+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 09:55:40 on 05-Sep-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in I4(1)/acd CELL 0.71069 33.7880 33.7880 22.0140 90.000 90.000 90.000 ZERR 16.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 2 SYMM - X, 1/2 - Y, Z SYMM X, - Y, 1/2 - Z SYMM 1/2 - X, Y, - Z SYMM 1/4 - Y, 1/4 - X, 1/4 - Z SYMM 3/4 + Y, 1/4 + X, 1/4 - Z SYMM 1/4 + Y, 1/4 - X, 3/4 + Z SYMM 1/4 - Y, 3/4 + X, 1/4 + Z SFAC C H N O P CL PD UNIT 1056 928 32 96 64 32 16 V = 25131.82 F(000) = 10496.0 Mu = 0.53 mm-1 Cell Wt = 20421.19 Rho = 1.349 MERG 2 OMIT 4 4 0 OMIT 1 6 3 OMIT 1 4 3 OMIT 3 8 3 ACTA SHEL 7 0.84 DFIX 0.84 0.0001 O1 H1 EADP CL2A CL2B FMAP 2 PLAN 10 SIZE 0.12 0.18 0.20 HTAB O2 CL2B HTAB O2 CL2A HTAB O1 CL1 BOND $H WGHT 0.10410 L.S. 11 TEMP -153.00 FVAR 0.01380 0.60593 PD1 7 0.500000 0.000000 0.500000 10.50000 0.06845 0.05180 = 0.04915 -0.01020 -0.00270 0.00347 CL1 6 0.610182 -0.139818 0.625000 10.50000 0.08137 0.08137 = 0.08883 -0.00223 0.00223 0.03116 P1 5 0.481993 0.018662 0.599276 11.00000 0.07991 0.05530 = 0.05265 -0.00916 -0.00122 0.00756 P2 5 0.556691 0.040085 0.500909 11.00000 0.07462 0.05690 = 0.05521 -0.01042 -0.00324 -0.00406 N1 3 0.460672 -0.059357 0.613473 11.00000 0.07833 0.05548 = 0.05147 0.00200 -0.00250 -0.01427 O1 4 0.531225 -0.095149 0.613311 11.00000 0.06482 0.07213 = 0.07402 0.00768 -0.00247 0.00070 O2 4 0.399255 -0.056254 0.698674 11.00000 0.07734 0.11337 = 0.08102 -0.00699 0.01035 0.00354 AFIX 147 H2 2 0.376364 -0.046557 0.699032 11.00000 -1.50000 AFIX 0 O3 4 0.366778 -0.112527 0.701662 11.00000 0.09225 0.15217 = 0.11081 -0.01847 0.00628 -0.04093 C1 1 0.434704 0.044780 0.595144 11.00000 0.07304 0.06389 = 0.05720 -0.01843 -0.00048 -0.00558 C2 1 0.424361 0.064865 0.543602 11.00000 0.09241 0.07097 = 0.06693 -0.01058 0.00034 0.01673 AFIX 43 H2A 2 0.442064 0.065239 0.510080 11.00000 -1.20000 AFIX 0 C3 1 0.388571 0.084678 0.539313 11.00000 0.12098 0.07326 = 0.07633 -0.01152 -0.01756 0.03677 AFIX 43 H3 2 0.381879 0.098424 0.503095 11.00000 -1.20000 AFIX 0 C4 1 0.363229 0.084406 0.586718 11.00000 0.10522 0.09186 = 0.10309 -0.03973 0.00703 0.03129 AFIX 43 H4 2 0.338519 0.097669 0.583617 11.00000 -1.20000 AFIX 0 C5 1 0.373284 0.064587 0.640557 11.00000 0.09737 0.09690 = 0.09261 -0.02150 0.01619 0.03410 AFIX 43 H5 2 0.355474 0.064691 0.673949 11.00000 -1.20000 AFIX 0 C6 1 0.408650 0.045118 0.645110 11.00000 0.08365 0.07383 = 0.06875 -0.01386 -0.00499 0.02417 AFIX 43 H6 2 0.415596 0.031921 0.681694 11.00000 -1.20000 AFIX 0 C7 1 0.510796 0.049220 0.652433 11.00000 0.07899 0.07443 = 0.03473 -0.00328 -0.00074 -0.00893 C8 1 0.498424 0.087650 0.665200 11.00000 0.08703 0.07028 = 0.04444 -0.03274 -0.00507 0.00404 AFIX 43 H8 2 0.475972 0.098814 0.645676 11.00000 -1.20000 AFIX 0 C9 1 0.520077 0.108991 0.707430 11.00000 0.12482 0.05772 = 0.05940 -0.01322 0.02749 0.00803 AFIX 43 H9 2 0.511631 0.135011 0.717395 11.00000 -1.20000 AFIX 0 C10 1 0.553171 0.094204 0.735485 11.00000 0.08892 0.08139 = 0.06761 0.00334 -0.00042 -0.00689 AFIX 43 H10 2 0.567606 0.109860 0.763664 11.00000 -1.20000 AFIX 0 C11 1 0.564568 0.057818 0.722579 11.00000 0.08400 0.10566 = 0.04698 0.01743 -0.00520 -0.00248 AFIX 43 H11 2 0.587218 0.047180 0.742255 11.00000 -1.20000 AFIX 0 C12 1 0.543976 0.034550 0.680485 11.00000 0.07322 0.08597 = 0.05780 -0.00085 -0.01836 -0.00857 AFIX 43 H12 2 0.552979 0.008590 0.671335 11.00000 -1.20000 AFIX 0 C13 1 0.599022 0.018415 0.539709 11.00000 0.07102 0.04717 = 0.08000 -0.01918 -0.00627 0.00389 C14 1 0.635883 0.034074 0.531564 11.00000 0.06495 0.06545 = 0.12873 -0.00574 -0.01763 -0.00384 AFIX 43 H14 2 0.639909 0.056040 0.505345 11.00000 -1.20000 AFIX 0 C15 1 0.666609 0.017438 0.561904 11.00000 0.08512 0.09347 = 0.20345 0.02032 -0.04783 -0.00005 AFIX 43 H15 2 0.692574 0.027512 0.555980 11.00000 -1.20000 AFIX 0 C16 1 0.660822 -0.014005 0.601412 11.00000 0.09854 0.10528 = 0.22005 0.01439 -0.06079 0.03228 AFIX 43 H16 2 0.682752 -0.024175 0.623453 11.00000 -1.20000 AFIX 0 C17 1 0.624145 -0.030831 0.609484 11.00000 0.09945 0.09988 = 0.13158 -0.00858 -0.02916 0.02533 AFIX 43 H17 2 0.620393 -0.052470 0.636430 11.00000 -1.20000 AFIX 0 C18 1 0.592739 -0.014951 0.576676 11.00000 0.09929 0.07541 = 0.09521 -0.01395 -0.02325 0.00178 AFIX 43 H18 2 0.567193 -0.026578 0.579228 11.00000 -1.20000 AFIX 0 C19 1 0.548429 0.089261 0.532188 11.00000 0.08765 0.06023 = 0.05057 -0.00998 0.00443 0.01008 C20 1 0.575590 0.107038 0.572773 11.00000 0.08752 0.06959 = 0.05709 -0.00318 -0.00075 0.00282 AFIX 43 H20 2 0.597718 0.092410 0.587082 11.00000 -1.20000 AFIX 0 C21 1 0.570002 0.145600 0.591623 11.00000 0.11740 0.06827 = 0.06362 -0.01166 0.00066 -0.00148 AFIX 43 H21 2 0.588624 0.157739 0.618046 11.00000 -1.20000 AFIX 0 C22 1 0.537526 0.166343 0.572138 11.00000 0.17348 0.05421 = 0.08221 -0.00676 0.01077 0.01448 AFIX 43 H22 2 0.533306 0.192612 0.586090 11.00000 -1.20000 AFIX 0 C23 1 0.510299 0.148921 0.531459 11.00000 0.12775 0.07670 = 0.05850 -0.00022 0.00330 0.01401 AFIX 43 H23 2 0.488045 0.163469 0.517419 11.00000 -1.20000 AFIX 0 C24 1 0.516386 0.110710 0.512459 11.00000 0.09221 0.07215 = 0.06903 -0.00779 -0.00174 0.01050 AFIX 43 H24 2 0.498099 0.098886 0.485162 11.00000 -1.20000 AFIX 0 C25 1 0.464704 -0.096599 0.642562 11.00000 0.09239 0.07252 = 0.04941 -0.00245 -0.00890 -0.01690 C26 1 0.502000 -0.116324 0.637791 11.00000 0.06880 0.06722 = 0.04570 -0.00860 -0.01869 -0.00179 C27 1 0.505456 -0.155096 0.657871 11.00000 0.11542 0.04431 = 0.07023 -0.00868 -0.02754 0.00597 AFIX 43 H27 2 0.529881 -0.168780 0.653900 11.00000 -1.20000 AFIX 0 C28 1 0.472671 -0.173939 0.684054 11.00000 0.15757 0.05304 = 0.08657 0.00847 -0.02016 -0.03526 AFIX 43 H28 2 0.474676 -0.200887 0.695970 11.00000 -1.20000 AFIX 0 C29 1 0.437697 -0.154025 0.692737 11.00000 0.11187 0.08408 = 0.06373 -0.00711 -0.02379 -0.02158 AFIX 43 H29 2 0.416004 -0.166736 0.712053 11.00000 -1.20000 AFIX 0 C30 1 0.434356 -0.115329 0.673117 11.00000 0.09851 0.08106 = 0.05647 -0.02536 -0.00359 -0.01091 C31 1 0.396957 -0.094969 0.691042 11.00000 0.08026 0.08136 = 0.06382 -0.01595 0.00793 -0.01642 C32 1 0.476303 -0.026338 0.646444 11.00000 0.07338 0.07094 = 0.06297 -0.01307 -0.00826 -0.00033 AFIX 23 H32A 2 0.502433 -0.033683 0.663382 11.00000 -1.20000 H32B 2 0.458489 -0.020318 0.680932 11.00000 -1.20000 AFIX 0 C33 1 0.425768 -0.052105 0.576333 11.00000 0.06060 0.07721 = 0.07943 -0.01401 -0.00422 -0.00526 AFIX 23 H33A 2 0.410263 -0.029789 0.593152 11.00000 -1.20000 H33B 2 0.408695 -0.075909 0.575407 11.00000 -1.20000 AFIX 0 PART 1 CL2A 6 0.338009 0.000000 0.750000 20.50000 0.08301 0.11198 = 0.14542 -0.00794 0.00000 0.00000 PART 2 CL2B 6 0.319950 0.028488 0.789892 -20.50000 0.08301 0.11198 = 0.14542 -0.00794 0.00000 0.00000 PART 0 H1 2 0.553299 -0.106573 0.613228 11.00000 0.06032 HKLF 4 Covalent radii and connectivity table for s92 in I4(1)/acd C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 PD 1.380 Pd1 - P2_$1 P2 P1 P1_$1 Cl1 - no bonds found P1 - C1 C7 C32 Pd1 P2 - C13 C19 C33_$1 Pd1 N1 - C25 C32 C33 O1 - C26 O2 - C31 O3 - C31 C1 - C2 C6 P1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - C12 C8 P1 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C7 C11 C13 - C14 C18 P2 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 C19 - C24 C20 P2 C20 - C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C19 C25 - C30 N1 C26 C26 - O1 C27 C25 C27 - C26 C28 C28 - C29 C27 C29 - C28 C30 C30 - C25 C29 C31 C31 - O3 O2 C30 C32 - N1 P1 C33 - N1 P2_$1 Cl2A_a - no bonds found Cl2B_b - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 75488 Reflections read, of which 11678 rejected -40 =< h =< 40, -40 =< k =< 34, -26 =< l =< 26, Max. 2-theta = 50.05 0 Systematic absence violations 0 Inconsistent equivalents 5531 Unique reflections, of which 0 suppressed R(int) = 0.2781 R(sigma) = 0.1868 Friedel opposites merged Maximum memory for data reduction = 3770 / 75281 Special position constraints for Pd1 x = 0.5000 y = 0.0000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl1 z = 0.6250 y = 1.0 * x - 0.7500 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl2A_a y = 0.0000 z = 0.7500 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 4825 / 483362 wR2 = 0.2391 before cycle 1 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.202 OSF 2 0.60610 0.00871 0.019 FVAR 2 Mean shift/esd = 0.019 Maximum = 0.202 for OSF Max. shift = 0.005 A for H2 Max. dU =-0.001 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 2 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.039 OSF 2 0.60611 0.00871 0.002 FVAR 2 Mean shift/esd = 0.006 Maximum = 0.044 for U11 Pd1 Max. shift = 0.002 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 3 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.003 OSF 2 0.60611 0.00871 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.013 for x O1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 4 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.001 OSF 2 0.60611 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.010 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 5 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60611 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.008 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 6 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60611 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.007 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 7 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60610 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.006 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 8 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60610 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.005 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 9 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60610 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.004 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 10 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60610 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4825 / 483362 wR2 = 0.2391 before cycle 11 for 5531 data and 377 / 377 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.01381 0.00005 0.000 OSF 2 0.60610 0.00871 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Largest correlation matrix elements 0.992 y H1 / x H1 0.523 tors H2 / U13 O2 0.511 x C17 / x C16 Idealized hydrogen atom generation before cycle 12 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3764 -0.0466 0.6993 147 0.840 0.000 O2 C31 H2 H2A 0.4421 0.0652 0.5101 43 0.950 0.000 C2 C1 C3 H3 0.3819 0.0984 0.5031 43 0.950 0.000 C3 C4 C2 H4 0.3385 0.0977 0.5836 43 0.950 0.000 C4 C3 C5 H5 0.3555 0.0647 0.6740 43 0.950 0.000 C5 C6 C4 H6 0.4156 0.0319 0.6817 43 0.950 0.000 C6 C5 C1 H8 0.4760 0.0988 0.6457 43 0.950 0.000 C8 C9 C7 H9 0.5116 0.1350 0.7174 43 0.950 0.000 C9 C10 C8 H10 0.5676 0.1099 0.7637 43 0.950 0.000 C10 C11 C9 H11 0.5872 0.0471 0.7423 43 0.950 0.000 C11 C10 C12 H12 0.5530 0.0086 0.6713 43 0.950 0.000 C12 C7 C11 H14 0.6399 0.0560 0.5053 43 0.950 0.000 C14 C15 C13 H15 0.6926 0.0275 0.5560 43 0.950 0.000 C15 C14 C16 H16 0.6827 -0.0242 0.6235 43 0.950 0.000 C16 C17 C15 H17 0.6204 -0.0525 0.6364 43 0.950 0.000 C17 C16 C18 H18 0.5672 -0.0266 0.5792 43 0.950 0.000 C18 C17 C13 H20 0.5977 0.0924 0.5870 43 0.950 0.000 C20 C21 C19 H21 0.5886 0.1577 0.6180 43 0.950 0.000 C21 C22 C20 H22 0.5333 0.1926 0.5861 43 0.950 0.000 C22 C21 C23 H23 0.4880 0.1635 0.5174 43 0.950 0.000 C23 C24 C22 H24 0.4981 0.0989 0.4851 43 0.950 0.000 C24 C23 C19 H27 0.5299 -0.1688 0.6539 43 0.950 0.000 C27 C26 C28 H28 0.4746 -0.2009 0.6959 43 0.950 0.000 C28 C29 C27 H29 0.4160 -0.1667 0.7121 43 0.950 0.000 C29 C28 C30 H32A 0.5024 -0.0337 0.6634 23 0.990 0.000 C32 N1 P1 H32B 0.4585 -0.0203 0.6809 23 0.990 0.000 C32 N1 P1 H33A 0.4102 -0.0298 0.5931 23 0.990 0.000 C33 N1 P2_$1 H33B 0.4087 -0.0759 0.5754 23 0.990 0.000 C33 N1 P2_$1 s92 in I4(1)/acd ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Pd1 0.50000 0.00000 0.50000 0.50000 0.06857 0.05184 0.04921 -0.01022 -0.00269 0.00350 0.05654 0.00000 0.00000 0.00000 0.00000 0.00000 0.00075 0.00066 0.00054 0.00059 0.00062 0.00063 0.00035 Cl1 0.61018 -0.13982 0.62500 0.50000 0.08143 0.08143 0.08883 -0.00229 0.00229 0.03115 0.08390 0.00680 0.00010 0.00010 0.00000 0.00000 0.00184 0.00184 0.00299 0.00152 0.00152 0.00231 0.00129 P1 0.48199 0.01866 0.59928 1.00000 0.08011 0.05538 0.05255 -0.00921 -0.00115 0.00757 0.06268 0.00478 0.00009 0.00008 0.00012 0.00000 0.00211 0.00176 0.00154 0.00143 0.00150 0.00145 0.00078 P2 0.55669 0.04009 0.50091 1.00000 0.07462 0.05694 0.05529 -0.01038 -0.00322 -0.00402 0.06228 0.00468 0.00008 0.00008 0.00013 0.00000 0.00181 0.00162 0.00149 0.00152 0.00159 0.00146 0.00077 N1 0.46067 -0.05936 0.61348 1.00000 0.07846 0.05544 0.05182 0.00210 -0.00227 -0.01419 0.06191 0.01433 0.00026 0.00025 0.00036 0.00000 0.00652 0.00591 0.00506 0.00455 0.00481 0.00484 0.00230 O1 0.53124 -0.09515 0.61331 1.00000 0.06468 0.07251 0.07403 0.00794 -0.00224 0.00049 0.07041 0.01118 0.00012 0.00023 0.00034 0.00000 0.00567 0.00556 0.00528 0.00418 0.00459 0.00490 0.00199 O2 0.39925 -0.05626 0.69866 1.00000 0.07760 0.11350 0.08089 -0.00694 0.01050 0.00351 0.09066 0.01584 0.00023 0.00030 0.00038 0.00000 0.00579 0.00766 0.00575 0.00532 0.00491 0.00523 0.00249 H2 0.37636 -0.04658 0.69929 1.00000 0.13600 0.00000 0.00000 O3 0.36679 -0.11256 0.70169 1.00000 0.09202 0.15229 0.11078 -0.01845 0.00641 -0.04055 0.11836 0.01692 0.00030 0.00033 0.00041 0.00000 0.00697 0.00879 0.00730 0.00628 0.00582 0.00672 0.00331 C1 0.43470 0.04478 0.59515 1.00000 0.07303 0.06411 0.05693 -0.01834 -0.00037 -0.00553 0.06469 0.01705 0.00032 0.00032 0.00052 0.00000 0.00756 0.00724 0.00683 0.00624 0.00646 0.00596 0.00290 C2 0.42437 0.06486 0.54362 1.00000 0.09270 0.07099 0.06695 -0.01092 0.00035 0.01671 0.07688 0.01934 0.00038 0.00034 0.00056 0.00000 0.00981 0.00809 0.00825 0.00676 0.00710 0.00710 0.00337 H2A 0.44208 0.06523 0.51010 1.00000 0.09225 0.00000 0.00000 C3 0.38858 0.08469 0.53930 1.00000 0.12059 0.07330 0.07669 -0.01151 -0.01743 0.03663 0.09019 0.02151 0.00046 0.00036 0.00062 0.00000 0.01129 0.00867 0.00902 0.00723 0.00910 0.00835 0.00392 H3 0.38189 0.09842 0.50307 1.00000 0.10823 0.00000 0.00000 C4 0.36323 0.08444 0.58670 1.00000 0.10529 0.09175 0.10327 -0.03978 0.00695 0.03128 0.10010 0.02303 0.00043 0.00041 0.00079 0.00000 0.01127 0.01051 0.01113 0.00935 0.01001 0.00821 0.00437 H4 0.33853 0.09772 0.58360 1.00000 0.12012 0.00000 0.00000 C5 0.37329 0.06459 0.64058 1.00000 0.09777 0.09655 0.09275 -0.02158 0.01615 0.03449 0.09569 0.02356 0.00042 0.00040 0.00070 0.00000 0.01095 0.01004 0.01073 0.00867 0.00863 0.00844 0.00413 H5 0.35549 0.06469 0.67398 1.00000 0.11483 0.00000 0.00000 C6 0.40864 0.04513 0.64509 1.00000 0.08402 0.07383 0.06846 -0.01377 -0.00523 0.02425 0.07543 0.01866 0.00036 0.00033 0.00053 0.00000 0.00888 0.00820 0.00806 0.00637 0.00701 0.00709 0.00334 H6 0.41559 0.03192 0.68167 1.00000 0.09052 0.00000 0.00000 C7 0.51080 0.04921 0.65242 1.00000 0.07868 0.07450 0.03479 -0.00344 -0.00072 -0.00856 0.06265 0.01753 0.00033 0.00033 0.00042 0.00000 0.00868 0.00799 0.00544 0.00542 0.00556 0.00612 0.00300 C8 0.49841 0.08765 0.66519 1.00000 0.08708 0.07030 0.04447 -0.03253 -0.00524 0.00399 0.06728 0.01775 0.00035 0.00032 0.00041 0.00000 0.00792 0.00755 0.00583 0.00552 0.00605 0.00696 0.00290 H8 0.47596 0.09882 0.64567 1.00000 0.08074 0.00000 0.00000 C9 0.52007 0.10898 0.70744 1.00000 0.12508 0.05782 0.05958 -0.01336 0.02781 0.00735 0.08083 0.02380 0.00045 0.00034 0.00052 0.00000 0.01150 0.00757 0.00737 0.00633 0.00791 0.00762 0.00361 H9 0.51163 0.13499 0.71742 1.00000 0.09699 0.00000 0.00000 C10 0.55319 0.09420 0.73549 1.00000 0.08841 0.08210 0.06779 0.00352 -0.00046 -0.00669 0.07943 0.02307 0.00041 0.00045 0.00054 0.00000 0.00985 0.00963 0.00833 0.00748 0.00725 0.00812 0.00352 H10 0.56763 0.10986 0.76366 1.00000 0.09532 0.00000 0.00000 C11 0.56457 0.05779 0.72258 1.00000 0.08379 0.10555 0.04712 0.01760 -0.00471 -0.00204 0.07882 0.02288 0.00036 0.00045 0.00049 0.00000 0.00895 0.01108 0.00629 0.00713 0.00630 0.00836 0.00352 H11 0.58721 0.04713 0.74226 1.00000 0.09458 0.00000 0.00000 C12 0.54396 0.03454 0.68046 1.00000 0.07326 0.08585 0.05749 -0.00126 -0.01846 -0.00869 0.07220 0.01872 0.00034 0.00035 0.00047 0.00000 0.00808 0.00858 0.00658 0.00639 0.00646 0.00674 0.00318 H12 0.55296 0.00858 0.67130 1.00000 0.08664 0.00000 0.00000 C13 0.59901 0.01841 0.53971 1.00000 0.07135 0.04748 0.07998 -0.01905 -0.00613 0.00391 0.06627 0.01861 0.00036 0.00035 0.00051 0.00000 0.00858 0.00670 0.00778 0.00663 0.00658 0.00630 0.00302 C14 0.63589 0.03407 0.53156 1.00000 0.06497 0.06515 0.12899 -0.00539 -0.01779 -0.00365 0.08637 0.02078 0.00039 0.00035 0.00062 0.00000 0.00848 0.00817 0.01080 0.00754 0.00809 0.00734 0.00373 H14 0.63992 0.05604 0.50534 1.00000 0.10365 0.00000 0.00000 C15 0.66661 0.01744 0.56191 1.00000 0.08526 0.09325 0.20299 0.01993 -0.04751 -0.00025 0.12716 0.02633 0.00047 0.00051 0.00084 0.00000 0.01141 0.01126 0.01806 0.01208 0.01137 0.00936 0.00595 H15 0.69257 0.02750 0.55597 1.00000 0.15260 0.00000 0.00000 C16 0.66082 -0.01402 0.60146 1.00000 0.09812 0.10596 0.21935 0.01462 -0.06034 0.03201 0.14114 0.03200 0.00057 0.00056 0.00097 0.00000 0.01377 0.01315 0.02044 0.01347 0.01371 0.01061 0.00682 H16 0.68275 -0.02418 0.62353 1.00000 0.16937 0.00000 0.00000 C17 0.62417 -0.03084 0.60950 1.00000 0.09971 0.09965 0.13118 -0.00832 -0.02928 0.02576 0.11018 0.02817 0.00053 0.00044 0.00070 0.00000 0.01208 0.01147 0.01261 0.00938 0.01064 0.00996 0.00476 H17 0.62042 -0.05249 0.63643 1.00000 0.13222 0.00000 0.00000 C18 0.59275 -0.01496 0.57667 1.00000 0.09944 0.07553 0.09501 -0.01432 -0.02264 0.00165 0.08999 0.02131 0.00042 0.00040 0.00060 0.00000 0.01079 0.00919 0.00958 0.00816 0.00862 0.00803 0.00390 H18 0.56720 -0.02659 0.57922 1.00000 0.10799 0.00000 0.00000 C19 0.54843 0.08926 0.53219 1.00000 0.08722 0.06037 0.05047 -0.01020 0.00416 0.00993 0.06602 0.02015 0.00036 0.00032 0.00047 0.00000 0.00868 0.00703 0.00644 0.00576 0.00637 0.00696 0.00297 C20 0.57558 0.10705 0.57275 1.00000 0.08799 0.06947 0.05717 -0.00303 -0.00062 0.00300 0.07154 0.02115 0.00035 0.00036 0.00048 0.00000 0.00885 0.00861 0.00679 0.00650 0.00659 0.00668 0.00313 H20 0.59772 0.09243 0.58705 1.00000 0.08585 0.00000 0.00000 C21 0.56999 0.14560 0.59162 1.00000 0.11777 0.06826 0.06342 -0.01167 0.00059 -0.00118 0.08315 0.02218 0.00043 0.00040 0.00051 0.00000 0.01125 0.00921 0.00771 0.00713 0.00751 0.00823 0.00356 H21 0.58862 0.15774 0.61804 1.00000 0.09978 0.00000 0.00000 C22 0.53750 0.16634 0.57215 1.00000 0.17330 0.05443 0.08182 -0.00684 0.01091 0.01453 0.10318 0.02955 0.00056 0.00039 0.00062 0.00000 0.01553 0.00835 0.00936 0.00747 0.01038 0.00982 0.00464 H22 0.53326 0.19260 0.58613 1.00000 0.12382 0.00000 0.00000 C23 0.51030 0.14893 0.53146 1.00000 0.12821 0.07664 0.05844 -0.00026 0.00317 0.01396 0.08776 0.02614 0.00043 0.00041 0.00053 0.00000 0.01194 0.00922 0.00727 0.00701 0.00773 0.00840 0.00384 H23 0.48805 0.16348 0.51741 1.00000 0.10532 0.00000 0.00000 C24 0.51639 0.11071 0.51243 1.00000 0.09231 0.07211 0.06917 -0.00785 -0.00179 0.01046 0.07786 0.02176 0.00038 0.00038 0.00050 0.00000 0.00893 0.00842 0.00792 0.00677 0.00673 0.00691 0.00333 H24 0.49811 0.09890 0.48510 1.00000 0.09344 0.00000 0.00000 C25 0.46471 -0.09660 0.64256 1.00000 0.09230 0.07244 0.04935 -0.00245 -0.00883 -0.01686 0.07136 0.01835 0.00043 0.00036 0.00048 0.00000 0.01000 0.00880 0.00697 0.00634 0.00680 0.00799 0.00313 C26 0.50201 -0.11631 0.63778 1.00000 0.06929 0.06708 0.04568 -0.00875 -0.01886 -0.00133 0.06068 0.01732 0.00039 0.00032 0.00043 0.00000 0.00796 0.00748 0.00591 0.00550 0.00630 0.00779 0.00273 C27 0.50544 -0.15510 0.65785 1.00000 0.11561 0.04443 0.07047 -0.00888 -0.02770 0.00619 0.07684 0.01907 0.00044 0.00032 0.00049 0.00000 0.01109 0.00695 0.00736 0.00596 0.00752 0.00740 0.00359 H27 0.52986 -0.16880 0.65386 1.00000 0.09220 0.00000 0.00000 C28 0.47263 -0.17394 0.68404 1.00000 0.15786 0.05330 0.08643 0.00851 -0.02028 -0.03548 0.09920 0.02212 0.00062 0.00041 0.00059 0.00000 0.01557 0.00853 0.00942 0.00713 0.01017 0.01054 0.00460 H28 0.47462 -0.20090 0.69593 1.00000 0.11904 0.00000 0.00000 C29 0.43769 -0.15403 0.69276 1.00000 0.11151 0.08483 0.06325 -0.00745 -0.02348 -0.02156 0.08653 0.01966 0.00050 0.00048 0.00052 0.00000 0.01236 0.01126 0.00810 0.00758 0.00783 0.00929 0.00383 H29 0.41601 -0.16672 0.71214 1.00000 0.10384 0.00000 0.00000 C30 0.43434 -0.11531 0.67309 1.00000 0.09875 0.08077 0.05657 -0.02530 -0.00349 -0.01106 0.07870 0.01913 0.00041 0.00043 0.00052 0.00000 0.01099 0.01023 0.00765 0.00731 0.00748 0.00862 0.00362 C31 0.39695 -0.09497 0.69103 1.00000 0.08000 0.08177 0.06362 -0.01605 0.00797 -0.01616 0.07513 0.02283 0.00043 0.00045 0.00050 0.00000 0.01049 0.01040 0.00732 0.00686 0.00678 0.00880 0.00340 C32 0.47631 -0.02634 0.64644 1.00000 0.07307 0.07095 0.06283 -0.01314 -0.00827 -0.00030 0.06895 0.01719 0.00031 0.00030 0.00047 0.00000 0.00750 0.00769 0.00674 0.00616 0.00582 0.00604 0.00300 H32A 0.50244 -0.03368 0.66337 1.00000 0.08274 0.00000 0.00000 H32B 0.45850 -0.02031 0.68093 1.00000 0.08274 0.00000 0.00000 C33 0.42575 -0.05210 0.57632 1.00000 0.06058 0.07699 0.07965 -0.01364 -0.00437 -0.00507 0.07241 0.01894 0.00032 0.00035 0.00048 0.00000 0.00725 0.00809 0.00775 0.00651 0.00649 0.00592 0.00315 H33A 0.41024 -0.02979 0.59313 1.00000 0.08689 0.00000 0.00000 H33B 0.40868 -0.07591 0.57539 1.00000 0.08689 0.00000 0.00000 Cl2A_a 0.33800 0.00000 0.75000 0.30305 0.08332 0.11205 0.14564 -0.00795 0.00000 0.00000 0.11367 0.00815 0.00024 0.00000 0.00000 0.00436 0.00533 0.00653 0.00731 0.00526 0.00000 0.00000 0.00275 Cl2B_b 0.31995 0.02849 0.78993 0.19695 0.08332 0.11205 0.14564 -0.00795 0.00000 0.00000 0.11367 0.03377 0.00054 0.00059 0.00097 0.00436 0.00533 0.00653 0.00731 0.00526 0.00000 0.00000 0.00275 H1 0.55336 -0.10648 0.61341 1.00000 0.06022 0.15478 0.00126 0.00239 0.00435 0.00000 0.03195 Final Structure Factor Calculation for s92 in I4(1)/acd Total number of l.s. parameters = 377 Maximum vector length = 511 Memory required = 4448 / 26061 wR2 = 0.2391 before cycle 12 for 5531 data and 0 / 377 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.920; Restrained GooF = 0.920 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1041 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0801 for 1784 Fo > 4sig(Fo) and 0.2565 for all 5531 data wR2 = 0.2391, GooF = S = 0.920, Restrained GooF = 0.920 for all data Occupancy sum of asymmetric unit = 40.50 for non-hydrogen and 29.00 for hydrogen atoms Principal mean square atomic displacements U 0.0706 0.0588 0.0402 Pd1 0.1126 0.0891 0.0500 Cl1 0.0827 0.0612 0.0442 P1 0.0756 0.0665 0.0448 P2 0.0855 0.0518 0.0484 N1 0.0814 0.0668 0.0630 O1 0.1150 0.0895 0.0675 O2 0.1782 0.1054 0.0714 O3 0.0813 0.0714 0.0414 C1 0.1025 0.0740 0.0542 C2 0.1467 0.0707 0.0532 C3 0.1452 0.1113 0.0438 C4 0.1321 0.1080 0.0470 C5 0.1079 0.0679 0.0505 C6 0.0855 0.0681 0.0344 C7 0.0965 0.0830 0.0223 C8 0.1354 0.0692 0.0379 C9 0.0929 0.0785 0.0669 C10 0.1108 0.0838 0.0418 C11 0.0926 0.0796 0.0445 C12 0.0914 0.0688 0.0387 C13 0.1339 0.0680 0.0572 C14 0.2225 0.0922 0.0668 C15 0.2443 0.1284 0.0508 C16 0.1566 0.1045 0.0695 C17 0.1226 0.0830 0.0644 C18 0.0905 0.0653 0.0423 C19 0.0885 0.0697 0.0565 C20 0.1178 0.0777 0.0539 C21 0.1761 0.0829 0.0505 C22 0.1319 0.0732 0.0582 C23 0.0976 0.0745 0.0616 C24 0.1027 0.0653 0.0461 C25 0.0805 0.0683 0.0332 C26 0.1298 0.0591 0.0416 C27 0.1742 0.0811 0.0423 C28 0.1283 0.0842 0.0470 C29 0.1060 0.0908 0.0393 C30 0.1044 0.0668 0.0542 C31 0.0832 0.0727 0.0510 C32 0.0920 0.0696 0.0556 C33 0.1474 0.1103 0.0833 Cl2A_a 0.1474 0.1103 0.0833 Cl2B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.014 0.019 0.027 0.036 0.051 0.075 0.127 1.000 Number in group 647. 510. 567. 497. 609. 517. 544. 533. 549. 558. GooF 0.840 0.795 0.829 0.907 0.901 0.897 0.890 1.057 1.005 1.051 K 28.452 3.744 2.029 2.072 1.610 1.068 1.059 1.048 1.033 1.022 Resolution(A) 0.84 0.87 0.91 0.95 0.99 1.06 1.14 1.25 1.43 1.79 inf Number in group 565. 561. 534. 551. 559. 548. 559. 554. 549. 551. GooF 0.897 0.792 0.881 0.909 0.868 0.921 0.946 0.847 0.820 1.245 K 2.081 1.372 1.264 1.232 1.090 1.025 0.982 0.969 0.975 1.039 R1 0.633 0.574 0.493 0.444 0.344 0.268 0.211 0.141 0.089 0.073 Recommended weighting scheme: WGHT 0.1036 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 8 3 60929.10 107947.79 5.47 0.259 3.64 1 10 1 54003.77 35491.71 4.67 0.148 3.32 1 8 1 47341.41 31143.09 4.62 0.139 4.12 1 12 3 15556.54 8185.48 4.59 0.071 2.62 4 7 3 105432.42 70524.42 4.55 0.209 3.64 3 7 2 85011.66 57005.62 4.50 0.188 4.11 5 8 3 54245.70 36296.59 4.43 0.150 3.22 5 6 3 83714.05 56836.52 4.36 0.188 3.73 2 6 2 85450.49 60138.73 3.94 0.193 4.81 5 10 3 27029.79 18120.92 3.93 0.106 2.79 9 9 10 6670.66 523.66 3.89 0.018 1.69 3 6 3 587085.44 416015.94 3.87 0.508 4.15 4 5 3 11112.59 30566.37 3.59 0.138 4.28 3 5 2 22015.51 4402.48 3.54 0.052 5.13 1 9 2 16935.63 8351.58 3.53 0.072 3.53 2 6 0 143922.67 204498.73 3.52 0.356 5.34 2 6 6 21063.36 14146.38 3.38 0.094 3.02 20 26 14 18789.11 5858.32 3.35 0.060 0.86 2 12 0 9458.70 17088.98 3.33 0.103 2.78 7 13 14 5963.83 1501.75 3.30 0.031 1.30 11 31 8 7027.62 486.09 3.29 0.017 0.96 1 10 5 31388.42 22844.35 3.23 0.119 2.67 4 28 12 -1708.20 5667.44 3.22 0.059 1.00 0 36 0 17360.13 5576.61 3.19 0.059 0.94 6 11 5 10139.74 61.01 3.15 0.006 2.30 3 4 3 287177.28 390277.81 3.12 0.492 4.97 12 28 12 19516.44 10783.02 3.11 0.082 0.95 14 22 2 4356.58 141.56 3.10 0.009 1.29 1 20 9 7402.30 2810.07 3.10 0.042 1.39 8 9 19 5571.80 11373.37 3.10 0.084 1.07 1 3 22 4660.91 3.57 3.09 0.001 1.00 2 13 1 15227.56 10249.31 3.07 0.080 2.55 1 10 7 20778.46 14740.96 3.05 0.096 2.30 17 35 6 9998.32 218.59 2.99 0.012 0.85 21 25 2 6475.34 12.03 2.92 0.003 1.03 1 2 19 4237.10 8680.14 2.89 0.073 1.16 2 12 6 33221.98 25117.91 2.88 0.125 2.21 0 34 6 46921.57 28774.96 2.88 0.134 0.96 15 16 11 1789.82 5596.57 2.87 0.059 1.22 2 4 4 31611.21 22672.33 2.87 0.119 4.45 9 13 2 10784.57 6829.00 2.86 0.065 2.10 1 30 15 7756.45 260.29 2.85 0.013 0.89 0 10 0 19714.16 9257.63 2.85 0.076 3.38 22 32 2 15018.28 7196.08 2.82 0.067 0.87 12 26 0 5543.02 322.40 2.80 0.014 1.18 0 4 2 104967.69 138179.69 2.80 0.293 6.70 4 7 5 6364.94 1145.41 2.77 0.027 3.04 12 22 18 2563.28 11247.05 2.76 0.084 0.91 14 34 2 8090.98 521.36 2.75 0.018 0.92 13 16 13 846.11 4863.90 2.75 0.055 1.18 Bond lengths and angles Pd1 - Distance Angles P2_$1 2.3461 (0.0028) P2 2.3461 (0.0028) 180.00 (0.20) P1 2.3547 (0.0027) 87.22 (0.10) 92.78 (0.10) P1_$1 2.3547 (0.0027) 92.78 (0.10) 87.22 (0.10) 180.00 (0.05) Pd1 - P2_$1 P2 P1 P1 - Distance Angles C1 1.8276 (0.0114) C7 1.8386 (0.0105) 102.92 (0.50) C32 1.8511 (0.0107) 109.49 (0.52) 99.16 (0.48) Pd1 2.3547 (0.0027) 108.00 (0.37) 127.16 (0.34) 109.11 (0.34) P1 - C1 C7 C32 P2 - Distance Angles C13 1.8193 (0.0118) C19 1.8200 (0.0110) 108.08 (0.53) C33_$1 1.8458 (0.0110) 105.57 (0.54) 101.36 (0.52) Pd1 2.3461 (0.0028) 114.41 (0.43) 113.89 (0.40) 112.43 (0.36) P2 - C13 C19 C33_$1 N1 - Distance Angles C25 1.4183 (0.0132) C32 1.4319 (0.0116) 115.28 (0.81) C33 1.4564 (0.0124) 118.73 (0.88) 116.89 (0.87) N1 - C25 C32 O1 - Distance Angles C26 1.3329 (0.0125) H1 0.8400 (0.0005) 114.43 (6.65) O1 - C26 O2 - Distance Angles C31 1.3211 (0.0132) H2 0.8400 109.47 O2 - C31 O3 - Distance Angles C31 1.2027 (0.0134) O3 - C1 - Distance Angles C2 1.3671 (0.0146) C6 1.4086 (0.0143) 118.95 (1.06) P1 1.8276 (0.0114) 120.27 (0.89) 120.77 (0.91) C1 - C2 C6 C2 - Distance Angles C1 1.3671 (0.0145) C3 1.3859 (0.0155) 121.30 (1.17) H2A 0.9500 119.35 119.35 C2 - C1 C3 C3 - Distance Angles C4 1.3499 (0.0168) C2 1.3859 (0.0156) 119.85 (1.25) H3 0.9500 120.07 120.07 C3 - C4 C2 C4 - Distance Angles C3 1.3499 (0.0169) C5 1.4045 (0.0172) 120.13 (1.28) H4 0.9500 119.93 119.93 C4 - C3 C5 C5 - Distance Angles C6 1.3671 (0.0150) C4 1.4045 (0.0172) 120.18 (1.26) H5 0.9500 119.91 119.91 C5 - C6 C4 C6 - Distance Angles C5 1.3671 (0.0150) C1 1.4086 (0.0143) 119.56 (1.15) H6 0.9500 120.22 120.22 C6 - C5 C1 C7 - Distance Angles C12 1.3720 (0.0137) C8 1.3933 (0.0135) 119.42 (0.99) P1 1.8386 (0.0105) 121.06 (0.88) 119.51 (0.84) C7 - C12 C8 C8 - Distance Angles C9 1.3857 (0.0151) C7 1.3933 (0.0135) 117.48 (1.09) H8 0.9500 121.26 121.26 C8 - C9 C7 C9 - Distance Angles C10 1.3721 (0.0159) C8 1.3857 (0.0150) 122.93 (1.13) H9 0.9500 118.53 118.53 C9 - C10 C8 C10 - Distance Angles C11 1.3198 (0.0153) C9 1.3721 (0.0159) 118.68 (1.22) H10 0.9500 120.66 120.66 C10 - C11 C9 C11 - Distance Angles C10 1.3198 (0.0153) C12 1.4005 (0.0151) 121.36 (1.19) H11 0.9500 119.32 119.32 C11 - C10 C12 C12 - Distance Angles C7 1.3720 (0.0136) C11 1.4005 (0.0152) 120.10 (1.14) H12 0.9500 119.95 119.95 C12 - C7 C11 C13 - Distance Angles C14 1.3656 (0.0151) C18 1.4064 (0.0154) 121.59 (1.18) P2 1.8193 (0.0118) 119.97 (1.03) 118.43 (1.00) C13 - C14 C18 C14 - Distance Angles C15 1.3563 (0.0175) C13 1.3656 (0.0151) 118.23 (1.34) H14 0.9500 120.88 120.88 C14 - C15 C13 C15 - Distance Angles C14 1.3563 (0.0175) C16 1.3879 (0.0211) 121.24 (1.51) H15 0.9500 119.38 119.38 C15 - C14 C16 C16 - Distance Angles C17 1.3739 (0.0204) C15 1.3879 (0.0211) 121.63 (1.51) H16 0.9500 119.18 119.18 C16 - C17 C15 C17 - Distance Angles C16 1.3739 (0.0205) C18 1.3920 (0.0169) 117.47 (1.55) H17 0.9500 121.27 121.27 C17 - C16 C18 C18 - Distance Angles C17 1.3920 (0.0169) C13 1.4064 (0.0154) 119.65 (1.35) H18 0.9500 120.17 120.17 C18 - C17 C13 C19 - Distance Angles C24 1.3737 (0.0146) C20 1.4143 (0.0142) 119.14 (1.05) P2 1.8200 (0.0110) 118.87 (0.93) 121.83 (0.93) C19 - C24 C20 C20 - Distance Angles C21 1.3802 (0.0151) C19 1.4143 (0.0142) 120.15 (1.13) H20 0.9500 119.92 119.92 C20 - C21 C19 C21 - Distance Angles C22 1.3712 (0.0173) C20 1.3802 (0.0151) 119.86 (1.23) H21 0.9500 120.07 120.07 C21 - C22 C20 C22 - Distance Angles C21 1.3712 (0.0173) C23 1.4118 (0.0178) 120.44 (1.21) H22 0.9500 119.78 119.78 C22 - C21 C23 C23 - Distance Angles C24 1.3729 (0.0154) C22 1.4118 (0.0178) 119.21 (1.26) H23 0.9500 120.40 120.40 C23 - C24 C22 C24 - Distance Angles C23 1.3729 (0.0155) C19 1.3737 (0.0146) 121.18 (1.19) H24 0.9500 119.41 119.41 C24 - C23 C19 C25 - Distance Angles C30 1.3798 (0.0159) N1 1.4183 (0.0132) 123.69 (1.28) C26 1.4295 (0.0151) 118.55 (1.17) 117.71 (1.09) C25 - C30 N1 C26 - Distance Angles O1 1.3329 (0.0125) C27 1.3879 (0.0137) 124.99 (1.20) C25 1.4295 (0.0151) 115.65 (0.96) 119.36 (1.19) C26 - O1 C27 C27 - Distance Angles C26 1.3879 (0.0137) C28 1.4024 (0.0179) 119.57 (1.31) H27 0.9500 120.21 120.21 C27 - C26 C28 C28 - Distance Angles C29 1.3724 (0.0186) C27 1.4024 (0.0179) 120.99 (1.31) H28 0.9500 119.51 119.51 C28 - C29 C27 C29 - Distance Angles C28 1.3724 (0.0186) C30 1.3827 (0.0167) 119.38 (1.38) H29 0.9500 120.31 120.31 C29 - C28 C30 C30 - Distance Angles C25 1.3798 (0.0159) C29 1.3827 (0.0167) 121.68 (1.32) C31 1.4915 (0.0174) 123.21 (1.34) 114.98 (1.40) C30 - C25 C29 C31 - Distance Angles O3 1.2027 (0.0133) O2 1.3211 (0.0132) 120.96 (1.31) C30 1.4915 (0.0174) 122.79 (1.36) 116.10 (1.21) C31 - O3 O2 C32 - Distance Angles N1 1.4319 (0.0116) P1 1.8511 (0.0107) 113.21 (0.70) H32A 0.9900 108.93 108.93 H32B 0.9900 108.93 108.93 107.75 C32 - N1 P1 H32A C33 - Distance Angles N1 1.4564 (0.0124) P2_$1 1.8458 (0.0110) 107.10 (0.68) H33A 0.9900 110.30 110.30 H33B 0.9900 110.30 110.30 108.55 C33 - N1 P2_$1 H33A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) ** No suitable H-bond found for O2...Cl2B_b = 4.41(2) A ** 0.84 2.32 3.029(10) 141.7 O2-H2...Cl2A_a 0.84 2.240(13) 3.076(5) 173(9) O1-H1...Cl1 FMAP and GRID set by program FMAP 2 3 -14 GRID -1.136 -1 -1 1.136 1 1 R1 = 0.2556 for 5531 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.7165 0.9888 0.0945 [ 2.33 A from CL2B ] Deepest hole -0.33 at 0.5007 0.9705 0.0932 [ 1.41 A from C32 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 6101 / 89359 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2612 0.0335 0.8445 1.00000 0.05 0.57 2.33 CL2B 2.89 CL2B 3.20 H15 3.23 H15 Q2 1 0.6956 0.0074 0.7458 1.00000 0.05 0.57 2.93 H16 2.96 H16 3.46 C16 3.50 H15 Q3 1 0.4621 -0.0011 0.4994 1.00000 0.05 0.54 1.28 PD1 1.46 P2 2.20 H18 2.31 C13 Q4 1 0.4928 0.0303 0.5002 1.00000 0.05 0.44 1.05 PD1 2.09 H2A 2.18 P2 2.25 P1 Q5 1 0.5197 0.0210 0.5944 1.00000 0.05 0.41 1.28 P1 1.62 C7 2.08 H12 2.12 C12 Q6 1 0.4785 -0.0072 0.4644 1.00000 0.05 0.39 1.10 PD1 1.80 P2 1.97 P1 2.15 H18 Q7 1 0.7364 0.0233 0.6814 1.00000 0.05 0.37 2.74 H16 2.90 CL2B 3.07 H15 3.14 H15 Q8 1 0.4462 0.0421 0.5008 1.00000 0.05 0.31 0.82 H2A 1.42 C2 1.89 H18 2.12 C1 Q9 1 0.3896 -0.1396 0.6250 0.50000 0.05 0.30 2.02 C30 2.07 O3 2.11 C31 2.26 C29 Q10 1 0.5899 -0.1601 0.6250 0.50000 0.05 0.29 0.97 CL1 2.15 H27 2.21 H1 2.95 C27 Shortest distances between peaks (including symmetry equivalents) 2 2 0.53 3 6 0.97 1 7 1.07 5 6 1.38 4 6 1.47 3 4 1.48 3 8 1.55 4 6 1.57 4 8 1.62 1 1 1.72 3 4 1.81 2 7 2.05 4 4 2.10 6 8 2.15 3 6 2.18 6 6 2.19 3 5 2.26 4 5 2.29 2 7 2.35 1 7 2.52 3 3 2.56 4 5 2.74 6 8 2.91 3 5 2.95 Time profile in seconds ----------------------- 0.14: Read and process instructions 0.00: Fit rigid groups 0.00: 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 0.00: Analyse other restraints etc. 4.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 23.48: Structure factors and derivatives 19.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 1.89: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.13: Merge reflections for Fourier and .fcf 0.34: Fourier summations 1.14: Peaksearch 0.03: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:56:32 Total CPU time: 52.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++