+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:21:47 on 20-Oct-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 9.3024 9.7983 10.0972 110.719 109.620 102.964 ZERR 1.00 0.0005 0.0006 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H N O CL CU UNIT 24 24 10 12 2 2 V = 746.81 F(000) = 426.0 Mu = 1.69 mm-1 Cell Wt = 842.51 Rho = 1.873 MERG 2 OMIT -3.00 55.00 OMIT 1 -2 3 OMIT -2 2 2 OMIT -1 -1 3 OMIT 0 -1 3 OMIT 2 -3 4 OMIT -6 5 2 EXTI 0.02968 SHEL 7 0.77 DFIX 0.84 0.01 O1 H1A O1 H1B DANG 1.35 0.01 H1A H1B DFIX 0.84 0.01 O1W H1WA O1W H1WB DANG 1.35 0.01 H1WA H1WB EQIV $1 -X, -Y, -Z-1 EQIV $2 -X-1, -Y, -Z-1 HTAB O1 O1W_$1 HTAB O1 O24 HTAB O1W N4_$2 HTAB O1W O23 FMAP 2 ACTA PLAN 5 SIZE 0.12 0.18 0.20 BOND $H WGHT 0.06270 1.68830 L.S. 18 TEMP -153.00 FVAR 0.39494 MOLE 1 C1 1 0.309451 0.573598 0.299815 11.00000 0.03113 0.04518 = 0.03947 0.02629 0.02217 0.02389 AFIX 43 H1 2 0.420242 0.580121 0.340435 11.00000 -1.20000 AFIX 0 C2 1 0.282999 0.712058 0.340854 11.00000 0.03703 0.04093 = 0.03249 0.01792 0.02071 0.02060 AFIX 43 H2 2 0.373963 0.811635 0.406298 11.00000 -1.20000 AFIX 0 C3 1 0.122815 0.704367 0.285768 11.00000 0.04051 0.04272 = 0.03685 0.02309 0.02278 0.02932 AFIX 43 H3 2 0.101823 0.798512 0.314055 11.00000 -1.20000 AFIX 0 C4 1 -0.006717 0.558074 0.188953 11.00000 0.03308 0.04328 = 0.04071 0.02509 0.02392 0.02799 AFIX 43 H4 2 -0.118089 0.550091 0.149707 11.00000 -1.20000 AFIX 0 C5 1 0.027850 0.423809 0.150064 11.00000 0.03164 0.04388 = 0.04061 0.02969 0.02570 0.02622 C6 1 -0.096963 0.262993 0.050977 11.00000 0.03256 0.04209 = 0.05161 0.03461 0.03083 0.02910 C7 1 -0.302875 0.048432 -0.088460 11.00000 0.02807 0.04686 = 0.04103 0.03312 0.02257 0.02644 C8 1 -0.461262 -0.086029 -0.180658 11.00000 0.02989 0.04497 = 0.03141 0.02386 0.01821 0.02421 C9 1 -0.614130 -0.075649 -0.233480 11.00000 0.03062 0.05350 = 0.02995 0.02004 0.01539 0.02807 AFIX 43 H9 2 -0.621376 0.024378 -0.212578 11.00000 -1.20000 AFIX 0 C10 1 -0.756643 -0.212566 -0.317196 11.00000 0.02552 0.06779 = 0.03420 0.02179 0.01128 0.02893 AFIX 43 H10 2 -0.862696 -0.207864 -0.356003 11.00000 -1.20000 AFIX 0 C11 1 -0.742364 -0.355757 -0.343390 11.00000 0.02788 0.05072 = 0.02951 0.01328 0.01321 0.02127 AFIX 43 H11 2 -0.838027 -0.451412 -0.399753 11.00000 -1.20000 AFIX 0 C12 1 -0.585396 -0.356648 -0.285597 11.00000 0.02730 0.04726 = 0.03447 0.02113 0.01649 0.02218 AFIX 43 H12 2 -0.575803 -0.455071 -0.301482 11.00000 -1.20000 AFIX 0 N1 3 0.186582 0.430324 0.205470 11.00000 0.02973 0.04041 = 0.04205 0.02896 0.02368 0.02477 N2 3 -0.038325 0.149322 0.035841 11.00000 0.02828 0.04238 = 0.07960 0.04465 0.03440 0.02563 N3 3 -0.170443 0.010887 -0.053681 11.00000 0.02425 0.04148 = 0.06919 0.03979 0.02717 0.02285 N4 3 -0.263167 0.205988 -0.024486 11.00000 0.02903 0.04461 = 0.03813 0.02876 0.02145 0.02761 N5 3 -0.447406 -0.227503 -0.209146 11.00000 0.02465 0.04386 = 0.03586 0.02345 0.01908 0.02212 O1 4 0.212481 0.228463 -0.087392 11.00000 0.03111 0.03625 = 0.03122 0.00994 0.00844 0.01558 CU1 6 0.200734 0.209252 0.122906 11.00000 0.02437 0.04084 = 0.07511 0.04092 0.02916 0.02348 H1A 2 0.308586 0.253510 -0.078637 11.00000 -1.50000 H1B 2 0.148752 0.155503 -0.179832 11.00000 -1.50000 MOLE 2 O21 4 -0.164887 -0.264351 -0.594339 11.00000 0.06830 0.06276 = 0.05454 0.01613 0.04115 0.03448 O22 4 -0.280529 -0.275722 -0.425548 11.00000 0.06047 0.04363 = 0.04708 0.02036 0.02806 0.01417 O23 4 -0.304187 -0.099899 -0.530326 11.00000 0.04598 0.07147 = 0.07029 0.03700 0.01133 0.04149 O24 4 -0.047435 -0.053295 -0.337529 11.00000 0.03311 0.03613 = 0.05298 0.00753 0.00080 0.00930 CL21 5 -0.199160 -0.172556 -0.472039 11.00000 0.02542 0.03774 = 0.02909 0.01434 0.01080 0.01721 MOLE 3 O1W 4 -0.502285 -0.352550 -0.909648 11.00000 0.05470 0.13238 = 0.10151 0.09362 0.05596 0.07198 H1WA 2 -0.575602 -0.321280 -0.947232 11.00000 -1.50000 H1WB 2 -0.457250 -0.299110 -0.810431 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 CU 1.280 C1 - N1 C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - N1 C4 C6 C6 - N2 N4 C5 C7 - N3 N4 C8 C8 - N5 C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - N5 C11 N1 - C1 C5 Cu1 N2 - C6 N3 Cu1 N3 - C7 N2 Cu1_$3 N4 - C6 C7 N5 - C12 C8 Cu1_$3 O1 - Cu1 Cu1 - N3_$3 N2 N1 N5_$3 O1 O21 - Cl21 O22 - Cl21 O23 - Cl21 O24 - Cl21 Cl21 - O23 O21 O22 O24 O1W - no bonds found Operators for generating equivalent atoms: $1 -x, -y, -z-1 $2 -x-1, -y, -z-1 $3 -x, -y, -z 12290 Reflections read, of which 27 rejected -11 =< h =< 12, -12 =< k =< 12, -12 =< l =< 13, Max. 2-theta = 54.86 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 2 0 82.94 1.29 7 9.06 -9 4 3 81.41 4.21 4 22.96 1 2 5 72.23 1.25 7 7.33 3 Inconsistent equivalents 3346 Unique reflections, of which 0 suppressed R(int) = 0.0549 R(sigma) = 0.0629 Friedel opposites merged Maximum memory for data reduction = 2244 / 34457 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 = 2837 / 298455 wR2 = 0.1470 before cycle 1 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39502 0.00149 0.055 OSF 2 0.02983 0.00441 0.034 EXTI Mean shift/esd = 0.013 Maximum = 0.079 for U33 Cu1 Max. shift = 0.002 A for H1A Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1471 before cycle 2 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39506 0.00149 0.028 OSF 2 0.02991 0.00442 0.018 EXTI Mean shift/esd = 0.005 Maximum = 0.028 for OSF Max. shift = 0.001 A for H1A Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 3 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.001 OSF 2 0.02992 0.00442 0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for y H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for O24 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 4 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.001 OSF 2 0.02992 0.00442 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for y H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1471 before cycle 5 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for z H1WA Max. shift = 0.000 A for H1WB Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 6 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for z H1WA Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O1W Least-squares cycle 7 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 7 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z H1WA Max. shift = 0.000 A for H1WB Max. dU = 0.000 for N2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 8 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z H1WA Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O21 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 9 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O1W Least-squares cycle 10 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 10 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O22 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 11 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O23 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 12 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O23 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 13 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 Cu1 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O22 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 14 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Cu1 Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O1W Least-squares cycle 15 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 15 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WA Max. dU = 0.000 for N2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 16 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O21 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1470 before cycle 17 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WA Max. dU = 0.000 for O21 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2837 / 298455 wR2 = 0.1471 before cycle 18 for 3346 data and 239 / 239 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39507 0.00149 0.000 OSF 2 0.02992 0.00442 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1WB Max. dU = 0.000 for O1W Largest correlation matrix elements 0.900 y H1WA / x H1WA 0.740 U13 O1W / U23 O1W 0.698 EXTI / OSF 0.862 z H1A / x H1A 0.737 U13 O1W / U11 O1W 0.695 U23 N2 / U22 N2 0.784 U12 O1W / U13 O1W 0.736 U12 O1W / U22 O1W 0.692 U13 O1W / U33 O1W 0.782 U23 O1W / U22 O1W 0.728 U23 Cu1 / U22 Cu1 0.688 U13 Cu1 / U11 Cu1 0.779 x H1B / z H1A 0.728 U23 Cu1 / U33 Cu1 0.680 U23 N2 / U33 N2 0.775 x H1B / x H1A 0.727 U12 O1W / U23 O1W 0.679 U12 Cu1 / U11 Cu1 0.767 U23 O1W / U33 O1W 0.707 U12 Cu1 / U13 Cu1 0.677 U23 C7 / U22 C7 0.753 U12 O1W / U11 O1W -0.701 z H1B / y H1B 0.677 U13 Cu1 / U33 Cu1 Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.4202 0.5801 0.3405 43 0.950 0.000 C1 N1 C2 H2 0.3740 0.8116 0.4063 43 0.950 0.000 C2 C1 C3 H3 0.1018 0.7985 0.3141 43 0.950 0.000 C3 C2 C4 H4 -0.1181 0.5501 0.1497 43 0.950 0.000 C4 C5 C3 H9 -0.6214 0.0244 -0.2126 43 0.950 0.000 C9 C8 C10 H10 -0.8627 -0.2079 -0.3560 43 0.950 0.000 C10 C11 C9 H11 -0.8380 -0.4514 -0.3998 43 0.950 0.000 C11 C10 C12 H12 -0.5758 -0.4551 -0.3015 43 0.950 0.000 C12 N5 C11 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30945 0.57360 0.29982 1.00000 0.03116 0.04518 0.03951 0.02631 0.02219 0.02389 0.03278 0.01312 0.00055 0.00056 0.00054 0.00000 0.00228 0.00268 0.00246 0.00223 0.00207 0.00219 0.00100 H1 0.42024 0.58013 0.34046 1.00000 0.03934 0.00000 0.00000 C2 0.28299 0.71205 0.34085 1.00000 0.03707 0.04097 0.03251 0.01793 0.02074 0.02061 0.03400 0.01333 0.00058 0.00058 0.00054 0.00000 0.00245 0.00253 0.00227 0.00206 0.00204 0.00211 0.00099 H2 0.37395 0.81162 0.40629 1.00000 0.04080 0.00000 0.00000 C3 0.12282 0.70437 0.28578 1.00000 0.04055 0.04278 0.03692 0.02313 0.02281 0.02934 0.03438 0.01317 0.00056 0.00056 0.00054 0.00000 0.00255 0.00261 0.00240 0.00219 0.00216 0.00231 0.00102 H3 0.10183 0.79852 0.31408 1.00000 0.04125 0.00000 0.00000 C4 -0.00673 0.55805 0.18894 1.00000 0.03311 0.04331 0.04071 0.02507 0.02393 0.02800 0.03243 0.01304 0.00055 0.00054 0.00054 0.00000 0.00231 0.00260 0.00244 0.00220 0.00208 0.00218 0.00098 H4 -0.11810 0.55007 0.14967 1.00000 0.03891 0.00000 0.00000 C5 0.02785 0.42382 0.15008 1.00000 0.03165 0.04395 0.04069 0.02973 0.02574 0.02624 0.03032 0.01299 0.00053 0.00054 0.00054 0.00000 0.00221 0.00251 0.00242 0.00216 0.00202 0.00208 0.00095 C6 -0.09697 0.26299 0.05097 1.00000 0.03262 0.04213 0.05166 0.03463 0.03089 0.02914 0.03142 0.01335 0.00053 0.00054 0.00057 0.00000 0.00227 0.00248 0.00273 0.00230 0.00217 0.00210 0.00099 C7 -0.30286 0.04845 -0.08845 1.00000 0.02812 0.04692 0.04109 0.03316 0.02260 0.02645 0.03008 0.01291 0.00051 0.00055 0.00054 0.00000 0.00213 0.00260 0.00241 0.00221 0.00198 0.00205 0.00095 C8 -0.46127 -0.08603 -0.18066 1.00000 0.02992 0.04496 0.03141 0.02384 0.01819 0.02417 0.03023 0.01249 0.00052 0.00054 0.00051 0.00000 0.00221 0.00256 0.00220 0.00207 0.00190 0.00207 0.00095 C9 -0.61412 -0.07565 -0.23347 1.00000 0.03066 0.05349 0.02998 0.02002 0.01540 0.02804 0.03505 0.01308 0.00054 0.00061 0.00052 0.00000 0.00232 0.00283 0.00224 0.00217 0.00196 0.00224 0.00104 H9 -0.62137 0.02438 -0.21256 1.00000 0.04206 0.00000 0.00000 C10 -0.75666 -0.21258 -0.31721 1.00000 0.02553 0.06787 0.03423 0.02181 0.01129 0.02892 0.04179 0.01381 0.00056 0.00066 0.00056 0.00000 0.00227 0.00344 0.00244 0.00247 0.00199 0.00244 0.00120 H10 -0.86271 -0.20788 -0.35602 1.00000 0.05015 0.00000 0.00000 C11 -0.74237 -0.35576 -0.34339 1.00000 0.02791 0.05076 0.02956 0.01331 0.01325 0.02131 0.03663 0.01320 0.00056 0.00061 0.00053 0.00000 0.00225 0.00282 0.00225 0.00214 0.00192 0.00218 0.00106 H11 -0.83802 -0.45142 -0.39976 1.00000 0.04395 0.00000 0.00000 C12 -0.58540 -0.35664 -0.28559 1.00000 0.02731 0.04728 0.03452 0.02114 0.01651 0.02216 0.03342 0.01273 0.00052 0.00058 0.00053 0.00000 0.00223 0.00272 0.00230 0.00216 0.00194 0.00216 0.00101 H12 -0.57581 -0.45507 -0.30147 1.00000 0.04011 0.00000 0.00000 N1 0.18658 0.43033 0.20546 1.00000 0.02975 0.04044 0.04212 0.02899 0.02371 0.02479 0.02975 0.01057 0.00043 0.00044 0.00044 0.00000 0.00187 0.00210 0.00210 0.00184 0.00172 0.00177 0.00081 N2 -0.03832 0.14933 0.03586 1.00000 0.02834 0.04244 0.07970 0.04471 0.03445 0.02566 0.03942 0.01214 0.00045 0.00047 0.00056 0.00000 0.00194 0.00224 0.00302 0.00228 0.00208 0.00184 0.00099 N3 -0.17045 0.01088 -0.05369 1.00000 0.02429 0.04151 0.06928 0.03982 0.02722 0.02288 0.03661 0.01148 0.00043 0.00046 0.00053 0.00000 0.00186 0.00219 0.00275 0.00215 0.00192 0.00179 0.00093 N4 -0.26316 0.20598 -0.02449 1.00000 0.02906 0.04465 0.03817 0.02879 0.02149 0.02764 0.02962 0.01052 0.00043 0.00045 0.00044 0.00000 0.00182 0.00216 0.00198 0.00180 0.00163 0.00172 0.00080 N5 -0.44740 -0.22749 -0.20913 1.00000 0.02468 0.04391 0.03590 0.02347 0.01910 0.02215 0.02984 0.01029 0.00042 0.00045 0.00043 0.00000 0.00179 0.00215 0.00194 0.00177 0.00161 0.00173 0.00080 O1 0.21247 0.22847 -0.08739 1.00000 0.03115 0.03631 0.03126 0.00997 0.00845 0.01561 0.03611 0.00855 0.00039 0.00038 0.00037 0.00000 0.00163 0.00180 0.00163 0.00143 0.00138 0.00149 0.00074 Cu1 0.20073 0.20925 0.12291 1.00000 0.02439 0.04087 0.07516 0.04095 0.02919 0.02349 0.03808 0.00172 0.00006 0.00007 0.00008 0.00000 0.00032 0.00038 0.00050 0.00034 0.00030 0.00026 0.00025 H1A 0.30867 0.25328 -0.07841 1.00000 0.05713 0.10518 0.00234 0.00610 0.00553 0.00000 0.00000 H1B 0.14880 0.15564 -0.17992 1.00000 0.05713 0.04175 0.00439 0.00496 0.00281 0.00000 0.00000 O21 -0.16488 -0.26434 -0.59433 1.00000 0.06827 0.06278 0.05458 0.01618 0.04111 0.03446 0.05972 0.01148 0.00052 0.00049 0.00047 0.00000 0.00257 0.00244 0.00231 0.00201 0.00211 0.00218 0.00108 O22 -0.28055 -0.27571 -0.42555 1.00000 0.06047 0.04365 0.04712 0.02035 0.02806 0.01415 0.05082 0.01013 0.00048 0.00042 0.00044 0.00000 0.00237 0.00201 0.00203 0.00173 0.00189 0.00184 0.00093 O23 -0.30418 -0.09990 -0.53034 1.00000 0.04601 0.07149 0.07034 0.03701 0.01139 0.04150 0.06230 0.01149 0.00047 0.00051 0.00051 0.00000 0.00217 0.00266 0.00265 0.00225 0.00196 0.00210 0.00114 O24 -0.04744 -0.05330 -0.33749 1.00000 0.03320 0.03617 0.05296 0.00751 0.00085 0.00932 0.05181 0.00912 0.00042 0.00040 0.00044 0.00000 0.00181 0.00189 0.00218 0.00171 0.00165 0.00158 0.00098 Cl21 -0.19916 -0.17256 -0.47204 1.00000 0.02544 0.03777 0.02911 0.01435 0.01080 0.01721 0.03071 0.00282 0.00012 0.00013 0.00012 0.00000 0.00052 0.00059 0.00053 0.00046 0.00043 0.00046 0.00029 O1W -0.50228 -0.35254 -0.90962 1.00000 0.05474 0.13243 0.10159 0.09369 0.05600 0.07204 0.06999 0.01527 0.00053 0.00066 0.00059 0.00000 0.00255 0.00430 0.00352 0.00362 0.00269 0.00296 0.00141 H1WA -0.57547 -0.32105 -0.94698 1.00000 0.10499 0.18692 0.00713 0.00839 0.00719 0.00000 0.00000 H1WB -0.45720 -0.29933 -0.81038 1.00000 0.10499 0.13826 0.00898 0.00823 0.00148 0.00000 0.00000 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 239 Maximum vector length = 511 Memory required = 2598 / 25039 wR2 = 0.1470 before cycle 19 for 3346 data and 0 / 239 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.035 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 1.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0532 for 2394 Fo > 4sig(Fo) and 0.0841 for all 3346 data wR2 = 0.1470, GooF = S = 1.036, Restrained GooF = 1.035 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0483 0.0297 0.0203 C1 0.0434 0.0340 0.0246 C2 0.0512 0.0318 0.0201 C3 0.0492 0.0329 0.0152 C4 0.0509 0.0236 0.0165 C5 0.0579 0.0238 0.0125 C6 0.0533 0.0223 0.0146 C7 0.0470 0.0246 0.0191 C8 0.0582 0.0287 0.0182 C9 0.0734 0.0368 0.0152 C10 0.0586 0.0295 0.0217 C11 0.0483 0.0325 0.0195 C12 0.0488 0.0248 0.0156 N1 0.0811 0.0232 0.0139 N2 0.0715 0.0251 0.0132 N3 0.0499 0.0260 0.0129 N4 0.0453 0.0296 0.0146 N5 0.0506 0.0309 0.0268 O1 0.0767 0.0254 0.0121 Cu1 0.0806 0.0719 0.0267 O21 0.0673 0.0443 0.0409 O22 0.0958 0.0735 0.0176 O23 0.0869 0.0417 0.0269 O24 0.0416 0.0302 0.0203 Cl21 0.1470 0.0452 0.0177 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.035 0.052 0.072 0.094 0.120 0.155 0.207 0.300 1.000 Number in group 350. 324. 345. 331. 324. 335. 333. 341. 326. 337. GooF 0.951 0.934 1.074 1.147 1.072 1.095 0.994 1.053 1.027 0.998 K 2.786 1.378 1.037 0.981 0.984 0.998 0.994 1.013 1.023 1.012 Resolution(A) 0.77 0.80 0.84 0.87 0.92 0.98 1.05 1.15 1.32 1.64 inf Number in group 345. 335. 333. 327. 341. 330. 334. 333. 333. 335. GooF 0.866 0.861 0.863 0.889 0.935 0.862 1.037 1.106 1.349 1.406 K 0.992 1.018 1.002 0.992 1.003 1.014 1.048 1.038 1.038 0.992 R1 0.252 0.187 0.157 0.111 0.089 0.071 0.063 0.046 0.045 0.044 Recommended weighting scheme: WGHT 0.0632 1.6691 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 -4 6 164.35 45.40 7.64 0.069 1.23 -3 2 5 483.21 247.72 6.97 0.162 1.56 -4 4 3 287.52 111.47 6.91 0.108 1.56 4 -5 4 112.39 31.09 6.03 0.057 1.35 -5 5 1 140.97 53.01 5.53 0.075 1.47 -2 1 5 89.91 31.62 5.36 0.058 1.72 3 -4 4 1219.32 803.06 5.21 0.291 1.58 -3 3 2 70.55 20.19 5.17 0.046 2.15 2 -3 7 30.94 1.25 5.09 0.011 1.18 -2 1 1 60.35 6.98 4.99 0.027 4.34 0 -2 6 78.43 24.53 4.81 0.051 1.57 -3 1 4 93.03 13.82 4.80 0.038 2.06 5 -6 4 214.54 113.81 4.77 0.110 1.17 -5 4 2 258.22 111.79 4.72 0.109 1.57 3 -3 4 1103.86 753.58 4.70 0.282 1.60 6 -7 3 318.45 176.34 4.69 0.136 1.08 -4 3 5 53.75 13.37 4.60 0.038 1.39 -5 5 5 137.15 15.18 4.40 0.040 1.12 1 -2 6 348.99 228.65 4.12 0.155 1.44 -3 3 3 1107.72 811.54 3.96 0.292 1.87 -5 5 3 479.68 323.81 3.93 0.185 1.32 -6 6 2 476.93 315.70 3.84 0.182 1.20 -4 1 7 22.36 0.50 3.49 0.007 1.27 2 -3 3 1399.37 1067.83 3.47 0.335 2.19 -3 2 6 1793.82 1391.13 3.41 0.383 1.35 -3 4 0 161.48 86.64 3.38 0.096 2.11 5 -6 1 584.13 324.79 3.36 0.185 1.35 -2 1 0 537.43 352.85 3.33 0.193 4.36 -2 0 3 70.49 32.96 3.28 0.059 3.04 4 -5 6 104.87 55.69 3.24 0.077 1.12 2 2 2 83.41 139.08 3.18 0.121 1.75 2 1 8 18.74 54.70 3.17 0.076 0.87 -1 0 5 88.66 51.52 3.16 0.074 1.82 6 -6 1 467.89 344.44 3.10 0.191 1.23 -5 2 0 387.44 517.14 3.04 0.233 1.75 -3 -3 2 605.30 773.56 2.90 0.285 1.94 -6 6 4 254.47 172.24 2.88 0.135 1.07 -2 -2 2 154.78 218.89 2.87 0.152 2.97 7 -8 1 144.88 81.27 2.86 0.093 0.99 0 2 9 5.86 46.28 2.85 0.070 0.83 1 6 4 97.30 163.04 2.78 0.131 0.92 -5 3 5 28.13 0.15 2.74 0.004 1.34 0 3 7 18.72 0.19 2.74 0.005 0.96 0 1 9 4.68 31.77 2.73 0.058 0.88 -1 -3 8 205.80 139.52 2.73 0.121 1.23 0 0 8 49.45 24.34 2.71 0.051 1.05 1 -2 4 867.24 697.06 2.68 0.271 2.12 -3 3 5 403.44 299.22 2.67 0.178 1.40 -7 6 4 239.81 167.83 2.66 0.133 1.03 0 -2 3 291.48 381.22 2.65 0.200 3.09 Bond lengths and angles C1 - Distance Angles N1 1.3369 (0.0060) C2 1.3759 (0.0064) 123.08 (0.40) H1 0.9500 118.46 118.46 C1 - N1 C2 C2 - Distance Angles C1 1.3759 (0.0064) C3 1.3779 (0.0064) 119.13 (0.45) H2 0.9500 120.43 120.43 C2 - C1 C3 C3 - Distance Angles C2 1.3779 (0.0064) C4 1.3803 (0.0067) 119.11 (0.42) H3 0.9500 120.45 120.45 C3 - C2 C4 C4 - Distance Angles C5 1.3772 (0.0061) C3 1.3803 (0.0067) 119.03 (0.40) H4 0.9500 120.49 120.49 C4 - C5 C3 C5 - Distance Angles N1 1.3693 (0.0052) C4 1.3772 (0.0061) 122.23 (0.42) C6 1.4546 (0.0065) 113.29 (0.36) 124.47 (0.39) C5 - N1 C4 C6 - Distance Angles N2 1.3302 (0.0053) N4 1.3427 (0.0055) 112.83 (0.40) C5 1.4546 (0.0065) 115.12 (0.37) 131.99 (0.38) C6 - N2 N4 C7 - Distance Angles N3 1.3343 (0.0051) N4 1.3471 (0.0058) 112.95 (0.38) C8 1.4540 (0.0064) 114.79 (0.38) 132.19 (0.36) C7 - N3 N4 C8 - Distance Angles N5 1.3578 (0.0057) C9 1.3823 (0.0057) 121.53 (0.42) C7 1.4540 (0.0064) 113.63 (0.35) 124.82 (0.41) C8 - N5 C9 C9 - Distance Angles C8 1.3823 (0.0057) C10 1.3854 (0.0072) 119.33 (0.44) H9 0.9500 120.33 120.33 C9 - C8 C10 C10 - Distance Angles C11 1.3787 (0.0073) C9 1.3854 (0.0072) 119.04 (0.40) H10 0.9500 120.48 120.48 C10 - C11 C9 C11 - Distance Angles C10 1.3787 (0.0073) C12 1.3819 (0.0059) 118.33 (0.46) H11 0.9500 120.83 120.83 C11 - C10 C12 C12 - Distance Angles N5 1.3266 (0.0059) C11 1.3819 (0.0060) 123.55 (0.44) H12 0.9500 118.23 118.23 C12 - N5 C11 N1 - Distance Angles C1 1.3369 (0.0060) C5 1.3693 (0.0052) 117.40 (0.37) Cu1 2.0805 (0.0036) 128.95 (0.28) 113.63 (0.29) N1 - C1 C5 N2 - Distance Angles C6 1.3302 (0.0053) N3 1.3439 (0.0055) 106.59 (0.34) Cu1 1.9491 (0.0036) 118.57 (0.31) 134.57 (0.28) N2 - C6 N3 N3 - Distance Angles C7 1.3343 (0.0051) N2 1.3439 (0.0055) 105.83 (0.35) Cu1_$3 1.9362 (0.0038) 119.53 (0.31) 134.52 (0.27) N3 - C7 N2 N4 - Distance Angles C6 1.3427 (0.0055) C7 1.3471 (0.0058) 101.81 (0.33) N4 - C6 N5 - Distance Angles C12 1.3266 (0.0059) C8 1.3578 (0.0057) 118.16 (0.35) Cu1_$3 2.1023 (0.0033) 128.40 (0.30) 113.44 (0.28) N5 - C12 C8 O1 - Distance Angles Cu1 2.2329 (0.0034) H1A 0.8369 (0.0101) 112.61 (3.71) H1B 0.8366 (0.0102) 121.12 (3.76) 107.51 (1.73) O1 - Cu1 H1A Cu1 - Distance Angles N3_$3 1.9362 (0.0038) N2 1.9491 (0.0036) 90.41 (0.15) N1 2.0805 (0.0036) 167.00 (0.14) 78.88 (0.15) N5_$3 2.1023 (0.0033) 78.51 (0.15) 168.68 (0.15) 111.78 (0.14) O1 2.2329 (0.0034) 98.47 (0.15) 94.14 (0.15) 89.71 (0.13) 89.82 (0.13) Cu1 - N3_$3 N2 N1 N5_$3 O21 - Distance Angles Cl21 1.4292 (0.0037) O21 - O22 - Distance Angles Cl21 1.4304 (0.0037) O22 - O23 - Distance Angles Cl21 1.4248 (0.0036) O23 - O24 - Distance Angles Cl21 1.4325 (0.0035) O24 - Cl21 - Distance Angles O23 1.4248 (0.0036) O21 1.4292 (0.0037) 109.84 (0.26) O22 1.4304 (0.0037) 109.53 (0.26) 108.50 (0.24) O24 1.4325 (0.0035) 109.76 (0.23) 109.84 (0.25) 109.34 (0.24) Cl21 - O23 O21 O22 O1W - Distance Angles H1WA 0.8398 (0.0103) H1WB 0.8378 (0.0103) 107.34 (1.78) O1W - H1WA Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.837(10) 1.91(2) 2.712(5) 160(6) O1-H1A...O1W_$1 0.837(10) 2.03(3) 2.796(4) 152(5) O1-H1B...O24 0.840(10) 2.08(2) 2.894(5) 165(6) O1W-H1WA...N4_$2 0.838(10) 2.45(2) 3.271(7) 168(8) O1W-H1WB...O23 FMAP and GRID set by program FMAP 2 1 26 GRID -2.174 -2 -2 2.174 2 2 R1 = 0.0815 for 3346 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.78 at 0.3029 0.2927 0.1546 [ 0.97 A from CU1 ] Deepest hole -0.90 at 0.1384 0.1205 0.0170 [ 0.97 A from CU1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2598 / 21174 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3029 0.2927 0.1546 1.00000 0.05 0.78 0.97 CU1 1.63 N5 1.95 N1 2.09 O1 Q2 1 0.1008 0.1220 0.0999 1.00000 0.05 0.68 1.00 CU1 1.37 N2 1.58 N3 2.21 N3 Q3 1 -0.0602 -0.0823 -0.4386 1.00000 0.05 0.64 0.91 O24 1.25 CL21 1.68 O21 2.08 O23 Q4 1 0.0486 0.0570 0.0990 1.00000 0.05 0.60 1.51 N2 1.55 N3 1.69 CU1 1.93 N3 Q5 1 -0.1808 -0.2450 -0.3584 1.00000 0.05 0.57 0.85 O22 1.53 CL21 1.90 O24 2.36 CU1 Shortest distances between peaks (including symmetry equivalents) 2 4 0.70 4 4 1.68 2 4 1.89 1 2 1.97 2 5 2.21 4 5 2.27 3 5 2.28 2 2 2.31 3 3 2.63 1 4 2.64 1 5 2.78 Time profile in seconds ----------------------- 0.09: 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. 1.05: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.11: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.14: Structure factors and derivatives 9.08: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.14: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:22:03 Total CPU time: 16.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++