198 1.00000 0.02277 0.01545 0.02353 -0.00385 -0.00286 0.00418 0.02059 0.00426 0.00015 0.00012 0.00011 0.00000 0.00124 0.00125 0.00126 0.00096 0.00101 0.00093 0.00051 C16 0.66058 -0.11851 0.29265 1.00000 0.03913 0.01842 0.03714 -0.00757 -0.00841 0.00163 0.03156 0.00473 0.00018 0.00015 0.00013 0.00000 0.00162 0.00144 0.00162 0.00115 0.00126 0.00112 0.00065 H16A 0.69609 -0.15575 0.30579 1.00000 0.04735 0.00000 0.00000 H16B 0.64896 -0.12462 0.25116 1.00000 0.04735 0.00000 0.00000 H16C 0.61089 -0.12026 0.31491 1.00000 0.04735 0.00000 0.00000 C17 0.69925 -0.01000 0.35479 1.00000 0.01783 0.01511 0.01831 0.00033 -0.00068 0.00085 0.01708 0.00405 0.00014 0.00012 0.00010 0.00000 0.00114 0.00120 0.00114 0.00091 0.00090 0.00089 0.00048 C18 0.65875 -0.03279 0.40953 1.00000 0.02809 0.02339 0.02228 0.00455 -0.00031 -0.00312 0.02459 0.00469 0.00016 0.00014 0.00011 0.00000 0.00139 0.00141 0.00129 0.00105 0.00105 0.00103 0.00056 H18A 0.61158 -0.06034 0.39970 1.00000 0.03688 0.00000 0.00000 H18B 0.64271 0.00816 0.43204 1.00000 0.03688 0.00000 0.00000 H18C 0.69541 -0.06114 0.43271 1.00000 0.03688 0.00000 0.00000 C19 0.48348 0.22261 0.36577 1.00000 0.01867 0.01965 0.02367 -0.00083 0.00152 0.00285 0.02067 0.00431 0.00014 0.00013 0.00011 0.00000 0.00118 0.00128 0.00126 0.00098 0.00098 0.00094 0.00051 H19 0.45604 0.18263 0.38506 1.00000 0.02480 0.00000 0.00000 C20 0.44407 0.22917 0.30588 1.00000 0.02089 0.03052 0.03052 -0.00291 -0.00412 0.00613 0.02731 0.00466 0.00016 0.00015 0.00012 0.00000 0.00127 0.00151 0.00140 0.00115 0.00109 0.00108 0.00058 H20A 0.38612 0.22923 0.31047 1.00000 0.04096 0.00000 0.00000 H20B 0.45994 0.18978 0.28142 1.00000 0.04096 0.00000 0.00000 H20C 0.46095 0.27269 0.28743 1.00000 0.04096 0.00000 0.00000 C21 0.46112 0.28648 0.40214 1.00000 0.03075 0.03225 0.03424 -0.01308 -0.00057 0.01217 0.03241 0.00498 0.00017 0.00015 0.00013 0.00000 0.00149 0.00159 0.00154 0.00123 0.00122 0.00117 0.00065 H21A 0.48137 0.32853 0.38313 1.00000 0.04862 0.00000 0.00000 H21B 0.48459 0.28235 0.44104 1.00000 0.04862 0.00000 0.00000 H21C 0.40311 0.28942 0.40551 1.00000 0.04862 0.00000 0.00000 C22 0.64738 0.27601 0.34036 1.00000 0.02050 0.01532 0.03134 0.00324 0.00013 -0.00267 0.02239 0.00440 0.00014 0.00013 0.00012 0.00000 0.00124 0.00129 0.00139 0.00104 0.00104 0.00092 0.00054 H22 0.69969 0.25947 0.32493 1.00000 0.02686 0.00000 0.00000 C23 0.61025 0.32125 0.29300 1.00000 0.03031 0.02162 0.04679 0.01662 0.00332 0.00171 0.03291 0.00563 0.00017 0.00015 0.00014 0.00000 0.00147 0.00146 0.00177 0.00126 0.00130 0.00114 0.00066 H23A 0.56503 0.34692 0.30922 1.00000 0.04936 0.00000 0.00000 H23B 0.59189 0.29168 0.26096 1.00000 0.04936 0.00000 0.00000 H23C 0.65000 0.35421 0.27841 1.00000 0.04936 0.00000 0.00000 C24 0.66555 0.32150 0.39343 1.00000 0.04053 0.01647 0.04877 -0.00599 -0.00601 -0.00637 0.03526 0.00491 0.00019 0.00015 0.00015 0.00000 0.00164 0.00140 0.00184 0.00128 0.00143 0.00119 0.00068 H24A 0.70281 0.35837 0.38230 1.00000 0.05289 0.00000 0.00000 H24B 0.68934 0.29286 0.42413 1.00000 0.05289 0.00000 0.00000 H24C 0.61614 0.34237 0.40782 1.00000 0.05289 0.00000 0.00000 C25 0.82485 0.04552 0.45527 1.00000 0.03246 0.02488 0.03051 0.00066 -0.01249 0.00236 0.02928 0.00484 0.00018 0.00015 0.00012 0.00000 0.00148 0.00152 0.00151 0.00111 0.00118 0.00117 0.00062 H25 0.78423 0.01408 0.47312 1.00000 0.03514 0.00000 0.00000 C26 0.86999 0.07781 0.50673 1.00000 0.04985 0.05271 0.04365 -0.01612 -0.02995 0.02035 0.04874 0.00559 0.00022 0.00019 0.00015 0.00000 0.00198 0.00226 0.00192 0.00162 0.00164 0.00165 0.00094 H26A 0.88711 0.04093 0.53338 1.00000 0.07311 0.00000 0.00000 H26B 0.83497 0.11020 0.52743 1.00000 0.07311 0.00000 0.00000 H26C 0.91670 0.10290 0.49223 1.00000 0.07311 0.00000 0.00000 C27 0.88157 -0.00231 0.42217 1.00000 0.03572 0.02292 0.05178 -0.00609 -0.02061 0.01085 0.03681 0.00509 0.00018 0.00015 0.00014 0.00000 0.00159 0.00154 0.00191 0.00132 0.00146 0.00123 0.00073 H27A 0.92838 0.02418 0.40974 1.00000 0.05521 0.00000 0.00000 H27B 0.85444 -0.02130 0.38792 1.00000 0.05521 0.00000 0.00000 H27C 0.89828 -0.04050 0.44764 1.00000 0.05521 0.00000 0.00000 C28 0.83687 0.17819 0.38687 1.00000 0.01638 0.01910 0.04472 -0.00390 -0.00398 -0.00095 0.02673 0.00456 0.00015 0.00014 0.00013 0.00000 0.00119 0.00133 0.00166 0.00118 0.00114 0.00097 0.00058 H28 0.81253 0.20174 0.35238 1.00000 0.03208 0.00000 0.00000 C29 0.92111 0.15656 0.36846 1.00000 0.01611 0.03592 0.06055 -0.00904 -0.00154 -0.00037 0.03753 0.00531 0.00016 0.00016 0.00016 0.00000 0.00128 0.00174 0.00212 0.00145 0.00133 0.00113 0.00074 H29A 0.94639 0.19486 0.34725 1.00000 0.05629 0.00000 0.00000 H29B 0.91811 0.11554 0.34323 1.00000 0.05629 0.00000 0.00000 H29C 0.95260 0.14547 0.40314 1.00000 0.05629 0.00000 0.00000 C30 0.84313 0.23376 0.43498 1.00000 0.02462 0.02204 0.06700 -0.01448 -0.00259 -0.00413 0.03788 0.00506 0.00017 0.00016 0.00016 0.00000 0.00144 0.00157 0.00216 0.00147 0.00139 0.00111 0.00075 H30A 0.87728 0.21651 0.46640 1.00000 0.05682 0.00000 0.00000 H30B 0.79001 0.24373 0.45044 1.00000 0.05682 0.00000 0.00000 H30C 0.86607 0.27638 0.41871 1.00000 0.05682 0.00000 0.00000 P1 0.59170 0.19770 0.36370 1.00000 0.01515 0.01209 0.01630 -0.00025 0.00092 0.00043 0.01451 0.00102 0.00003 0.00003 0.00003 0.00000 0.00029 0.00030 0.00029 0.00022 0.00023 0.00021 0.00013 P2 0.76683 0.10820 0.40864 1.00000 0.01677 0.01622 0.02296 -0.00215 -0.00509 0.00045 0.01865 0.00106 0.00004 0.00003 0.00003 0.00000 0.00030 0.00032 0.00033 0.00024 0.00024 0.00023 0.00014 Fe1 0.65543 0.04955 0.28868 1.00000 0.01228 0.01436 0.01503 -0.00203 0.00027 0.00065 0.01389 0.00056 0.00002 0.00002 0.00001 0.00000 0.00017 0.00019 0.00017 0.00012 0.00012 0.00012 0.00009 Rh1 0.65011 0.15683 0.45234 1.00000 0.01925 0.02000 0.01351 -0.00024 -0.00050 -0.00005 0.01759 0.00032 0.00001 0.00001 0.00001 0.00000 0.00012 0.00013 0.00011 0.00007 0.00007 0.00007 0.00008 Cl1 0.29263 0.12572 0.44401 1.00000 0.02152 0.03234 0.01679 -0.00243 0.00147 -0.00168 0.02355 0.00107 0.00004 0.00004 0.00003 0.00000 0.00031 0.00036 0.00028 0.00024 0.00022 0.00025 0.00015 Final Structure Factor Calculation for 04src0553 in Pbca Total number of l.s. parameters = 448 Maximum vector length = 511 Memory required = 6153 / 26061 wR2 = 0.1007 before cycle 5 for 8466 data and 0 / 448 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0577 * P )^2 + 5.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0340 for 6749 Fo > 4sig(Fo) and 0.0491 for all 8466 data wR2 = 0.1007, GooF = S = 1.039, Restrained GooF = 1.039 for all data Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 60.00 for hydrogen atoms Principal mean square atomic displacements U 0.0742 0.0285 0.0136 C31 0.0527 0.0338 0.0146 C32 0.0562 0.0435 0.0152 C33 0.0646 0.0356 0.0161 C34 0.0865 0.0358 0.0118 C35 0.0760 0.0477 0.0171 C36 0.0743 0.0529 0.0171 C37 0.1311 0.0392 0.0206 O1 0.2706 0.0424 0.0240 O2 may be split into 0.2918 0.1833 0.4030 and 0.2948 0.1621 0.3923 0.2790 0.0823 0.0307 O3 may be split into 0.2894 0.0540 0.4273 and 0.2919 0.0666 0.4112 0.1346 0.0631 0.0230 O4 0.0176 0.0153 0.0108 C1 0.0247 0.0168 0.0113 C2 0.0366 0.0207 0.0134 C3 0.0386 0.0166 0.0126 C4 0.0689 0.0231 0.0141 C5 0.0393 0.0165 0.0115 C6 0.0708 0.0208 0.0165 C7 0.0286 0.0152 0.0127 C8 0.0449 0.0256 0.0146 C9 0.0198 0.0167 0.0127 C10 0.0276 0.0196 0.0121 C11 0.0456 0.0260 0.0137 C12 0.0312 0.0207 0.0121 C13 0.0583 0.0286 0.0151 C14 0.0285 0.0203 0.0130 C15 0.0480 0.0311 0.0157 C16 0.0188 0.0176 0.0148 C17 0.0305 0.0254 0.0179 C18 0.0241 0.0220 0.0159 C19 0.0368 0.0277 0.0174 C20 0.0507 0.0318 0.0148 C21 0.0320 0.0215 0.0137 C22 0.0556 0.0298 0.0134 C23 0.0521 0.0403 0.0134 C24 0.0441 0.0255 0.0183 C25 0.0934 0.0363 0.0165 C26 0.0686 0.0263 0.0155 C27 0.0458 0.0192 0.0152 C28 0.0636 0.0330 0.0160 C29 0.0713 0.0270 0.0154 C30 0.0168 0.0147 0.0120 P1 0.0263 0.0160 0.0137 P2 0.0168 0.0132 0.0118 Fe1 0.0200 0.0193 0.0135 Rh1 0.0330 0.0215 0.0161 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.030 0.047 0.064 0.084 0.107 0.138 0.179 0.255 1.000 Number in group 881. 838. 840. 829. 856. 837. 854. 835. 842. 854. GooF 0.946 1.051 1.191 1.175 1.139 1.084 1.033 0.880 0.929 0.910 K 0.751 0.809 0.913 0.946 0.964 0.979 0.993 1.010 1.026 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 850. 868. 830. 859. 843. 850. 823. 851. 841. 851. GooF 0.872 0.896 0.891 0.973 0.969 0.953 1.001 1.047 1.092 1.530 K 0.984 1.009 1.004 1.012 1.020 1.035 1.038 1.029 1.017 0.984 R1 0.102 0.090 0.073 0.059 0.052 0.042 0.037 0.035 0.028 0.031 Recommended weighting scheme: WGHT 0.0428 8.6916 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) 0 0 4 25071.11 46865.86 6.61 0.473 5.74 2 6 5 -28.31 120.48 5.21 0.024 2.51 3 8 4 109.65 358.98 5.17 0.041 2.06 1 8 4 2250.82 1473.87 5.16 0.084 2.20 0 6 7 1071.99 1730.88 4.85 0.091 2.29 2 3 0 660.16 353.29 4.84 0.041 5.10 2 6 7 753.56 1269.80 4.81 0.078 2.21 4 21 11 227.94 1561.07 4.80 0.086 0.82 2 4 4 80.96 258.00 4.54 0.035 3.38 5 1 7 2544.25 3596.69 4.50 0.131 2.33 2 0 10 2314.74 1576.20 4.37 0.087 2.22 1 14 6 549.49 962.39 4.32 0.068 1.29 8 2 3 6612.35 10324.71 4.23 0.222 1.98 3 4 4 1581.49 1102.44 4.20 0.072 3.08 5 3 6 1864.01 1290.72 4.17 0.078 2.35 6 3 2 156.15 29.54 4.16 0.012 2.51 5 1 9 1880.98 2690.91 4.10 0.113 2.02 8 4 7 466.92 776.27 4.09 0.061 1.66 5 7 16 10.74 178.88 4.08 0.029 1.19 8 11 19 -60.42 226.87 4.04 0.033 0.90 9 5 6 3987.32 3010.51 3.94 0.120 1.54 2 8 8 3207.85 2371.40 3.92 0.106 1.80 7 6 6 2568.62 1903.84 3.85 0.095 1.72 4 4 8 3292.55 2475.83 3.81 0.109 2.13 9 12 17 382.63 733.46 3.78 0.059 0.90 6 3 0 5475.18 7114.42 3.77 0.184 2.57 5 3 4 1351.74 965.68 3.74 0.068 2.64 8 5 21 -56.75 101.03 3.68 0.022 0.94 3 12 5 180.23 404.03 3.66 0.044 1.46 10 4 6 1612.51 1168.34 3.66 0.075 1.47 1 6 3 601.67 377.72 3.66 0.042 2.91 5 15 2 31.03 235.31 3.65 0.033 1.19 6 19 12 596.58 1104.58 3.64 0.073 0.85 7 13 18 49.07 360.24 3.58 0.041 0.90 5 3 8 333.18 548.21 3.57 0.051 2.07 7 5 2 1622.13 2207.94 3.56 0.103 2.01 9 0 8 4344.69 3180.23 3.55 0.123 1.57 1 10 7 477.57 252.37 3.54 0.035 1.65 10 1 6 409.37 744.77 3.54 0.060 1.53 11 9 23 2782.00 4398.96 3.53 0.145 0.78 1 16 5 848.57 526.63 3.52 0.050 1.16 1 15 11 -77.31 119.04 3.49 0.024 1.09 1 6 7 589.99 898.61 3.49 0.065 2.27 2 4 9 370.21 205.89 3.48 0.031 2.18 8 6 2 372.17 208.26 3.46 0.032 1.74 5 13 6 792.85 492.33 3.45 0.048 1.28 2 8 0 6340.80 8061.07 3.45 0.196 2.31 2 10 7 970.29 1367.60 3.36 0.081 1.63 5 2 10 533.43 797.18 3.34 0.062 1.86 4 5 3 3966.25 3141.51 3.34 0.122 2.66 Bond lengths and angles C31 - Distance Angles C32 1.3703 (0.0047) C36 1.5234 (0.0046) 106.35 (0.28) Rh1 2.1711 (0.0029) 72.89 (0.17) 96.20 (0.20) H31 0.9554 (0.0372) 128.89 (2.00) 121.90 (2.06) 114.23 (2.19) C31 - C32 C36 Rh1 C32 - Distance Angles C31 1.3703 (0.0047) C33 1.5205 (0.0042) 106.83 (0.28) Rh1 2.2001 (0.0028) 70.58 (0.17) 97.94 (0.19) H32 0.9671 (0.0356) 124.17 (2.11) 125.72 (2.12) 114.41 (2.08) C32 - C31 C33 Rh1 C33 - Distance Angles C34 1.5162 (0.0045) C32 1.5205 (0.0042) 100.25 (0.23) C37 1.5417 (0.0048) 100.76 (0.29) 100.89 (0.26) H33 1.0000 117.29 117.30 117.30 C33 - C34 C32 C37 C34 - Distance Angles C35 1.3558 (0.0054) C33 1.5162 (0.0045) 107.20 (0.31) Rh1 2.2050 (0.0028) 70.72 (0.18) 97.87 (0.19) H34 0.9861 (0.0355) 128.53 (1.90) 121.54 (1.89) 114.44 (1.77) C34 - C35 C33 Rh1 C35 - Distance Angles C34 1.3558 (0.0054) C36 1.5428 (0.0053) 106.37 (0.31) Rh1 2.1738 (0.0031) 73.22 (0.19) 95.51 (0.20) H35 0.8278 (0.0346) 133.50 (2.59) 118.53 (2.58) 111.72 (2.50) C35 - C34 C36 Rh1 C36 - Distance Angles C31 1.5234 (0.0047) C37 1.5408 (0.0046) 100.68 (0.29) C35 1.5428 (0.0053) 101.47 (0.24) 99.60 (0.30) H36 1.0000 117.33 117.33 117.33 C36 - C31 C37 C35 C37 - Distance Angles C36 1.5408 (0.0046) C33 1.5417 (0.0048) 93.19 (0.24) H37A 0.9900 113.07 113.07 H37B 0.9900 113.07 113.07 110.46 C37 - C36 C33 H37A O1 - Distance Angles Cl1 1.4090 (0.0023) O1 - O2 - Distance Angles Cl1 1.3964 (0.0028) O2 - O3 - Distance Angles Cl1 1.3801 (0.0032) O3 - O4 - Distance Angles Cl1 1.4079 (0.0025) O4 - C1 - Distance Angles C2 1.4453 (0.0032) C8 1.4575 (0.0032) 107.13 (0.20) P1 1.8221 (0.0024) 119.31 (0.17) 133.29 (0.18) Fe1 2.0328 (0.0023) 69.47 (0.13) 69.65 (0.13) 130.18 (0.12) C1 - C2 C8 P1 C2 - Distance Angles C4 1.4384 (0.0034) C1 1.4453 (0.0032) 107.59 (0.21) C3 1.4954 (0.0033) 124.47 (0.22) 127.87 (0.21) Fe1 2.0397 (0.0022) 70.21 (0.13) 68.96 (0.13) 128.40 (0.18) C2 - C4 C1 C3 C3 - Distance Angles C2 1.4954 (0.0033) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C2 H3A H3B C4 - Distance Angles C6 1.4161 (0.0038) C2 1.4384 (0.0034) 108.61 (0.22) C5 1.5014 (0.0036) 125.94 (0.24) 125.41 (0.25) Fe1 2.0597 (0.0024) 70.11 (0.13) 68.72 (0.13) 128.75 (0.19) C4 - C6 C2 C5 C5 - Distance Angles C4 1.5014 (0.0036) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C4 H5A H5B C6 - Distance Angles C4 1.4161 (0.0038) C8 1.4231 (0.0037) 108.87 (0.21) C7 1.5022 (0.0035) 125.71 (0.26) 125.39 (0.26) Fe1 2.0648 (0.0024) 69.73 (0.14) 69.14 (0.13) 128.77 (0.18) C6 - C4 C8 C7 C7 - Distance Angles C6 1.5022 (0.0035) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C6 1.4231 (0.0037) C1 1.4575 (0.0032) 107.80 (0.21) C9 1.5017 (0.0036) 121.76 (0.22) 130.37 (0.23) Fe1 2.0485 (0.0024) 70.38 (0.15) 68.50 (0.13) 128.93 (0.18) C8 - C6 C1 C9 C9 - Distance Angles C8 1.5017 (0.0036) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C8 H9A H9B C10 - Distance Angles C17 1.4493 (0.0032) C11 1.4537 (0.0033) 107.13 (0.20) P2 1.8290 (0.0024) 118.62 (0.18) 133.92 (0.18) Fe1 2.0355 (0.0023) 69.32 (0.13) 69.40 (0.13) 130.96 (0.12) C10 - C17 C11 P2 C11 - Distance Angles C13 1.4305 (0.0036) C10 1.4537 (0.0033) 107.80 (0.21) C12 1.4973 (0.0035) 122.04 (0.23) 130.15 (0.24) Fe1 2.0432 (0.0024) 70.46 (0.14) 68.84 (0.13) 125.36 (0.18) C11 - C13 C10 C12 C12 - Distance Angles C11 1.4973 (0.0035) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles C11 1.4305 (0.0036) C15 1.4311 (0.0036) 108.67 (0.21) C14 1.5022 (0.0035) 125.53 (0.25) 125.72 (0.25) Fe1 2.0653 (0.0024) 68.80 (0.13) 69.88 (0.13) 129.78 (0.18) C13 - C11 C15 C14 C14 - Distance Angles C13 1.5022 (0.0035) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles C13 1.4311 (0.0036) C17 1.4308 (0.0033) 108.19 (0.21) C16 1.5004 (0.0036) 125.90 (0.23) 125.87 (0.24) Fe1 2.0689 (0.0024) 69.61 (0.14) 68.52 (0.13) 129.25 (0.19) C15 - C13 C17 C16 C16 - Distance Angles C15 1.5004 (0.0036) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C15 H16A H16B C17 - Distance Angles C15 1.4308 (0.0033) C10 1.4493 (0.0032) 108.21 (0.21) C18 1.4954 (0.0034) 124.18 (0.22) 127.51 (0.22) Fe1 2.0395 (0.0024) 70.73 (0.14) 69.02 (0.13) 128.76 (0.17) C17 - C15 C10 C18 C18 - Distance Angles C17 1.4954 (0.0034) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B C19 - Distance Angles C21 1.5322 (0.0035) C20 1.5321 (0.0035) 108.51 (0.21) P1 1.8821 (0.0025) 117.06 (0.18) 114.60 (0.17) H19 1.0000 105.16 105.16 105.16 C19 - C21 C20 P1 C20 - Distance Angles C19 1.5321 (0.0035) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C19 H20A H20B C21 - Distance Angles C19 1.5322 (0.0035) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C19 H21A H21B C22 - Distance Angles C23 1.5264 (0.0036) C24 1.5310 (0.0039) 108.87 (0.23) P1 1.8523 (0.0025) 117.57 (0.18) 109.57 (0.19) H22 1.0000 106.76 106.76 106.76 C22 - C23 C24 P1 C23 - Distance Angles C22 1.5264 (0.0036) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C24 - Distance Angles C22 1.5310 (0.0039) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B C25 - Distance Angles C27 1.5275 (0.0041) C26 1.5359 (0.0039) 108.54 (0.25) P2 1.8844 (0.0028) 115.18 (0.20) 115.77 (0.21) H25 1.0000 105.44 105.44 105.44 C25 - C27 C26 P2 C26 - Distance Angles C25 1.5359 (0.0039) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5275 (0.0041) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C25 H27A H27B C28 - Distance Angles C29 1.5355 (0.0037) C30 1.5408 (0.0041) 108.81 (0.22) P2 1.8569 (0.0027) 117.56 (0.20) 110.66 (0.21) H28 1.0000 106.38 106.38 106.38 C28 - C29 C30 P2 C29 - Distance Angles C28 1.5355 (0.0037) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C28 H29A H29B C30 - Distance Angles C28 1.5408 (0.0041) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C28 H30A H30B P1 - Distance Angles C1 1.8221 (0.0024) C22 1.8523 (0.0025) 109.42 (0.12) C19 1.8821 (0.0025) 98.88 (0.11) 106.80 (0.11) Rh1 2.3931 (0.0006) 116.03 (0.08) 107.81 (0.09) 117.30 (0.08) P1 - C1 C22 C19 P2 - Distance Angles C10 1.8290 (0.0024) C28 1.8569 (0.0028) 109.43 (0.12) C25 1.8844 (0.0028) 99.04 (0.12) 106.76 (0.13) Rh1 2.3944 (0.0007) 114.54 (0.08) 110.46 (0.09) 115.83 (0.10) P2 - C10 C28 C25 Fe1 - Distance Angles C1 2.0328 (0.0023) C10 2.0355 (0.0023) 107.19 (0.09) C2 2.0397 (0.0022) 41.57 (0.09) 123.93 (0.09) C17 2.0395 (0.0024) 121.95 (0.09) 41.67 (0.09) 106.70 (0.10) C11 2.0432 (0.0024) 124.14 (0.10) 41.76 (0.09) 161.84 (0.10) 69.79 (0.10) C8 2.0485 (0.0024) 41.84 (0.09) 122.31 (0.10) 69.68 (0.10) 159.21 (0.10) 106.95 (0.10) C4 2.0597 (0.0024) 69.30 (0.09) 160.86 (0.10) 41.08 (0.09) 123.07 (0.10) 155.72 (0.10) 68.41 (0.10) C6 2.0648 (0.0024) 69.22 (0.10) 157.82 (0.10) 68.78 (0.10) 158.90 (0.10) 120.94 (0.10) 40.48 (0.10) 40.16 (0.11) C13 2.0653 (0.0024) 160.76 (0.10) 69.26 (0.09) 156.05 (0.10) 68.76 (0.09) 40.75 (0.10) 122.93 (0.10) 120.32 (0.10) C15 2.0689 (0.0024) 157.57 (0.10) 69.28 (0.09) 120.81 (0.10) 40.75 (0.09) 68.85 (0.10) 158.80 (0.10) 106.41 (0.10) Fe1 - C1 C10 C2 C17 C11 C8 C4 Rh1 - Distance Angles C31 2.1711 (0.0029) C35 2.1738 (0.0031) 66.24 (0.13) C32 2.2001 (0.0028) 36.53 (0.12) 76.84 (0.13) C34 2.2050 (0.0028) 76.82 (0.12) 36.06 (0.14) 63.88 (0.12) P1 2.3931 (0.0006) 95.55 (0.09) 156.74 (0.11) 97.36 (0.08) 157.53 (0.09) P2 2.3944 (0.0007) 158.88 (0.10) 97.39 (0.10) 156.58 (0.09) 98.00 (0.09) 96.19 (0.02) Rh1 - C31 C35 C32 C34 P1 Cl1 - Distance Angles O3 1.3801 (0.0032) O2 1.3964 (0.0028) 106.03 (0.33) O4 1.4079 (0.0025) 107.39 (0.25) 112.03 (0.21) O1 1.4090 (0.0023) 109.19 (0.24) 110.41 (0.18) 111.56 (0.17) Cl1 - O3 O2 O4 FMAP and GRID set by program FMAP 2 2 24 GRID -1.190 24 -2 1.190 1 2 R1 = 0.0483 for 8466 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.04 at 0.3016 0.1071 0.3887 [ 1.16 A from O3 ] Deepest hole -0.85 at 0.2897 0.0309 0.4529 [ 0.96 A from O3 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 6544 / 57129 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3016 0.1071 0.3887 1.00000 0.05 1.04 1.16 O3 1.29 O2 1.33 CL1 2.33 O1 Q2 1 0.3623 0.0768 0.4569 1.00000 0.05 0.88 1.17 O1 1.52 O3 1.53 CL1 2.57 O2 Q3 1 0.2328 0.0769 0.4622 1.00000 0.05 0.88 1.15 O4 1.42 O3 1.44 CL1 2.31 H25 Q4 1 0.2984 0.1995 0.4414 1.00000 0.05 0.67 1.13 O2 1.42 CL1 1.87 O1 1.99 O4 Q5 1 0.3140 0.1804 0.4766 1.00000 0.05 0.61 1.23 O1 1.34 CL1 1.77 O4 1.85 O2 Q6 1 0.6578 0.4462 0.3082 1.00000 0.05 0.47 1.90 H23C 1.95 H27B 2.04 H5A 2.09 C13 Q7 1 0.5531 0.3441 0.5455 1.00000 0.05 0.45 1.87 H32 2.07 H29C 2.35 H7C 2.50 C32 Q8 1 0.6478 0.1594 0.6446 1.00000 0.05 0.45 0.79 H37A 1.51 C37 2.08 C33 2.17 H37B Q9 1 0.6594 0.2640 0.2893 1.00000 0.05 0.40 1.07 H22 1.21 C22 1.38 C23 1.41 H23B Q10 1 0.6010 0.1933 0.4102 1.00000 0.05 0.39 1.08 P1 1.45 RH1 2.29 C19 2.39 C22 Shortest distances between peaks (including symmetry equivalents) 4 5 0.93 1 2 1.96 1 3 2.13 1 4 2.15 2 3 2.18 2 5 2.20 3 5 2.43 1 5 2.47 2 4 2.62 3 4 2.65 Time profile in seconds ----------------------- 0.03: 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 0.02: Analyse other restraints etc. 1.88: Read intensity data, sort/merge etc. 0.02: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.44: Structure factors and derivatives 8.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.19: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0553 finished at 16:40:42 Total CPU time: 17.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++