+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0060p-1 started at 10:25:18 on 09-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0060p-1 in P-1 CELL 0.71073 7.2550 8.1110 16.9310 80.408 78.681 89.674 ZERR 1.00 0.0002 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H O S LA W UNIT 20 20 32 4 4 4 V = 962.90 F(000) = 984.0 Mu = 16.56 mm-1 Cell Wt = 2191.64 Rho = 3.780 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 ISOR 0.005 O32 O36 O23 FMAP 2 PLAN 10 SIZE 0.01 0.03 0.14 ACTA BOND WGHT 0.00000 23.95970 L.S. 8 TEMP -153.00 FVAR 0.19500 MOLE 1 C1 1 -0.324288 -0.038584 0.088179 11.00000 0.02051 0.01957 = 0.01547 -0.00470 -0.00012 -0.00036 AFIX 43 H1 2 -0.453085 -0.031638 0.112565 11.00000 -1.20000 AFIX 0 C2 1 -0.208336 -0.151475 0.126051 11.00000 0.02206 0.00755 = 0.01309 -0.00493 -0.00350 -0.00407 C3 1 -0.020653 -0.158588 0.095914 11.00000 0.02119 0.01288 = 0.00555 -0.00176 -0.00339 0.00053 AFIX 43 H3 2 0.056005 -0.231192 0.124809 11.00000 -1.20000 AFIX 0 C4 1 0.058793 -0.055496 0.020435 11.00000 0.01630 0.01141 = 0.01231 -0.00239 -0.00784 -0.00324 C5 1 -0.250820 0.059897 0.016798 11.00000 0.01784 0.02361 = 0.02171 -0.01040 -0.00422 0.00952 AFIX 43 H5 2 -0.330317 0.134582 -0.009352 11.00000 -1.20000 AFIX 0 O1 3 -0.161950 -0.382543 0.247076 11.00000 0.01200 0.01615 = 0.00865 -0.00445 -0.00110 -0.00022 O2 3 -0.396493 -0.176008 0.275584 11.00000 0.01566 0.01597 = 0.01002 -0.00392 -0.00026 -0.00030 O3 3 -0.452483 -0.389177 0.197954 11.00000 0.00995 0.01956 = 0.01120 -0.00712 0.00275 -0.00316 S1 4 -0.312503 -0.284333 0.217881 11.00000 0.00967 0.01152 = 0.01061 -0.00273 -0.00193 -0.00112 MOLE 2 C21 1 0.248466 -0.648417 0.068847 11.00000 0.01865 0.01130 = 0.01108 0.00005 -0.00907 0.00216 AFIX 43 H21 2 0.360355 -0.694461 0.083310 11.00000 -1.20000 AFIX 0 C22 1 0.072773 -0.684181 0.123799 11.00000 0.00632 0.00849 = 0.01101 -0.00048 0.00528 0.00004 C23 1 -0.090652 -0.624560 0.104176 11.00000 0.01308 0.01274 = 0.01249 -0.00193 -0.00499 -0.00712 AFIX 43 H23 2 -0.206506 -0.653505 0.141311 11.00000 -1.20000 AFIX 0 C24 1 -0.088214 -0.518355 0.027701 11.00000 0.01879 0.01250 = 0.01149 -0.00127 -0.00541 0.00000 C25 1 -0.255315 -0.452967 0.005157 11.00000 0.01302 0.02962 = 0.01439 -0.00743 0.00234 -0.00895 AFIX 43 H25 2 -0.372772 -0.479430 0.041458 11.00000 -1.20000 AFIX 0 O21 3 0.101637 -0.685890 0.273929 11.00000 0.01454 0.01543 = 0.01526 -0.00176 -0.00585 -0.00162 O22 3 -0.114656 -0.884430 0.246435 11.00000 0.01186 0.01494 = 0.01383 -0.00103 -0.00059 -0.00273 O23 3 0.221025 -0.921345 0.209945 11.00000 0.01386 0.00913 = 0.01102 -0.00100 -0.00601 0.00691 S21 4 0.069156 -0.803511 0.220330 11.00000 0.00621 0.01157 = 0.00908 -0.00164 -0.00092 -0.00069 MOLE 3 O1W 3 0.203166 -0.300461 0.261995 11.00000 0.01430 0.01828 = 0.01773 0.00352 -0.00275 -0.00382 MOLE 4 O2W 3 -0.492510 -0.799727 0.264629 11.00000 0.01808 0.02363 = 0.02242 -0.00408 -0.00752 0.00273 MOLE 5 O31 3 -0.312553 -0.675511 0.373937 11.00000 0.01499 0.00795 = 0.00912 0.00209 -0.00405 -0.00497 O32 3 -0.085466 -0.652001 0.512372 11.00000 0.01599 0.00350 = 0.01578 0.00077 -0.00568 0.00013 O33 3 -0.081933 -0.930901 0.449810 11.00000 0.00727 0.01670 = 0.01014 -0.00308 -0.00332 0.00085 O34 3 -0.577031 -0.844766 0.485914 11.00000 0.01662 0.00770 = 0.01777 -0.00403 0.00083 -0.00044 O35 3 -0.694813 -0.567369 0.384776 11.00000 0.00882 0.01719 = 0.00847 -0.00507 -0.00037 0.00268 O36 3 -0.628261 -0.570208 0.550387 11.00000 0.00775 0.00937 = 0.00931 -0.00132 -0.00074 -0.00670 O37 3 -0.303036 -0.927103 0.612146 11.00000 0.01520 0.01707 = 0.00977 -0.00638 0.00066 -0.00261 O38 3 0.071088 -0.823703 0.625928 11.00000 0.01440 0.01181 = 0.01057 -0.00417 -0.00215 0.00081 LA1 5 -0.033229 -0.485561 0.370237 11.00000 0.00738 0.00723 = 0.00874 -0.00125 -0.00148 -0.00153 LA2 5 -0.349375 -0.985921 0.372836 11.00000 0.00748 0.00737 = 0.00871 -0.00149 -0.00104 -0.00100 W1 6 -0.078140 -0.869082 0.556277 11.00000 0.00751 0.00714 = 0.00930 -0.00114 -0.00124 -0.00092 W2 6 -0.526223 -0.628161 0.442715 11.00000 0.00771 0.00692 = 0.00898 -0.00160 -0.00193 -0.00066 HKLF 4 Covalent radii and connectivity table for 2009src0060p-1 in P-1 C 0.770 H 0.320 O 0.660 S 1.030 LA 1.870 W 1.370 C1 - C5 C2 C2 - C3 C1 S1 C3 - C2 C4 C4 - C5_$1 C3 C4_$1 C5 - C1 C4_$1 O1 - S1 La1 O2 - S1 La2_$10 O3 - S1 S1 - O3 O1 O2 C2 C21 - C25_$3 C22 C22 - C23 C21 S21 C23 - C22 C24 C24 - C25 C23 C24_$3 C25 - C21_$3 C24 O21 - S21 La1 O22 - S21 La2 O23 - S21 S21 - O22 O23 O21 C22 O1W - La1 O2W - La2 O31 - W2 La2 La1 O32 - W1 La1 La1_$4 O33 - W1 W1_$5 La2 O34 - W2 La2_$6 La2 O35 - W2 La1_$9 O36 - W2 W2_$8 La1_$8 O37 - W1 La2_$6 O38 - W1 La1_$4 La2_$5 La1 - O1 O32 O38_$4 O1W O31 O21 O35_$7 O36_$8 O32_$4 W1_$4 W2 La2 - O22 O2_$2 O34_$6 O38_$5 O31 O2W O37_$6 O33 O34 W2 W1_$5 W1 - O37 O32 O38 O33 O33_$5 W1_$5 La1_$4 La2_$5 W2 - O35 O34 O31 O36 O36_$8 W2_$8 La2 La1 Operators for generating equivalent atoms: $1 -x, -y, -z $2 x, y-1, z $3 -x, -y-1, -z $4 -x, -y-1, -z+1 $5 -x, -y-2, -z+1 $6 -x-1, -y-2, -z+1 $7 x+1, y, z $8 -x-1, -y-1, -z+1 $9 x-1, y, z $10 x, y+1, z 19709 Reflections read, of which 36 rejected -9 =< h =< 9, -10 =< k =< 10, -21 =< l =< 21, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 4394 Unique reflections, of which 0 suppressed R(int) = 0.0598 R(sigma) = 0.0494 Friedel opposites merged Maximum memory for data reduction = 2980 / 43810 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 20.00 20.00 H 20.00 12.00 O 32.00 32.00 S 4.00 4.00 LA 4.00 4.00 W 4.00 4.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0828 before cycle 1 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19500 0.00026 0.011 OSF Mean shift/su = 0.002 Maximum = -0.028 for U12 W2 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C24 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0828 before cycle 2 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.008 OSF Mean shift/su = 0.001 Maximum = -0.010 for U12 W2 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C24 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 3 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for H21 Max. dU = 0.000 for O32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 4 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for O36 Max. dU = 0.000 for O32 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 5 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for H25 Max. dU = 0.000 for O32 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 6 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19500 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for O34 Max. dU = 0.000 for O33 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 7 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for O2W Max. dU = 0.000 for O33 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3689 / 362880 wR2 = 0.0827 before cycle 8 for 4394 data and 289 / 289 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19501 0.00026 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z W1 Max. shift = 0.000 A for O33 Max. dU = 0.000 for O33 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 -0.4531 -0.0316 0.1126 43 0.950 0.000 C1 C5 C2 H3 0.0560 -0.2312 0.1248 43 0.950 0.000 C3 C2 C4 H5 -0.3303 0.1346 -0.0094 43 0.950 0.000 C5 C1 C4_$1 H21 0.3604 -0.6945 0.0833 43 0.950 0.000 C21 C25_$3 C22 H23 -0.2065 -0.6535 0.1413 43 0.950 0.000 C23 C22 C24 H25 -0.3728 -0.4794 0.0415 43 0.950 0.000 C25 C21_$3 C24 2009src0060p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.32429 -0.03858 0.08818 1.00000 0.02051 0.01957 0.01547 -0.00470 -0.00012 -0.00036 0.01879 0.01627 0.00148 0.00133 0.00064 0.00000 0.00515 0.00532 0.00523 0.00430 0.00402 0.00413 0.00215 H1 -0.45309 -0.03164 0.11256 1.00000 0.02254 0.00000 0.00000 C2 -0.20834 -0.15148 0.12605 1.00000 0.02206 0.00755 0.01310 -0.00493 -0.00350 -0.00407 0.01384 0.01434 0.00140 0.00118 0.00061 0.00000 0.00503 0.00440 0.00487 0.00379 0.00384 0.00371 0.00195 C3 -0.02065 -0.15859 0.09591 1.00000 0.02119 0.01288 0.00555 -0.00176 -0.00339 0.00053 0.01308 0.01484 0.00138 0.00122 0.00057 0.00000 0.00494 0.00463 0.00448 0.00374 0.00364 0.00379 0.00191 H3 0.05601 -0.23119 0.12481 1.00000 0.01570 0.00000 0.00000 C4 0.05879 -0.05550 0.02043 1.00000 0.01630 0.01141 0.01231 -0.00239 -0.00784 -0.00324 0.01259 0.01405 0.00133 0.00120 0.00060 0.00000 0.00470 0.00454 0.00479 0.00388 0.00378 0.00368 0.00192 C5 -0.25082 0.05990 0.01680 1.00000 0.01784 0.02362 0.02171 -0.01040 -0.00422 0.00952 0.02028 0.01681 0.00144 0.00139 0.00068 0.00000 0.00512 0.00567 0.00570 0.00468 0.00416 0.00426 0.00225 H5 -0.33032 0.13458 -0.00935 1.00000 0.02434 0.00000 0.00000 O1 -0.16195 -0.38254 0.24708 1.00000 0.01200 0.01615 0.00865 -0.00445 -0.00110 -0.00022 0.01212 0.00999 0.00089 0.00084 0.00040 0.00000 0.00316 0.00346 0.00329 0.00274 0.00250 0.00260 0.00135 O2 -0.39649 -0.17601 0.27558 1.00000 0.01566 0.01597 0.01002 -0.00392 -0.00026 -0.00030 0.01400 0.01040 0.00092 0.00086 0.00041 0.00000 0.00335 0.00351 0.00339 0.00280 0.00262 0.00270 0.00140 O3 -0.45248 -0.38918 0.19795 1.00000 0.00995 0.01956 0.01120 -0.00712 0.00275 -0.00316 0.01370 0.01014 0.00088 0.00087 0.00041 0.00000 0.00313 0.00361 0.00343 0.00288 0.00254 0.00265 0.00140 S1 -0.31250 -0.28433 0.21788 1.00000 0.00967 0.01152 0.01061 -0.00273 -0.00193 -0.00112 0.01050 0.00348 0.00031 0.00029 0.00014 0.00000 0.00102 0.00110 0.00111 0.00090 0.00083 0.00083 0.00044 C21 0.24847 -0.64842 0.06885 1.00000 0.01865 0.01130 0.01108 0.00005 -0.00907 0.00216 0.01306 0.01467 0.00138 0.00119 0.00059 0.00000 0.00482 0.00456 0.00473 0.00380 0.00378 0.00375 0.00192 H21 0.36036 -0.69446 0.08331 1.00000 0.01568 0.00000 0.00000 C22 0.07277 -0.68418 0.12380 1.00000 0.00632 0.00849 0.01101 -0.00048 0.00528 0.00004 0.00971 0.01467 0.00120 0.00114 0.00057 0.00000 0.00400 0.00425 0.00457 0.00359 0.00333 0.00327 0.00179 C23 -0.09065 -0.62456 0.10418 1.00000 0.01309 0.01274 0.01249 -0.00193 -0.00499 -0.00712 0.01243 0.01378 0.00132 0.00119 0.00059 0.00000 0.00444 0.00464 0.00483 0.00386 0.00361 0.00360 0.00190 H23 -0.20651 -0.65350 0.14131 1.00000 0.01491 0.00000 0.00000 C24 -0.08821 -0.51835 0.02770 1.00000 0.01879 0.01250 0.01149 -0.00127 -0.00541 0.00000 0.01401 0.01498 0.00134 0.00122 0.00061 0.00000 0.00505 0.00472 0.00484 0.00382 0.00390 0.00383 0.00197 C25 -0.25532 -0.45297 0.00516 1.00000 0.01302 0.02962 0.01439 -0.00743 0.00234 -0.00895 0.01924 0.01561 0.00139 0.00142 0.00064 0.00000 0.00472 0.00589 0.00526 0.00448 0.00382 0.00418 0.00222 H25 -0.37277 -0.47943 0.04146 1.00000 0.02309 0.00000 0.00000 O21 0.10164 -0.68589 0.27393 1.00000 0.01454 0.01543 0.01526 -0.00176 -0.00585 -0.00162 0.01476 0.01026 0.00092 0.00086 0.00043 0.00000 0.00333 0.00352 0.00363 0.00290 0.00272 0.00271 0.00143 O22 -0.11466 -0.88443 0.24643 1.00000 0.01186 0.01494 0.01383 -0.00103 -0.00059 -0.00272 0.01396 0.01037 0.00090 0.00085 0.00042 0.00000 0.00322 0.00349 0.00355 0.00284 0.00262 0.00264 0.00141 O23 0.22102 -0.92135 0.20995 1.00000 0.01386 0.00913 0.01102 -0.00100 -0.00601 0.00691 0.01096 0.01004 0.00088 0.00079 0.00040 0.00000 0.00273 0.00272 0.00283 0.00233 0.00227 0.00226 0.00132 S21 0.06916 -0.80351 0.22033 1.00000 0.00621 0.01157 0.00908 -0.00164 -0.00092 -0.00069 0.00904 0.00346 0.00030 0.00029 0.00014 0.00000 0.00096 0.00107 0.00107 0.00087 0.00079 0.00081 0.00043 O1W 0.20317 -0.30046 0.26200 1.00000 0.01430 0.01828 0.01773 0.00352 -0.00275 -0.00382 0.01758 0.01108 0.00095 0.00090 0.00044 0.00000 0.00336 0.00366 0.00379 0.00300 0.00279 0.00279 0.00150 O2W -0.49251 -0.79973 0.26463 1.00000 0.01808 0.02363 0.02242 -0.00408 -0.00752 0.00273 0.02088 0.01149 0.00100 0.00096 0.00047 0.00000 0.00364 0.00402 0.00411 0.00328 0.00302 0.00301 0.00159 O31 -0.31255 -0.67551 0.37394 1.00000 0.01499 0.00795 0.00912 0.00209 -0.00405 -0.00497 0.01085 0.00969 0.00090 0.00079 0.00040 0.00000 0.00322 0.00311 0.00325 0.00257 0.00254 0.00250 0.00131 O32 -0.08547 -0.65200 0.51237 1.00000 0.01600 0.00350 0.01578 0.00077 -0.00568 0.00014 0.01169 0.01001 0.00090 0.00078 0.00042 0.00000 0.00280 0.00254 0.00296 0.00232 0.00235 0.00220 0.00133 O33 -0.08193 -0.93090 0.44981 1.00000 0.00727 0.01670 0.01014 -0.00308 -0.00332 0.00085 0.01106 0.00978 0.00084 0.00083 0.00040 0.00000 0.00299 0.00347 0.00330 0.00274 0.00246 0.00252 0.00133 O34 -0.57703 -0.84477 0.48591 1.00000 0.01662 0.00770 0.01777 -0.00403 0.00083 -0.00044 0.01439 0.01050 0.00093 0.00081 0.00043 0.00000 0.00339 0.00316 0.00369 0.00281 0.00275 0.00258 0.00141 O35 -0.69481 -0.56737 0.38478 1.00000 0.00882 0.01719 0.00847 -0.00507 -0.00037 0.00268 0.01135 0.01004 0.00086 0.00084 0.00039 0.00000 0.00302 0.00348 0.00326 0.00273 0.00245 0.00254 0.00133 O36 -0.62826 -0.57021 0.55039 1.00000 0.00775 0.00937 0.00932 -0.00132 -0.00074 -0.00670 0.00895 0.00929 0.00083 0.00078 0.00039 0.00000 0.00256 0.00270 0.00274 0.00227 0.00215 0.00216 0.00127 O37 -0.30304 -0.92710 0.61215 1.00000 0.01520 0.01707 0.00977 -0.00638 0.00066 -0.00261 0.01395 0.01018 0.00092 0.00086 0.00041 0.00000 0.00334 0.00355 0.00338 0.00282 0.00262 0.00269 0.00140 O38 0.07109 -0.82370 0.62593 1.00000 0.01440 0.01181 0.01057 -0.00417 -0.00215 0.00081 0.01204 0.01007 0.00090 0.00082 0.00041 0.00000 0.00323 0.00328 0.00334 0.00268 0.00257 0.00257 0.00134 La1 -0.03323 -0.48556 0.37024 1.00000 0.00738 0.00723 0.00874 -0.00125 -0.00148 -0.00153 0.00781 0.00078 0.00007 0.00006 0.00003 0.00000 0.00023 0.00025 0.00026 0.00020 0.00018 0.00018 0.00012 La2 -0.34937 -0.98592 0.37284 1.00000 0.00748 0.00737 0.00871 -0.00149 -0.00104 -0.00100 0.00791 0.00078 0.00007 0.00006 0.00003 0.00000 0.00023 0.00025 0.00026 0.00020 0.00018 0.00018 0.00012 W1 -0.07814 -0.86908 0.55628 1.00000 0.00751 0.00714 0.00930 -0.00114 -0.00124 -0.00092 0.00807 0.00055 0.00005 0.00004 0.00002 0.00000 0.00017 0.00018 0.00019 0.00014 0.00013 0.00013 0.00010 W2 -0.52622 -0.62816 0.44272 1.00000 0.00771 0.00692 0.00898 -0.00160 -0.00193 -0.00066 0.00780 0.00054 0.00005 0.00004 0.00002 0.00000 0.00017 0.00018 0.00019 0.00014 0.00013 0.00013 0.00010 Final Structure Factor Calculation for 2009src0060p-1 in P-1 Total number of l.s. parameters = 289 Maximum vector length = 511 Memory required = 3400 / 25039 wR2 = 0.0827 before cycle 9 for 4394 data and 0 / 289 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.000 GooF = S = 1.119; Restrained GooF = 1.118 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 23.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0387 for 3837 Fo > 4sig(Fo) and 0.0483 for all 4394 data wR2 = 0.0827, GooF = S = 1.119, Restrained GooF = 1.118 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0236 0.0191 0.0137 C1 0.0237 0.0140 0.0039 C2 0.0212 0.0129 0.0051 C3 0.0203 0.0120 0.0055 C4 0.0310 0.0201 0.0097 C5 0.0168 0.0121 0.0075 O1 0.0178 0.0152 0.0089 O2 0.0238 0.0111 0.0063 O3 0.0126 0.0103 0.0086 S1 0.0211 0.0127 0.0054 C21 0.0182 0.0085 0.0024 C22 0.0210 0.0124 0.0039 C23 0.0193 0.0127 0.0101 C24 0.0357 0.0135 0.0085 C25 0.0189 0.0147 0.0107 O21 0.0170 0.0154 0.0096 O22 0.0184 0.0113 0.0031 O23 0.0118 0.0093 0.0061 S21 0.0262 0.0159 0.0106 O1W 0.0247 0.0229 0.0151 O2W 0.0189 0.0088 0.0048 O31 0.0185 0.0132 0.0033 O32 0.0167 0.0103 0.0061 O33 0.0226 0.0137 0.0069 O34 0.0179 0.0103 0.0058 O35 0.0158 0.0094 0.0016 O36 0.0218 0.0130 0.0070 O37 0.0145 0.0132 0.0084 O38 0.0091 0.0088 0.0055 La1 0.0093 0.0082 0.0062 La2 0.0095 0.0085 0.0062 W1 0.0090 0.0083 0.0061 W2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.046 0.073 0.104 0.134 0.165 0.202 0.243 0.315 1.000 Number in group 453. 425. 446. 452. 430. 444. 423. 441. 442. 438. GooF 1.208 1.259 1.208 1.224 1.197 1.181 0.989 0.991 0.894 0.960 K 2.369 1.196 1.025 0.981 0.982 0.995 1.000 1.005 1.009 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 444. 448. 427. 444. 442. 437. 435. 437. 443. 437. GooF 1.251 1.221 1.287 1.138 1.109 1.046 1.018 1.016 0.920 1.129 K 1.009 1.024 1.027 1.021 1.007 1.012 1.000 1.001 1.003 1.000 R1 0.088 0.078 0.070 0.063 0.048 0.042 0.035 0.029 0.024 0.024 Recommended weighting scheme: WGHT 0.0000 23.9592 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 7 7 5 850.45 3243.12 4.90 0.114 0.77 5 1 18 3437.41 6062.95 4.75 0.155 0.85 2 -6 13 4283.54 1785.13 4.55 0.084 0.85 -2 -1 4 6849.30 5238.19 3.56 0.144 2.27 -3 8 0 1457.01 2511.24 3.54 0.100 0.93 6 -5 8 3374.80 4925.96 3.47 0.140 0.89 2 -1 4 1748.48 2726.79 3.46 0.104 2.72 5 3 18 4447.88 6782.03 3.45 0.164 0.84 -3 -7 7 2913.70 4358.74 3.38 0.132 0.86 4 -6 13 3547.74 1824.76 3.36 0.085 0.81 -6 -3 10 7715.14 10614.85 3.33 0.206 0.81 2 -5 16 6909.57 4766.73 3.32 0.138 0.81 7 -1 2 425.46 4.43 3.28 0.004 1.03 -2 5 18 2872.47 1293.51 3.17 0.072 0.80 -5 -1 14 2001.59 3491.12 3.14 0.118 0.81 3 4 21 2861.49 4496.82 3.12 0.134 0.78 -2 -8 7 2178.72 3631.57 3.06 0.120 0.82 1 1 4 5479.73 4279.46 3.02 0.131 3.72 -8 -4 1 925.60 52.96 3.01 0.015 0.79 3 -9 5 -194.34 1101.88 3.00 0.066 0.80 1 5 11 2432.11 3678.05 2.98 0.121 1.21 0 -9 2 501.85 6.41 2.94 0.005 0.87 -1 0 13 765.49 295.50 2.93 0.034 1.20 5 -1 13 1631.42 2614.27 2.92 0.102 1.03 -8 -3 1 1438.85 443.44 2.92 0.042 0.83 3 9 5 6219.69 4122.62 2.87 0.128 0.85 5 -8 2 3642.41 1123.78 2.86 0.067 0.82 8 3 0 768.74 1657.41 2.85 0.081 0.84 -3 1 10 1801.39 1081.82 2.84 0.066 1.25 3 9 9 1269.04 2216.01 2.83 0.094 0.82 0 2 15 44832.50 50365.15 2.79 0.448 1.10 -8 3 2 1250.20 349.10 2.79 0.037 0.83 0 2 14 19505.83 22336.37 2.74 0.298 1.18 5 -6 8 -147.69 278.77 2.73 0.033 0.89 -6 1 11 498.78 1307.03 2.71 0.072 0.85 -4 3 12 1128.94 561.21 2.70 0.047 0.97 1 2 5 1031.85 548.66 2.65 0.047 2.72 9 1 8 13735.13 10729.91 2.65 0.207 0.79 -4 2 12 173.94 597.33 2.64 0.049 0.99 -3 7 13 1121.16 386.28 2.64 0.039 0.83 5 3 6 11274.89 13213.05 2.63 0.229 1.25 -1 5 10 4035.51 5296.01 2.63 0.145 1.21 4 -7 10 1188.61 182.35 2.62 0.027 0.82 1 3 19 5279.41 7355.86 2.62 0.171 0.88 2 1 10 1150.66 1788.38 2.61 0.084 1.63 -4 8 3 1304.36 2476.09 2.61 0.099 0.88 -3 -8 7 462.02 1069.52 2.60 0.065 0.79 2 1 5 28703.13 25752.85 2.60 0.320 2.64 -6 6 9 8267.69 10835.43 2.58 0.208 0.79 -2 -2 18 815.91 230.58 2.58 0.030 0.80 Bond lengths and angles C1 - Distance Angles C5 1.3465 (0.0154) C2 1.4016 (0.0147) 119.16 (0.96) C1 - C5 C2 - Distance Angles C3 1.3616 (0.0138) C1 1.4016 (0.0147) 122.40 (0.93) S1 1.7718 (0.0102) 119.84 (0.77) 117.74 (0.77) C2 - C3 C1 C3 - Distance Angles C2 1.3616 (0.0137) C4 1.4229 (0.0135) 118.92 (0.90) C3 - C2 C4 - Distance Angles C5_$1 1.4148 (0.0137) C3 1.4229 (0.0135) 122.59 (0.91) C4_$1 1.4256 (0.0189) 118.14 (1.14) 119.27 (1.12) C4 - C5_$1 C3 C5 - Distance Angles C1 1.3465 (0.0154) C4_$1 1.4148 (0.0137) 121.98 (0.99) C5 - C1 O1 - Distance Angles S1 1.4638 (0.0069) La1 2.4685 (0.0066) 143.35 (0.39) O1 - S1 O2 - Distance Angles S1 1.4643 (0.0070) La2_$10 2.5056 (0.0067) 148.02 (0.40) O2 - S1 O3 - Distance Angles S1 1.4520 (0.0068) O3 - S1 - Distance Angles O3 1.4520 (0.0068) O1 1.4638 (0.0069) 111.98 (0.41) O2 1.4643 (0.0070) 112.17 (0.39) 111.38 (0.40) C2 1.7718 (0.0102) 106.94 (0.43) 107.11 (0.44) 106.89 (0.43) S1 - O3 O1 O2 C21 - Distance Angles C25_$3 1.3716 (0.0144) C22 1.4224 (0.0127) 119.58 (0.89) C21 - C25_$3 C22 - Distance Angles C23 1.3581 (0.0131) C21 1.4224 (0.0126) 121.80 (0.89) S21 1.7507 (0.0097) 119.39 (0.70) 118.79 (0.69) C22 - C23 C21 C23 - Distance Angles C22 1.3581 (0.0131) C24 1.4277 (0.0138) 119.95 (0.88) C23 - C22 C24 - Distance Angles C25 1.4155 (0.0143) C23 1.4277 (0.0138) 121.68 (0.90) C24_$3 1.4307 (0.0194) 119.87 (1.14) 118.43 (1.09) C24 - C25 C23 C25 - Distance Angles C21_$3 1.3716 (0.0144) C24 1.4155 (0.0143) 120.32 (0.92) C25 - C21_$3 O21 - Distance Angles S21 1.4711 (0.0071) La1 2.5485 (0.0070) 148.66 (0.40) O21 - S21 O22 - Distance Angles S21 1.4444 (0.0067) La2 2.4811 (0.0066) 140.54 (0.42) O22 - S21 O23 - Distance Angles S21 1.4582 (0.0064) O23 - S21 - Distance Angles O22 1.4444 (0.0067) O23 1.4582 (0.0064) 113.09 (0.41) O21 1.4711 (0.0071) 111.93 (0.41) 111.65 (0.39) C22 1.7507 (0.0097) 106.54 (0.42) 106.51 (0.40) 106.62 (0.43) S21 - O22 O23 O21 O1W - Distance Angles La1 2.5362 (0.0069) O1W - O2W - Distance Angles La2 2.5539 (0.0074) O2W - O31 - Distance Angles W2 1.8276 (0.0066) La2 2.5369 (0.0063) 103.70 (0.26) La1 2.5373 (0.0061) 113.58 (0.29) 133.53 (0.27) O31 - W2 La2 O32 - Distance Angles W1 1.7983 (0.0062) La1 2.5144 (0.0066) 135.87 (0.34) La1_$4 2.7127 (0.0066) 98.82 (0.27) 117.98 (0.24) O32 - W1 La1 O33 - Distance Angles W1 1.9551 (0.0065) W1_$5 1.9946 (0.0064) 105.62 (0.29) La2 2.6189 (0.0061) 134.18 (0.29) 104.16 (0.26) O33 - W1 W1_$5 O34 - Distance Angles W2 1.7974 (0.0066) La2_$6 2.5105 (0.0070) 136.07 (0.35) La2 2.6780 (0.0067) 99.38 (0.28) 115.93 (0.25) O34 - W2 La2_$6 O35 - Distance Angles W2 1.7333 (0.0064) La1_$9 2.5871 (0.0062) 152.11 (0.34) O35 - W2 O36 - Distance Angles W2 1.9606 (0.0064) W2_$8 1.9983 (0.0059) 105.06 (0.27) La1_$8 2.6337 (0.0061) 134.84 (0.29) 104.06 (0.25) O36 - W2 W2_$8 O37 - Distance Angles W1 1.7415 (0.0065) La2_$6 2.5750 (0.0065) 153.68 (0.36) O37 - W1 O38 - Distance Angles W1 1.8299 (0.0065) La1_$4 2.5321 (0.0066) 104.56 (0.28) La2_$5 2.5360 (0.0065) 112.91 (0.29) 132.99 (0.27) O38 - W1 La1_$4 La1 - Distance Angles O1 2.4685 (0.0066) O32 2.5144 (0.0067) 148.09 (0.21) O38_$4 2.5321 (0.0066) 76.68 (0.21) 110.91 (0.21) O1W 2.5362 (0.0069) 68.13 (0.22) 143.75 (0.22) 66.42 (0.23) O31 2.5373 (0.0061) 72.96 (0.21) 77.10 (0.20) 121.43 (0.21) 136.91 (0.22) O21 2.5485 (0.0070) 77.35 (0.21) 106.37 (0.22) 141.25 (0.22) 77.43 (0.23) 76.67 (0.21) O35_$7 2.5871 (0.0062) 130.30 (0.21) 77.93 (0.21) 109.37 (0.21) 70.02 (0.22) 128.53 (0.21) 68.39 (0.20) O36_$8 2.6337 (0.0061) 84.32 (0.20) 70.68 (0.20) 69.61 (0.20) 132.10 (0.21) 58.66 (0.20) 135.01 (0.20) 145.04 (0.20) O32_$4 2.7127 (0.0066) 136.36 (0.20) 62.02 (0.24) 59.86 (0.20) 89.64 (0.22) 132.37 (0.20) 135.70 (0.20) 67.37 (0.20) W1_$4 3.4769 (0.0006) 105.83 (0.16) 90.30 (0.15) 30.62 (0.15) 69.97 (0.17) 140.49 (0.15) 142.63 (0.15) 83.38 (0.15) W2 3.6725 (0.0006) 79.73 (0.15) 68.53 (0.15) 99.28 (0.15) 146.89 (0.16) 27.14 (0.15) 103.80 (0.15) 141.92 (0.15) La1 - O1 O32 O38_$4 O1W O31 O21 O35_$7 La2 - Distance Angles O22 2.4811 (0.0066) O2_$2 2.5056 (0.0067) 75.34 (0.22) O34_$6 2.5105 (0.0070) 148.88 (0.22) 107.16 (0.22) O38_$5 2.5360 (0.0065) 73.10 (0.22) 77.22 (0.21) 77.23 (0.21) O31 2.5369 (0.0063) 76.10 (0.22) 138.96 (0.22) 112.55 (0.21) 120.95 (0.21) O2W 2.5539 (0.0074) 67.36 (0.23) 75.85 (0.23) 143.77 (0.23) 136.45 (0.23) 66.20 (0.22) O37_$6 2.5750 (0.0065) 128.85 (0.22) 67.39 (0.21) 77.53 (0.22) 127.33 (0.21) 111.31 (0.21) 70.42 (0.23) O33 2.6189 (0.0061) 85.27 (0.21) 135.58 (0.21) 71.33 (0.21) 58.86 (0.20) 69.58 (0.20) 132.12 (0.22) 145.73 (0.21) O34 2.6780 (0.0067) 135.96 (0.21) 134.96 (0.21) 64.07 (0.25) 134.63 (0.22) 60.40 (0.20) 87.89 (0.23) 67.60 (0.21) W2 3.4601 (0.0006) 105.15 (0.16) 141.05 (0.16) 92.04 (0.15) 141.14 (0.15) 30.88 (0.15) 69.11 (0.17) 84.93 (0.15) W1_$5 3.6596 (0.0006) 80.94 (0.16) 104.63 (0.15) 68.31 (0.15) 27.43 (0.15) 99.26 (0.14) 147.25 (0.17) 140.89 (0.16) La2 - O22 O2_$2 O34_$6 O38_$5 O31 O2W O37_$6 W1 - Distance Angles O37 1.7415 (0.0065) O32 1.7983 (0.0063) 106.65 (0.31) O38 1.8299 (0.0065) 109.08 (0.30) 92.53 (0.30) O33 1.9551 (0.0065) 103.33 (0.28) 89.76 (0.29) 145.31 (0.27) O33_$5 1.9946 (0.0065) 110.49 (0.29) 142.02 (0.28) 82.87 (0.27) 74.38 (0.29) W1_$5 3.1465 (0.0007) 111.42 (0.22) 119.81 (0.22) 115.61 (0.20) 37.63 (0.19) 36.76 (0.18) La1_$4 3.4769 (0.0006) 103.53 (0.22) 50.44 (0.21) 44.82 (0.21) 136.99 (0.20) 124.86 (0.18) 144.75 (0.02) La2_$5 3.6596 (0.0006) 122.85 (0.23) 117.74 (0.20) 39.67 (0.20) 110.61 (0.18) 43.94 (0.18) 76.25 (0.02) 81.23 (0.01) W1 - O37 O32 O38 O33 O33_$5 W1_$5 La1_$4 W2 - Distance Angles O35 1.7333 (0.0064) O34 1.7974 (0.0066) 106.39 (0.31) O31 1.8276 (0.0066) 108.17 (0.29) 92.83 (0.29) O36 1.9606 (0.0064) 104.98 (0.28) 88.83 (0.28) 144.83 (0.26) O36_$8 1.9983 (0.0059) 110.22 (0.29) 142.64 (0.29) 82.84 (0.26) 74.94 (0.27) W2_$8 3.1421 (0.0007) 112.41 (0.22) 119.52 (0.22) 115.52 (0.20) 37.89 (0.17) 37.06 (0.18) La2 3.4601 (0.0006) 103.52 (0.22) 49.78 (0.21) 45.43 (0.19) 135.01 (0.19) 125.15 (0.18) 143.85 (0.02) La1 3.6725 (0.0006) 121.04 (0.21) 118.84 (0.21) 39.29 (0.19) 111.36 (0.17) 44.08 (0.18) 76.73 (0.01) 81.58 (0.01) W2 - O35 O34 O31 O36 O36_$8 W2_$8 La2 FMAP and GRID set by program FMAP 2 1 35 GRID -3.125 -2 -1 3.125 2 1 R1 = 0.0467 for 4394 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.12 at 0.0895 0.7797 0.4907 [ 1.00 A from W1 ] Deepest hole -1.76 at 0.9401 0.8158 0.4625 [ 1.06 A from W1 ] Mean = 0.00, Rms deviation from mean = 0.36 e/A^3, Highest memory used = 3466 / 33601 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0895 -0.7797 0.5093 1.00000 0.05 2.12 1.00 W1 1.05 O32 1.71 O33 2.27 O37 Q2 1 -0.5942 -0.7457 0.4871 1.00000 0.05 1.69 0.82 O34 1.16 W2 1.91 O36 2.30 O35 Q3 1 -0.3394 -0.5599 0.3879 1.00000 0.05 1.60 1.01 O31 1.53 W2 1.59 O36 2.25 LA1 Q4 1 0.1968 -0.8221 0.1930 1.00000 0.05 1.47 0.84 O23 0.97 S21 1.84 C22 1.92 O21 Q5 1 0.1264 -0.8482 0.3078 1.00000 0.05 1.36 1.37 O21 1.60 S21 1.86 O23 2.25 O22 Q6 1 0.0299 -0.3753 0.3286 1.00000 0.05 1.35 1.08 LA1 1.56 O1W 1.98 O38 2.15 O1 Q7 1 -0.1687 -0.9216 0.6205 1.00000 0.05 1.33 1.01 O37 1.17 W1 1.94 O38 2.40 O33 Q8 1 -0.5348 -0.5843 0.3916 1.00000 0.05 1.30 0.89 W2 1.19 O35 1.76 O31 2.19 O36 Q9 1 -0.4112 -0.6593 0.4092 1.00000 0.05 1.29 0.86 O31 0.97 W2 2.04 O34 2.13 O36 Q10 1 -0.0639 -0.7057 0.3655 1.00000 0.05 1.27 1.75 O21 1.80 O31 1.82 LA1 2.11 O33 Shortest distances between peaks (including symmetry equivalents) 3 9 0.94 8 9 1.14 3 8 1.42 2 9 1.73 2 8 1.88 4 5 1.89 5 10 2.01 1 7 2.02 5 7 2.11 3 10 2.32 1 10 2.38 9 10 2.53 2 3 2.55 6 10 2.71 6 7 2.94 3 6 2.99 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 0.00: Analyse other restraints etc. 0.89: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.03: Generate idealized H-atoms 1.28: Structure factors and derivatives 4.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.50: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0060p-1 finished at 10:25:26 Total CPU time: 7.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++