+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:51:57 on 12-Jun-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 6.9577 17.1010 17.8604 90.000 97.345 90.000 ZERR 2.00 0.0003 0.0007 0.0008 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CU UNIT 72 72 24 40 8 V = 2107.66 F(000) = 1224.0 Mu = 2.09 mm-1 Cell Wt = 2421.86 Rho = 1.908 MERG 2 OMIT -3.00 55.00 OMIT 1 1 0 OMIT 0 2 2 OMIT -1 1 1 DFIX 0.84 0.02 O1W H1WA O1W H1WB DANG 1.35 0.02 H1WA H1WB EQIV $1 X+1,Y, Z HTAB O1W O21 HTAB O1W O12_$1 FMAP 2 PLAN 10 BOND $H ACTA SIZE 0.01 0.06 0.10 WGHT 0.05800 3.37700 L.S. 19 TEMP -153.00 FVAR 0.19781 MOLE 1 C1 1 0.912877 0.108343 1.003351 11.00000 0.02986 0.02550 = 0.01975 0.00014 0.00334 0.00241 AFIX 43 H1 2 0.893926 0.053564 1.007377 11.00000 -1.20000 AFIX 0 C2 1 0.988878 0.150210 1.067318 11.00000 0.03525 0.03554 = 0.01936 0.00150 -0.00248 0.00866 AFIX 43 H2 2 1.024489 0.124106 1.113983 11.00000 -1.20000 AFIX 0 C3 1 1.011461 0.229288 1.061995 11.00000 0.02773 0.03767 = 0.02130 -0.00616 -0.00202 0.00049 AFIX 43 H3 2 1.063680 0.258732 1.104937 11.00000 -1.20000 AFIX 0 C4 1 0.957595 0.266206 0.993466 11.00000 0.02770 0.02848 = 0.02061 -0.00428 0.00420 0.00137 AFIX 43 H4 2 0.968901 0.321343 0.989224 11.00000 -1.20000 AFIX 0 C5 1 0.886991 0.221588 0.931190 11.00000 0.01952 0.02821 = 0.01655 -0.00095 0.00238 0.00254 C6 1 0.831192 0.253053 0.854522 11.00000 0.01844 0.02739 = 0.01975 -0.00177 0.00408 -0.00017 C7 1 0.822612 0.330576 0.832579 11.00000 0.02943 0.02349 = 0.02173 -0.00393 0.00524 -0.00517 AFIX 43 H7 2 0.855732 0.371077 0.868311 11.00000 -1.20000 AFIX 0 C8 1 0.764176 0.348085 0.756709 11.00000 0.03214 0.02591 = 0.02064 0.00357 0.00473 0.00057 AFIX 43 H8 2 0.758783 0.401042 0.740507 11.00000 -1.20000 AFIX 0 C9 1 0.714154 0.289152 0.705008 11.00000 0.03547 0.02811 = 0.01851 0.00764 0.00619 0.00263 AFIX 43 H9 2 0.671518 0.300628 0.653517 11.00000 -1.20000 AFIX 0 C10 1 0.728248 0.213028 0.730730 11.00000 0.02485 0.02531 = 0.01816 -0.00101 0.00287 0.00033 C11 1 0.682469 0.141741 0.684346 11.00000 0.03038 0.02911 = 0.01601 0.00465 0.00094 -0.00196 C12 1 0.676457 -0.057615 0.699340 11.00000 0.02949 0.03209 = 0.00876 0.00314 -0.00062 -0.00381 AFIX 43 H12 2 0.717011 -0.063620 0.751863 11.00000 -1.20000 AFIX 0 C13 1 0.649730 -0.127223 0.654230 11.00000 0.02503 0.02863 = 0.01678 0.00047 0.00197 -0.00336 C14 1 0.693880 -0.198672 0.691160 11.00000 0.02666 0.02806 = 0.01274 0.00605 -0.00105 0.00137 AFIX 43 H14 2 0.738687 -0.198213 0.743684 11.00000 -1.20000 AFIX 0 C15 1 0.674733 -0.269181 0.654220 11.00000 0.02942 0.02390 = 0.01987 0.00594 0.00318 0.00232 AFIX 43 H15 2 0.702754 -0.316802 0.680775 11.00000 -1.20000 AFIX 0 C16 1 0.613103 -0.269239 0.576700 11.00000 0.03112 0.02429 = 0.01915 -0.00223 0.00464 -0.00226 AFIX 43 H16 2 0.602745 -0.317450 0.550062 11.00000 -1.20000 AFIX 0 C17 1 0.566906 -0.200391 0.538044 11.00000 0.03674 0.02385 = 0.01459 0.00115 0.00493 -0.00104 AFIX 43 H17 2 0.524511 -0.202114 0.485354 11.00000 -1.20000 AFIX 0 C18 1 0.581531 -0.128035 0.575253 11.00000 0.02575 0.02296 = 0.01410 0.00104 0.00328 -0.00145 N1 3 0.865889 0.143176 0.936447 11.00000 0.02303 0.02572 = 0.01361 0.00139 0.00157 0.00183 N2 3 0.783632 0.196347 0.803262 11.00000 0.02570 0.02190 = 0.01615 -0.00051 0.00333 0.00150 N3 3 0.688251 0.075414 0.723279 11.00000 0.03313 0.02535 = 0.01530 0.00075 -0.00179 -0.00148 N4 3 0.649234 0.012485 0.673508 11.00000 0.03796 0.02294 = 0.01322 -0.00250 -0.00361 -0.00288 O1 4 0.645164 0.147134 0.613064 11.00000 0.05262 0.02304 = 0.01254 0.00461 -0.00487 -0.00428 O2 4 0.529713 -0.062092 0.536489 11.00000 0.05500 0.02111 = 0.01175 0.00222 -0.00107 0.00174 CU1 5 0.779317 0.088501 0.836743 11.00000 0.02882 0.02123 = 0.01369 0.00085 0.00017 -0.00027 CU2 5 0.573834 0.044377 0.570119 11.00000 0.07415 0.02083 = 0.01390 0.00224 -0.00868 -0.00336 MOLE 2 N11 3 0.530677 -0.011928 0.894970 11.00000 0.03079 0.02776 = 0.01949 -0.00324 0.00097 -0.00341 O11 4 0.707362 -0.013032 0.879291 11.00000 0.02879 0.02601 = 0.01949 0.00321 0.00281 0.00195 O12 4 0.439683 0.050550 0.883288 11.00000 0.03106 0.02902 = 0.04837 -0.00265 0.00117 0.00395 O13 4 0.462023 -0.070798 0.919798 11.00000 0.04898 0.03558 = 0.04443 0.00770 0.01235 -0.01275 MOLE 3 N21 3 1.176043 0.079818 0.653232 11.00000 0.05628 0.02944 = 0.01964 -0.00122 0.00023 -0.00351 O21 4 1.121804 0.016883 0.676828 11.00000 0.08953 0.02876 = 0.04638 -0.00425 0.03308 -0.00537 O22 4 1.175992 0.138791 0.692422 11.00000 0.13874 0.03318 = 0.02072 -0.00380 -0.00116 -0.01251 O23 4 1.224211 0.082795 0.586793 11.00000 0.06880 0.05811 = 0.01871 0.00081 0.00680 -0.01620 MOLE 4 O1W 4 1.051150 0.027196 0.824682 11.00000 0.02788 0.03872 = 0.01896 0.00014 0.00292 0.00105 H1WA 2 1.158137 0.031558 0.850121 11.00000 -1.20000 H1WB 2 1.059844 0.037325 0.780019 11.00000 -1.20000 MOLE 5 O2W 4 0.872191 0.040376 0.509713 11.00000 0.14611 0.11386 = 0.09846 0.00962 0.00366 -0.00709 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 CU 1.280 C1 - N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C6 C8 C8 - C9 C7 C9 - C10 C8 C10 - N2 C9 C11 C11 - O1 N3 C10 C12 - N4 C13 C13 - C14 C18 C12 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - O2 C17 C13 N1 - C1 C5 Cu1 N2 - C10 C6 Cu1 N3 - C11 N4 Cu1 N4 - C12 N3 Cu2 O1 - C11 Cu2 O2 - C18 Cu2 Cu2_$2 Cu1 - N2 O11 N1 N3 O1W Cu2 - O2 N4 O1 O2_$2 Cu2_$2 N11 - O13 O12 O11 O11 - N11 Cu1 O12 - N11 O13 - N11 N21 - O22 O21 O23 O21 - N21 O22 - N21 O23 - N21 O1W - Cu1 O2W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+1, -y, -z+1 h k l Fo^2 Sigma Why rejected -4 0 3 71.80 13.17 observed but should be systematically absent 4 0 5 9.52 2.38 observed but should be systematically absent 25950 Reflections read, of which 471 rejected -8 =< h =< 8, -22 =< k =< 22, -23 =< l =< 23, Max. 2-theta = 54.98 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 12 1 27.39 7.05 2 36.85 4 16 2 5.97 2.59 5 18.44 2 18 2 -3.53 4.25 3 48.87 -3 17 5 50.02 4.67 5 31.73 -4 12 8 39.38 2.13 8 11.00 3 15 8 39.14 6.30 3 33.50 -3 11 12 3.48 1.79 7 11.17 3 5 13 8.26 2.43 5 13.63 -7 8 13 1.98 3.54 2 26.08 -3 10 13 4.48 1.66 7 11.34 -4 15 14 4.66 2.25 3 16.31 11 Inconsistent equivalents 4743 Unique reflections, of which 0 suppressed R(int) = 0.0971 R(sigma) = 0.0830 Friedel opposites merged Maximum memory for data reduction = 2760 / 46979 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 72.00 72.00 H 72.00 56.00 N 24.00 24.00 O 40.00 40.00 CU 8.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 1 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.021 OSF Mean shift/esd = 0.004 Maximum = 0.040 for U22 Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O2W Least-squares cycle 2 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 2 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.008 OSF Mean shift/esd = 0.001 Maximum = 0.015 for U22 Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O2W Least-squares cycle 3 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 3 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 O2W Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O2W Least-squares cycle 4 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 4 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O2W Least-squares cycle 5 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 5 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O2W Least-squares cycle 6 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 6 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O2W Least-squares cycle 7 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 7 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 8 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O22 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 9 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H15 Max. dU = 0.000 for N1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 10 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for C4 Max. dU = 0.000 for N1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 11 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for C5 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 12 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O2W Least-squares cycle 13 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 13 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O21 Least-squares cycle 14 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 14 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O2W Least-squares cycle 15 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 15 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O1W Least-squares cycle 16 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 16 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O2W Least-squares cycle 17 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 17 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for N1 Least-squares cycle 18 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 18 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H15 Max. dU = 0.000 for O21 Least-squares cycle 19 Maximum vector length = 511 Memory required = 3598 / 417907 wR2 = 0.1412 before cycle 19 for 4743 data and 331 / 331 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19782 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Cu2 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O2W Largest correlation matrix elements -0.596 z H1WA / x H1WA 0.518 x H1WB / z H1WA Idealized hydrogen atom generation before cycle 20 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.8939 0.0536 1.0074 43 0.950 0.000 C1 N1 C2 H2 1.0245 0.1241 1.1140 43 0.950 0.000 C2 C3 C1 H3 1.0637 0.2587 1.1049 43 0.950 0.000 C3 C2 C4 H4 0.9689 0.3213 0.9892 43 0.950 0.000 C4 C3 C5 H7 0.8557 0.3711 0.8683 43 0.950 0.000 C7 C6 C8 H8 0.7588 0.4010 0.7405 43 0.950 0.000 C8 C9 C7 H9 0.6715 0.3006 0.6535 43 0.950 0.000 C9 C10 C8 H12 0.7170 -0.0636 0.7519 43 0.950 0.000 C12 N4 C13 H14 0.7387 -0.1982 0.7437 43 0.950 0.000 C14 C15 C13 H15 0.7028 -0.3168 0.6808 43 0.950 0.000 C15 C14 C16 H16 0.6027 -0.3174 0.5501 43 0.950 0.000 C16 C17 C15 H17 0.5245 -0.2021 0.4854 43 0.950 0.000 C17 C16 C18 s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.91288 0.10834 1.00335 1.00000 0.02987 0.02551 0.01977 0.00015 0.00334 0.00241 0.02503 0.00871 0.00067 0.00029 0.00025 0.00000 0.00263 0.00272 0.00238 0.00197 0.00199 0.00201 0.00106 H1 0.89393 0.05356 1.00738 1.00000 0.03004 0.00000 0.00000 C2 0.98888 0.15021 1.06731 1.00000 0.03527 0.03555 0.01935 0.00149 -0.00247 0.00866 0.03057 0.00928 0.00072 0.00031 0.00028 0.00000 0.00280 0.00314 0.00248 0.00214 0.00209 0.00229 0.00116 H2 1.02449 0.12411 1.11398 1.00000 0.03669 0.00000 0.00000 C3 1.01146 0.22929 1.06199 1.00000 0.02773 0.03767 0.02129 -0.00615 -0.00200 0.00050 0.02934 0.00909 0.00069 0.00032 0.00027 0.00000 0.00261 0.00318 0.00249 0.00220 0.00200 0.00227 0.00113 H3 1.06368 0.25873 1.10494 1.00000 0.03521 0.00000 0.00000 C4 0.95759 0.26621 0.99346 1.00000 0.02769 0.02850 0.02061 -0.00427 0.00420 0.00137 0.02550 0.00860 0.00066 0.00030 0.00025 0.00000 0.00256 0.00282 0.00242 0.00203 0.00197 0.00206 0.00106 H4 0.96889 0.32134 0.98922 1.00000 0.03061 0.00000 0.00000 C5 0.88699 0.22159 0.93120 1.00000 0.01953 0.02821 0.01655 -0.00095 0.00239 0.00253 0.02142 0.00831 0.00062 0.00028 0.00025 0.00000 0.00229 0.00266 0.00222 0.00195 0.00178 0.00195 0.00097 C6 0.83119 0.25306 0.85452 1.00000 0.01844 0.02736 0.01976 -0.00177 0.00406 -0.00018 0.02171 0.00830 0.00063 0.00028 0.00025 0.00000 0.00227 0.00267 0.00234 0.00191 0.00182 0.00186 0.00099 C7 0.82261 0.33058 0.83258 1.00000 0.02942 0.02349 0.02173 -0.00394 0.00523 -0.00514 0.02471 0.00861 0.00067 0.00028 0.00026 0.00000 0.00263 0.00259 0.00244 0.00200 0.00199 0.00201 0.00104 H7 0.85574 0.37108 0.86831 1.00000 0.02965 0.00000 0.00000 C8 0.76418 0.34808 0.75671 1.00000 0.03214 0.02591 0.02065 0.00357 0.00474 0.00058 0.02612 0.00887 0.00069 0.00029 0.00026 0.00000 0.00267 0.00274 0.00245 0.00203 0.00202 0.00210 0.00107 H8 0.75878 0.40104 0.74050 1.00000 0.03134 0.00000 0.00000 C9 0.71416 0.28915 0.70501 1.00000 0.03548 0.02811 0.01851 0.00762 0.00617 0.00263 0.02713 0.00924 0.00070 0.00029 0.00027 0.00000 0.00285 0.00274 0.00244 0.00203 0.00209 0.00216 0.00110 H9 0.67153 0.30062 0.65352 1.00000 0.03256 0.00000 0.00000 C10 0.72824 0.21303 0.73073 1.00000 0.02485 0.02532 0.01815 -0.00101 0.00286 0.00032 0.02276 0.00846 0.00066 0.00028 0.00025 0.00000 0.00244 0.00259 0.00234 0.00193 0.00187 0.00195 0.00100 C11 0.68247 0.14174 0.68435 1.00000 0.03038 0.02911 0.01602 0.00465 0.00093 -0.00196 0.02535 0.00868 0.00068 0.00029 0.00026 0.00000 0.00261 0.00280 0.00235 0.00196 0.00194 0.00209 0.00106 C12 0.67645 -0.05761 0.69934 1.00000 0.02947 0.03211 0.00876 0.00315 -0.00063 -0.00379 0.02371 0.00827 0.00065 0.00028 0.00024 0.00000 0.00259 0.00288 0.00207 0.00190 0.00184 0.00205 0.00105 H12 0.71700 -0.06362 0.75186 1.00000 0.02845 0.00000 0.00000 C13 0.64973 -0.12722 0.65423 1.00000 0.02503 0.02860 0.01678 0.00046 0.00196 -0.00335 0.02353 0.00841 0.00066 0.00029 0.00025 0.00000 0.00243 0.00271 0.00228 0.00197 0.00187 0.00202 0.00101 C14 0.69388 -0.19867 0.69116 1.00000 0.02667 0.02808 0.01274 0.00605 -0.00105 0.00137 0.02280 0.00846 0.00065 0.00027 0.00025 0.00000 0.00250 0.00275 0.00217 0.00192 0.00185 0.00199 0.00102 H14 0.73869 -0.19822 0.74368 1.00000 0.02736 0.00000 0.00000 C15 0.67473 -0.26918 0.65422 1.00000 0.02941 0.02391 0.01987 0.00593 0.00318 0.00230 0.02439 0.00868 0.00066 0.00029 0.00026 0.00000 0.00260 0.00261 0.00236 0.00197 0.00194 0.00203 0.00103 H15 0.70276 -0.31680 0.68077 1.00000 0.02927 0.00000 0.00000 C16 0.61310 -0.26924 0.57670 1.00000 0.03112 0.02428 0.01913 -0.00222 0.00464 -0.00225 0.02472 0.00860 0.00067 0.00029 0.00025 0.00000 0.00263 0.00265 0.00234 0.00198 0.00196 0.00208 0.00103 H16 0.60274 -0.31745 0.55006 1.00000 0.02966 0.00000 0.00000 C17 0.56691 -0.20039 0.53804 1.00000 0.03674 0.02386 0.01460 0.00114 0.00493 -0.00104 0.02492 0.00873 0.00069 0.00027 0.00026 0.00000 0.00282 0.00267 0.00229 0.00191 0.00201 0.00206 0.00106 H17 0.52451 -0.20211 0.48535 1.00000 0.02991 0.00000 0.00000 C18 0.58153 -0.12804 0.57525 1.00000 0.02574 0.02296 0.01411 0.00104 0.00328 -0.00146 0.02087 0.00811 0.00064 0.00027 0.00024 0.00000 0.00244 0.00253 0.00217 0.00187 0.00184 0.00194 0.00097 N1 0.86589 0.14318 0.93645 1.00000 0.02304 0.02572 0.01360 0.00139 0.00158 0.00183 0.02085 0.00672 0.00052 0.00022 0.00020 0.00000 0.00199 0.00223 0.00188 0.00157 0.00152 0.00162 0.00083 N2 0.78363 0.19635 0.80326 1.00000 0.02570 0.02192 0.01613 -0.00051 0.00334 0.00150 0.02119 0.00678 0.00053 0.00022 0.00021 0.00000 0.00210 0.00213 0.00190 0.00159 0.00157 0.00162 0.00083 N3 0.68825 0.07541 0.72328 1.00000 0.03312 0.02533 0.01530 0.00075 -0.00180 -0.00147 0.02501 0.00695 0.00056 0.00023 0.00021 0.00000 0.00225 0.00225 0.00190 0.00167 0.00162 0.00173 0.00088 N4 0.64924 0.01248 0.67351 1.00000 0.03796 0.02293 0.01322 -0.00249 -0.00360 -0.00287 0.02530 0.00691 0.00058 0.00024 0.00021 0.00000 0.00238 0.00222 0.00189 0.00161 0.00165 0.00176 0.00089 O1 0.64517 0.14713 0.61306 1.00000 0.05264 0.02306 0.01253 0.00461 -0.00485 -0.00427 0.03019 0.00589 0.00051 0.00019 0.00017 0.00000 0.00219 0.00188 0.00164 0.00135 0.00147 0.00156 0.00080 O2 0.52972 -0.06209 0.53649 1.00000 0.05499 0.02112 0.01174 0.00221 -0.00107 0.00174 0.02975 0.00600 0.00051 0.00019 0.00017 0.00000 0.00228 0.00183 0.00159 0.00134 0.00149 0.00155 0.00080 Cu1 0.77932 0.08850 0.83674 1.00000 0.02883 0.02124 0.01369 0.00085 0.00017 -0.00027 0.02147 0.00100 0.00008 0.00003 0.00003 0.00000 0.00033 0.00031 0.00028 0.00023 0.00022 0.00024 0.00017 Cu2 0.57384 0.04438 0.57012 1.00000 0.07415 0.02085 0.01389 0.00224 -0.00868 -0.00336 0.03754 0.00116 0.00011 0.00004 0.00003 0.00000 0.00051 0.00035 0.00031 0.00025 0.00029 0.00032 0.00021 N11 0.53068 -0.01193 0.89497 1.00000 0.03079 0.02777 0.01947 -0.00325 0.00096 -0.00341 0.02621 0.00700 0.00058 0.00025 0.00021 0.00000 0.00244 0.00244 0.00210 0.00175 0.00176 0.00188 0.00092 O11 0.70736 -0.01303 0.87929 1.00000 0.02878 0.02603 0.01949 0.00321 0.00281 0.00195 0.02479 0.00581 0.00046 0.00019 0.00017 0.00000 0.00191 0.00185 0.00168 0.00137 0.00138 0.00139 0.00074 O12 0.43968 0.05055 0.88329 1.00000 0.03106 0.02903 0.04837 -0.00264 0.00116 0.00397 0.03649 0.00666 0.00049 0.00022 0.00022 0.00000 0.00195 0.00213 0.00236 0.00173 0.00168 0.00162 0.00088 O13 0.46202 -0.07080 0.91980 1.00000 0.04900 0.03558 0.04442 0.00770 0.01234 -0.01277 0.04245 0.00714 0.00056 0.00023 0.00022 0.00000 0.00239 0.00231 0.00237 0.00182 0.00188 0.00180 0.00097 N21 1.17604 0.07982 0.65323 1.00000 0.05629 0.02945 0.01965 -0.00121 0.00024 -0.00349 0.03553 0.00804 0.00068 0.00027 0.00023 0.00000 0.00295 0.00264 0.00223 0.00193 0.00199 0.00219 0.00106 O21 1.12180 0.01688 0.67683 1.00000 0.08955 0.02878 0.04637 -0.00426 0.03310 -0.00540 0.05278 0.00822 0.00067 0.00024 0.00023 0.00000 0.00334 0.00231 0.00256 0.00190 0.00234 0.00215 0.00116 O22 1.17600 0.13879 0.69242 1.00000 0.13871 0.03318 0.02072 -0.00380 -0.00115 -0.01251 0.06519 0.00808 0.00081 0.00025 0.00022 0.00000 0.00452 0.00247 0.00204 0.00183 0.00240 0.00261 0.00143 O23 1.22421 0.08280 0.58679 1.00000 0.06883 0.05809 0.01870 0.00081 0.00681 -0.01620 0.04844 0.00712 0.00062 0.00025 0.00020 0.00000 0.00277 0.00284 0.00188 0.00182 0.00181 0.00221 0.00107 O1W 1.05115 0.02720 0.82468 1.00000 0.02788 0.03873 0.01896 0.00013 0.00292 0.00105 0.02853 0.00626 0.00046 0.00022 0.00019 0.00000 0.00188 0.00218 0.00172 0.00156 0.00144 0.00156 0.00079 H1WA 1.15811 0.03157 0.85013 1.00000 0.03424 0.05947 0.00418 0.00320 0.00202 0.00000 0.00000 H1WB 1.05984 0.03732 0.78002 1.00000 0.03424 0.07860 0.00630 0.00316 0.00119 0.00000 0.00000 O2W 0.87220 0.04037 0.50972 1.00000 0.14621 0.11392 0.09852 0.00961 0.00366 -0.00709 0.12059 0.01361 0.00111 0.00044 0.00041 0.00000 0.00641 0.00609 0.00524 0.00443 0.00446 0.00471 0.00240 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 331 Maximum vector length = 511 Memory required = 3267 / 24017 wR2 = 0.1412 before cycle 20 for 4743 data and 0 / 331 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.015 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0580 * P )^2 + 3.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0631 for 3315 Fo > 4sig(Fo) and 0.1022 for all 4743 data wR2 = 0.1412, GooF = S = 1.063, Restrained GooF = 1.063 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0310 0.0244 0.0197 C1 0.0450 0.0295 0.0172 C2 0.0404 0.0299 0.0177 C3 0.0308 0.0275 0.0182 C4 0.0290 0.0189 0.0164 C5 0.0278 0.0204 0.0170 C6 0.0331 0.0226 0.0184 C7 0.0323 0.0275 0.0186 C8 0.0373 0.0301 0.0140 C9 0.0256 0.0247 0.0180 C10 0.0335 0.0280 0.0145 C11 0.0360 0.0269 0.0083 C12 0.0308 0.0231 0.0168 C13 0.0302 0.0280 0.0102 C14 0.0305 0.0270 0.0156 C15 0.0319 0.0241 0.0181 C16 0.0368 0.0239 0.0140 C17 0.0264 0.0225 0.0137 C18 0.0267 0.0225 0.0134 N1 0.0262 0.0215 0.0159 N2 0.0354 0.0251 0.0146 N3 0.0410 0.0235 0.0114 N4 0.0569 0.0234 0.0103 O1 0.0566 0.0216 0.0111 O2 0.0297 0.0213 0.0134 Cu1 0.0798 0.0209 0.0119 Cu2 0.0331 0.0276 0.0179 N11 0.0298 0.0264 0.0182 O11 0.0505 0.0331 0.0259 O12 0.0567 0.0488 0.0218 O13 0.0580 0.0293 0.0193 N21 0.0984 0.0323 0.0277 O21 0.1431 0.0332 0.0192 O22 0.0807 0.0464 0.0182 O23 0.0388 0.0278 0.0189 O1W 0.1534 0.1148 0.0935 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.029 0.044 0.058 0.074 0.093 0.120 0.158 0.217 1.000 Number in group 504. 448. 509. 469. 465. 451. 483. 471. 466. 477. GooF 1.104 1.077 1.101 1.120 1.092 1.061 0.960 1.046 0.996 1.063 K 7.486 1.929 1.392 1.150 1.060 1.042 1.024 1.003 0.996 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 482. 477. 478. 481. 455. 477. 482. 462. 471. 478. GooF 1.053 1.048 1.108 1.070 1.033 0.989 1.002 0.919 0.936 1.394 K 1.120 1.144 1.080 1.062 1.026 1.002 0.998 0.998 1.001 1.018 R1 0.271 0.226 0.187 0.149 0.119 0.101 0.072 0.048 0.038 0.043 Recommended weighting scheme: WGHT 0.0579 3.3923 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 1 5 3076.72 2124.64 4.98 0.183 2.95 1 20 5 704.88 131.67 4.16 0.046 0.82 -2 2 3 116.08 29.92 4.10 0.022 2.96 4 1 4 445.57 139.34 4.09 0.047 1.54 0 0 4 30349.24 22101.94 3.94 0.591 4.43 0 2 4 15578.64 12051.38 3.87 0.436 3.93 0 7 6 466.68 263.41 3.79 0.065 1.88 2 17 6 776.97 372.33 3.73 0.077 0.91 1 3 7 82.31 205.60 3.65 0.057 2.12 1 3 5 708.98 487.77 3.59 0.088 2.65 2 11 18 416.11 26.12 3.59 0.020 0.79 -1 7 5 2248.70 1703.87 3.53 0.164 1.97 -2 3 2 641.11 914.58 3.51 0.120 2.90 -2 13 17 -54.80 251.48 3.46 0.063 0.81 5 4 4 152.79 19.58 3.44 0.018 1.22 0 1 8 19540.03 15626.02 3.44 0.497 2.20 -2 13 18 -133.65 179.07 3.29 0.053 0.79 6 6 7 206.12 0.64 3.22 0.003 0.94 0 18 5 357.10 89.06 3.22 0.038 0.92 -1 2 4 643.20 457.90 3.18 0.085 3.60 -2 11 16 254.98 30.51 3.16 0.022 0.90 0 2 9 3956.65 3164.31 3.15 0.224 1.92 0 1 7 23106.55 18873.26 3.10 0.546 2.50 -7 5 8 0.00 204.42 3.08 0.057 0.91 0 1 10 1352.21 1037.79 3.06 0.128 1.76 -4 12 6 196.07 59.02 3.05 0.031 1.06 -7 7 9 388.66 113.03 3.03 0.042 0.87 -6 10 8 303.99 139.22 3.01 0.047 0.91 6 1 15 678.22 256.34 2.97 0.064 0.78 1 2 5 2125.25 1683.91 2.96 0.163 2.83 -1 16 4 1065.15 684.99 2.94 0.104 1.03 -2 6 1 210.89 336.28 2.94 0.073 2.20 0 8 2 102.00 222.86 2.94 0.059 2.08 -1 1 3 7452.82 6093.43 2.93 0.310 4.62 -4 7 13 126.11 1.75 2.93 0.005 1.04 1 4 1 1260.40 970.37 2.86 0.124 3.51 1 1 4 104.38 22.39 2.86 0.019 3.45 2 9 0 1746.21 2199.39 2.85 0.186 1.66 6 11 4 252.76 28.39 2.80 0.021 0.89 -2 10 1 279.41 453.75 2.79 0.085 1.53 4 9 16 467.52 6.30 2.79 0.010 0.80 0 3 7 10930.64 9078.45 2.79 0.379 2.31 -6 3 1 64.54 0.88 2.79 0.004 1.13 -3 16 6 285.24 90.13 2.78 0.038 0.94 -3 18 11 741.24 394.71 2.76 0.079 0.79 0 8 0 2406.63 3030.30 2.71 0.219 2.14 -3 19 8 244.92 21.24 2.68 0.018 0.80 6 0 6 134.42 0.02 2.67 0.001 1.03 -1 4 6 194.05 102.61 2.67 0.040 2.37 5 13 10 950.26 599.85 2.66 0.097 0.81 Bond lengths and angles C1 - Distance Angles N1 1.3378 (0.0058) C2 1.3939 (0.0067) 121.81 (0.46) H1 0.9500 119.09 119.09 C1 - N1 C2 C2 - Distance Angles C3 1.3661 (0.0073) C1 1.3939 (0.0067) 119.11 (0.46) H2 0.9500 120.45 120.45 C2 - C3 C1 C3 - Distance Angles C2 1.3661 (0.0073) C4 1.3856 (0.0067) 119.47 (0.46) H3 0.9500 120.27 120.27 C3 - C2 C4 C4 - Distance Angles C3 1.3856 (0.0067) C5 1.3859 (0.0064) 119.09 (0.47) H4 0.9500 120.46 120.46 C4 - C3 C5 C5 - Distance Angles N1 1.3535 (0.0060) C4 1.3859 (0.0064) 121.35 (0.42) C6 1.4764 (0.0063) 114.04 (0.39) 124.60 (0.44) C5 - N1 C4 C6 - Distance Angles N2 1.3456 (0.0058) C7 1.3815 (0.0067) 120.04 (0.42) C5 1.4764 (0.0063) 112.40 (0.41) 127.56 (0.43) C6 - N2 C7 C7 - Distance Angles C6 1.3815 (0.0067) C8 1.3965 (0.0066) 118.53 (0.44) H7 0.9500 120.73 120.73 C7 - C6 C8 C8 - Distance Angles C9 1.3810 (0.0067) C7 1.3965 (0.0066) 120.63 (0.45) H8 0.9500 119.69 119.68 C8 - C9 C7 C9 - Distance Angles C10 1.3797 (0.0065) C8 1.3810 (0.0067) 117.70 (0.43) H9 0.9500 121.15 121.15 C9 - C10 C8 C10 - Distance Angles N2 1.3344 (0.0058) C9 1.3797 (0.0065) 121.63 (0.44) C11 1.4854 (0.0067) 112.37 (0.40) 125.99 (0.42) C10 - N2 C9 C11 - Distance Angles O1 1.2698 (0.0055) N3 1.3283 (0.0059) 125.13 (0.45) C10 1.4854 (0.0067) 120.09 (0.42) 114.77 (0.40) C11 - O1 N3 C12 - Distance Angles N4 1.2897 (0.0060) C13 1.4361 (0.0066) 124.56 (0.41) H12 0.9500 117.72 117.72 C12 - N4 C13 C13 - Distance Angles C14 1.4038 (0.0065) C18 1.4297 (0.0062) 118.70 (0.43) C12 1.4361 (0.0066) 116.94 (0.40) 124.36 (0.43) C13 - C14 C18 C14 - Distance Angles C15 1.3727 (0.0066) C13 1.4038 (0.0065) 122.47 (0.42) H14 0.9500 118.77 118.77 C14 - C15 C13 C15 - Distance Angles C14 1.3727 (0.0066) C16 1.3961 (0.0064) 118.42 (0.44) H15 0.9500 120.79 120.79 C15 - C14 C16 C16 - Distance Angles C17 1.3818 (0.0066) C15 1.3961 (0.0064) 121.15 (0.45) H16 0.9500 119.43 119.43 C16 - C17 C15 C17 - Distance Angles C16 1.3818 (0.0066) C18 1.4020 (0.0065) 121.13 (0.43) H17 0.9500 119.43 119.43 C17 - C16 C18 C18 - Distance Angles O2 1.3480 (0.0054) C17 1.4020 (0.0065) 119.76 (0.39) C13 1.4297 (0.0062) 122.13 (0.41) 118.10 (0.42) C18 - O2 C17 N1 - Distance Angles C1 1.3378 (0.0058) C5 1.3535 (0.0060) 119.13 (0.40) Cu1 2.0332 (0.0037) 126.07 (0.32) 114.68 (0.28) N1 - C1 C5 N2 - Distance Angles C10 1.3344 (0.0057) C6 1.3456 (0.0058) 121.45 (0.40) Cu1 1.9402 (0.0037) 119.24 (0.32) 119.18 (0.30) N2 - C10 C6 N3 - Distance Angles C11 1.3283 (0.0059) N4 1.4001 (0.0053) 109.49 (0.37) Cu1 2.0567 (0.0038) 114.06 (0.31) 136.01 (0.30) N3 - C11 N4 N4 - Distance Angles C12 1.2897 (0.0060) N3 1.4001 (0.0053) 118.66 (0.38) Cu2 1.9326 (0.0038) 127.85 (0.33) 113.37 (0.29) N4 - C12 N3 O1 - Distance Angles C11 1.2698 (0.0055) Cu2 1.9558 (0.0033) 109.70 (0.30) O1 - C11 O2 - Distance Angles C18 1.3480 (0.0054) Cu2 1.9295 (0.0033) 127.45 (0.28) Cu2_$2 1.9712 (0.0031) 131.71 (0.28) 100.35 (0.14) O2 - C18 Cu2 Cu1 - Distance Angles N2 1.9402 (0.0038) O11 1.9850 (0.0033) 164.59 (0.14) N1 2.0332 (0.0037) 79.53 (0.15) 97.35 (0.14) N3 2.0567 (0.0038) 79.32 (0.16) 102.77 (0.15) 158.83 (0.16) O1W 2.1970 (0.0033) 112.08 (0.14) 83.25 (0.13) 98.22 (0.14) 90.69 (0.14) Cu1 - N2 O11 N1 N3 Cu2 - Distance Angles O2 1.9295 (0.0033) N4 1.9326 (0.0038) 92.53 (0.15) O1 1.9558 (0.0033) 172.84 (0.14) 81.64 (0.15) O2_$2 1.9712 (0.0031) 79.65 (0.14) 170.89 (0.16) 106.49 (0.13) Cu2_$2 2.9958 (0.0012) 40.34 (0.09) 132.69 (0.13) 145.67 (0.10) 39.31 (0.09) Cu2 - O2 N4 O1 O2_$2 N11 - Distance Angles O13 1.2217 (0.0052) O12 1.2458 (0.0052) 123.61 (0.43) O11 1.2954 (0.0050) 119.50 (0.42) 116.89 (0.39) N11 - O13 O12 O11 - Distance Angles N11 1.2954 (0.0050) Cu1 1.9850 (0.0032) 111.27 (0.27) O11 - N11 O12 - Distance Angles N11 1.2458 (0.0052) O12 - O13 - Distance Angles N11 1.2217 (0.0053) O13 - N21 - Distance Angles O22 1.2276 (0.0056) O21 1.2325 (0.0056) 120.00 (0.43) O23 1.2747 (0.0054) 121.15 (0.46) 118.79 (0.44) N21 - O22 O21 O21 - Distance Angles N21 1.2325 (0.0056) O21 - O22 - Distance Angles N21 1.2276 (0.0056) O22 - O23 - Distance Angles N21 1.2747 (0.0054) O23 - O1W - Distance Angles Cu1 2.1970 (0.0033) H1WA 0.8244 (0.0189) 129.08 (3.71) H1WB 0.8259 (0.0187) 99.49 (3.43) 109.94 (3.08) O1W - Cu1 H1WA Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.826(19) 1.98(3) 2.753(5) 156(5) O1W-H1WB...O21 0.824(19) 2.00(2) 2.800(5) 164(4) O1W-H1WA...O12_$1 FMAP and GRID set by program FMAP 2 1 18 GRID -3.333 -2 -1 3.333 2 1 R1 = 0.0989 for 4743 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.74 at 0.1308 0.9593 0.4919 [ 0.03 A from O2W ] Deepest hole -0.85 at 0.4639 0.4552 0.0865 [ 0.85 A from CU2 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3843 / 37233 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7418 0.1432 0.8161 1.00000 0.05 0.71 0.99 N2 1.03 CU1 1.93 C10 2.02 N3 Q2 1 0.6026 0.1005 0.5907 1.00000 0.05 0.67 0.92 O1 1.04 CU2 1.83 C11 2.11 N4 Q3 1 0.6955 0.0218 0.5794 1.00000 0.05 0.62 0.93 CU2 1.76 N4 1.88 O2W 1.94 O2 Q4 1 0.6944 0.0757 0.5890 1.00000 0.05 0.59 1.02 CU2 1.35 O1 1.91 N4 2.05 C11 Q5 1 0.9014 0.1170 0.8517 1.00000 0.05 0.58 0.99 CU1 1.63 N1 1.76 N2 1.95 O1W Q6 1 0.8685 0.0403 0.8505 1.00000 0.05 0.58 1.04 CU1 1.42 O1W 1.58 O11 1.95 H1WB Q7 1 0.7968 0.1403 0.8488 1.00000 0.05 0.55 0.92 CU1 1.25 N2 1.58 N1 1.94 C6 Q8 1 0.6355 0.1030 0.8218 1.00000 0.05 0.52 1.03 CU1 1.90 N3 1.95 N2 2.06 O12 Q9 1 1.2387 0.0241 0.5776 1.00000 0.05 0.52 1.02 O23 1.75 N21 1.98 O2W 2.05 O21 Q10 1 1.3023 0.1127 0.6950 1.00000 0.05 0.48 0.98 O22 1.22 N21 2.01 O23 2.06 O21 Shortest distances between peaks (including symmetry equivalents) 1 7 0.66 2 4 0.77 5 7 0.83 3 4 0.94 1 8 1.02 1 5 1.29 7 8 1.33 5 6 1.33 2 3 1.52 6 7 1.78 5 8 1.87 6 8 1.96 1 6 2.03 9 10 2.58 2 9 2.83 2 10 2.98 Time profile in seconds ----------------------- 0.22: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 2.48: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.02: Generate idealized H-atoms 10.56: Structure factors and derivatives 24.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 2.78: Solve l.s. equations 0.00: Generate HTAB table 0.22: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:52:38 Total CPU time: 41.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++