+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 09:59:20 on 21-Feb-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pbcn CELL 0.71073 7.5225 24.7605 7.5372 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0007 0.0002 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N S CU UNIT 56 32 16 8 4 V = 1403.89 F(000) = 724.0 Mu = 1.85 mm-1 Cell Wt = 1439.62 Rho = 1.703 MERG 2 OMIT -3.00 55.00 OMIT 1 0 2 OMIT 2 0 4 OMIT 1 1 2 OMIT 2 8 0 SHEL 7 0.77 HFIX 43 -1.20 C12 C14 C15 C13 FMAP 2 PLAN 5 SIZE 0.02 0.03 0.24 ACTA BOND $H WGHT 0.01970 2.17710 L.S. 20 TEMP -153.00 FVAR 0.64415 C1 1 -0.077958 -0.104105 0.203629 11.00000 0.01932 0.01245 = 0.01931 -0.00033 -0.00051 -0.00058 C2 1 -0.161095 -0.154192 0.155880 11.00000 0.01864 0.01547 = 0.02385 0.00119 -0.00208 0.00270 C11 1 0.087895 0.130468 0.294647 11.00000 0.02035 0.01385 = 0.01576 -0.00003 0.00042 0.00055 C12 1 0.177727 0.177150 0.342081 11.00000 0.02529 0.01251 = 0.02549 0.00024 -0.00114 -0.00108 C13 1 0.340270 0.173007 0.427717 11.00000 0.02564 0.01725 = 0.02711 -0.00171 -0.00200 -0.00511 C14 1 0.407765 0.122234 0.464299 11.00000 0.01972 0.02111 = 0.03014 -0.00114 -0.00505 -0.00165 C15 1 0.311411 0.077509 0.412310 11.00000 0.02012 0.01696 = 0.02542 -0.00003 -0.00452 0.00149 N1 3 -0.230376 -0.193629 0.115738 11.00000 0.02735 0.01741 = 0.03241 -0.00006 -0.00626 -0.00155 N11 3 0.155268 0.080890 0.329297 11.00000 0.01831 0.01184 = 0.02096 -0.00061 -0.00105 -0.00029 S1 4 -0.183791 -0.045067 0.138420 11.00000 0.01951 0.01164 = 0.02627 0.00016 -0.00576 -0.00034 CU1 5 0.000000 0.018703 0.250000 10.50000 0.01697 0.00990 = 0.02247 0.00000 -0.00368 0.00000 HKLF 4 Covalent radii and connectivity table for s93 in Pbcn C 0.770 H 0.320 N 0.700 S 1.030 CU 1.280 C1 - C1_$1 C2 S1 C2 - N1 C1 C11 - N11 C12 C11_$1 C12 - C11 C13 C13 - C14 C12 C14 - C15 C13 C15 - N11 C14 N1 - C2 N11 - C15 C11 Cu1 S1 - C1 Cu1 Cu1 - N11 N11_$1 S1 S1_$1 Operators for generating equivalent atoms: $1 -x, y, -z+1/2 h k l Fo^2 Sigma Why rejected 6 1 0 35.68 7.91 observed but should be systematically absent 1 2 0 6.60 1.52 observed but should be systematically absent 1 2 0 10.64 1.84 observed but should be systematically absent 1 2 0 7.26 1.60 observed but should be systematically absent 1 2 0 12.11 2.57 observed but should be systematically absent 1 2 0 5.88 1.18 observed but should be systematically absent 1 2 0 13.58 3.14 observed but should be systematically absent 1 2 0 9.74 1.85 observed but should be systematically absent 3 2 0 16.80 3.91 observed but should be systematically absent 3 2 0 19.14 3.84 observed but should be systematically absent 3 2 0 14.15 2.34 observed but should be systematically absent 0 3 5 24.72 5.95 observed but should be systematically absent 2 3 0 43.60 5.91 observed but should be systematically absent 2 3 0 41.51 5.02 observed but should be systematically absent 2 3 0 39.78 7.00 observed but should be systematically absent 2 3 0 60.34 12.70 observed but should be systematically absent 2 3 0 42.45 4.38 observed but should be systematically absent 2 3 0 58.03 6.25 observed but should be systematically absent 2 3 0 38.37 7.48 observed but should be systematically absent 2 3 0 53.28 9.27 observed but should be systematically absent 2 3 0 34.79 6.00 observed but should be systematically absent 2 3 0 55.50 7.47 observed but should be systematically absent 2 3 0 39.58 6.04 observed but should be systematically absent 2 3 0 39.89 7.40 observed but should be systematically absent 2 3 0 54.33 8.74 observed but should be systematically absent 3 4 0 47.16 10.55 observed but should be systematically absent 3 4 0 30.60 6.92 observed but should be systematically absent 3 4 0 41.00 7.54 observed but should be systematically absent 3 4 0 41.93 9.21 observed but should be systematically absent 3 4 0 40.09 7.11 observed but should be systematically absent 3 4 0 34.52 8.33 observed but should be systematically absent 3 4 0 34.65 8.50 observed but should be systematically absent 0 5 0 20.25 4.51 observed but should be systematically absent 0 5 0 18.10 4.27 observed but should be systematically absent 0 5 0 21.38 4.86 observed but should be systematically absent 0 5 0 27.97 6.12 observed but should be systematically absent 0 5 0 27.01 6.33 observed but should be systematically absent 0 5 0 24.47 4.92 observed but should be systematically absent 4 5 0 23.69 5.85 observed but should be systematically absent 4 5 0 19.95 4.48 observed but should be systematically absent 3 6 0 23.51 4.10 observed but should be systematically absent 3 6 0 20.79 4.44 observed but should be systematically absent 3 6 0 25.18 4.11 observed but should be systematically absent 3 6 0 32.80 7.63 observed but should be systematically absent 3 6 0 23.17 4.67 observed but should be systematically absent 0 7 5 43.69 9.33 observed but should be systematically absent 0 7 0 25.94 6.28 observed but should be systematically absent 0 7 0 46.34 11.03 observed but should be systematically absent 0 7 5 21.30 4.68 observed but should be systematically absent 2 7 0 140.43 27.12 observed but should be systematically absent ** etc. ** 21583 Reflections read, of which 2189 rejected -9 =< h =< 9, -30 =< k =< 32, -9 =< l =< 9, Max. 2-theta = 54.94 84 Systematic absence violations 0 Inconsistent equivalents 1608 Unique reflections, of which 0 suppressed R(int) = 0.0395 R(sigma) = 0.0193 Friedel opposites merged Maximum memory for data reduction = 1142 / 15956 Special position constraints for Cu1 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 1 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64405 0.00120 -0.083 OSF Mean shift/esd = 0.017 Maximum = -0.083 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 2 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 -0.026 OSF Mean shift/esd = 0.006 Maximum = -0.026 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 3 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for x C1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 4 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H14 Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 5 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 Cu1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C12 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 6 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C13 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 7 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for C11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 8 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C11 Max. shift = 0.000 A for C2 Max. dU = 0.000 for N1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 9 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C14 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 10 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H14 Max. dU = 0.000 for C15 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 11 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C11 Max. dU = 0.000 for N11 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 12 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C14 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 13 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C13 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 14 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C11 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 15 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C14 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 16 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C12 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 17 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C11 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 18 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 19 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C11 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1382 / 126977 wR2 = 0.0717 before cycle 20 for 1608 data and 96 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64402 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C12 Largest correlation matrix elements 0.517 U22 Cu1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H12 0.1285 0.2116 0.3162 43 0.950 0.000 C12 C11 C13 H13 0.4043 0.2045 0.4608 43 0.950 0.000 C13 C14 C12 H14 0.5182 0.1182 0.5240 43 0.950 0.000 C14 C15 C13 H15 0.3585 0.0427 0.4368 43 0.950 0.000 C15 N11 C14 s93 in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.07794 -0.10410 0.20363 1.00000 0.01932 0.01240 0.01929 -0.00032 -0.00047 -0.00057 0.01700 0.00363 0.00030 0.00008 0.00028 0.00000 0.00105 0.00089 0.00102 0.00077 0.00087 0.00083 0.00042 C2 -0.16110 -0.15419 0.15588 1.00000 0.01859 0.01546 0.02381 0.00120 -0.00207 0.00269 0.01929 0.00383 0.00030 0.00008 0.00030 0.00000 0.00110 0.00101 0.00108 0.00083 0.00090 0.00086 0.00045 C11 0.08788 0.13047 0.29464 1.00000 0.02036 0.01383 0.01572 -0.00004 0.00044 0.00052 0.01664 0.00362 0.00029 0.00008 0.00027 0.00000 0.00113 0.00090 0.00098 0.00074 0.00086 0.00083 0.00043 C12 0.17775 0.17715 0.34208 1.00000 0.02525 0.01249 0.02547 0.00025 -0.00113 -0.00106 0.02107 0.00386 0.00031 0.00009 0.00030 0.00000 0.00120 0.00096 0.00112 0.00083 0.00097 0.00086 0.00047 H12 0.12853 0.21160 0.31620 1.00000 0.02529 0.00000 0.00000 C13 0.34026 0.17301 0.42772 1.00000 0.02564 0.01723 0.02708 -0.00174 -0.00198 -0.00513 0.02332 0.00395 0.00032 0.00009 0.00031 0.00000 0.00125 0.00102 0.00116 0.00089 0.00098 0.00092 0.00049 H13 0.40426 0.20452 0.46075 1.00000 0.02798 0.00000 0.00000 C14 0.40775 0.12224 0.46429 1.00000 0.01968 0.02112 0.03008 -0.00114 -0.00506 -0.00166 0.02363 0.00395 0.00031 0.00009 0.00033 0.00000 0.00118 0.00105 0.00121 0.00093 0.00099 0.00091 0.00049 H14 0.51820 0.11824 0.52399 1.00000 0.02836 0.00000 0.00000 C15 0.31141 0.07751 0.41231 1.00000 0.02009 0.01696 0.02541 -0.00001 -0.00451 0.00149 0.02082 0.00386 0.00030 0.00009 0.00031 0.00000 0.00114 0.00101 0.00109 0.00085 0.00093 0.00087 0.00047 H15 0.35853 0.04270 0.43680 1.00000 0.02498 0.00000 0.00000 N1 -0.23038 -0.19363 0.11575 1.00000 0.02730 0.01740 0.03239 -0.00006 -0.00624 -0.00152 0.02570 0.00345 0.00028 0.00008 0.00028 0.00000 0.00109 0.00094 0.00108 0.00080 0.00092 0.00084 0.00045 N11 0.15527 0.08089 0.32930 1.00000 0.01830 0.01182 0.02091 -0.00061 -0.00104 -0.00029 0.01701 0.00308 0.00024 0.00007 0.00024 0.00000 0.00092 0.00078 0.00087 0.00067 0.00075 0.00068 0.00037 S1 -0.18379 -0.04507 0.13842 1.00000 0.01950 0.01162 0.02626 0.00016 -0.00576 -0.00034 0.01913 0.00092 0.00007 0.00002 0.00007 0.00000 0.00028 0.00024 0.00028 0.00020 0.00022 0.00020 0.00014 Cu1 0.00000 0.01870 0.25000 0.50000 0.01696 0.00989 0.02247 0.00000 -0.00368 0.00000 0.01644 0.00032 0.00000 0.00001 0.00000 0.00000 0.00021 0.00018 0.00021 0.00000 0.00016 0.00000 0.00012 Final Structure Factor Calculation for s93 in Pbcn Total number of l.s. parameters = 96 Maximum vector length = 511 Memory required = 1286 / 24017 wR2 = 0.0717 before cycle 21 for 1608 data and 0 / 96 parameters GooF = S = 1.200; Restrained GooF = 1.200 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0197 * P )^2 + 2.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0291 for 1479 Fo > 4sig(Fo) and 0.0341 for all 1608 data wR2 = 0.0717, GooF = S = 1.200, Restrained GooF = 1.200 for all data Occupancy sum of asymmetric unit = 10.50 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0198 0.0189 0.0123 C1 0.0245 0.0198 0.0135 C2 0.0204 0.0157 0.0138 C11 0.0266 0.0243 0.0124 C12 0.0289 0.0267 0.0143 C13 0.0322 0.0220 0.0167 C14 0.0280 0.0185 0.0159 C15 0.0366 0.0234 0.0171 N1 0.0213 0.0180 0.0118 N11 0.0296 0.0162 0.0116 S1 0.0243 0.0151 0.0099 Cu1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.045 0.068 0.096 0.127 0.160 0.203 0.261 0.358 1.000 Number in group 170. 160. 154. 164. 160. 156. 162. 161. 162. 159. GooF 1.740 1.268 1.482 1.069 0.970 0.912 0.944 0.959 1.084 1.267 K 2.640 1.085 1.034 1.016 0.990 0.987 0.998 1.001 1.002 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.31 1.66 inf Number in group 162. 160. 167. 157. 162. 163. 154. 161. 160. 162. GooF 1.329 0.928 0.833 0.820 0.938 0.983 1.073 0.824 1.308 2.236 K 0.920 0.994 1.011 1.015 1.022 1.017 1.024 1.005 0.990 0.998 R1 0.093 0.057 0.042 0.034 0.031 0.030 0.025 0.019 0.023 0.031 Recommended weighting scheme: WGHT 0.0195 2.1877 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) 2 3 2 150.41 0.16 7.14 0.003 2.53 3 8 1 293.58 88.99 6.94 0.062 1.89 2 11 1 92.91 20.39 5.86 0.030 1.87 2 5 2 53.96 0.87 5.42 0.006 2.34 3 0 4 344.53 205.98 4.48 0.094 1.51 2 12 0 16.19 74.11 4.44 0.057 1.81 3 1 2 827.94 1089.90 4.40 0.217 2.08 3 2 2 34.98 1.81 4.38 0.009 2.06 4 0 0 18.02 75.82 4.23 0.057 1.88 3 6 1 295.92 165.89 4.08 0.085 2.06 3 10 1 672.72 504.88 3.77 0.148 1.72 3 0 6 2985.92 2498.10 3.67 0.329 1.12 0 8 0 4470.94 3927.77 3.46 0.412 3.10 3 8 2 3743.08 3285.63 3.43 0.377 1.73 0 6 1 109.72 58.77 3.35 0.050 3.62 3 4 1 367.42 264.15 3.34 0.107 2.22 2 12 1 2976.83 3378.08 3.20 0.382 1.76 5 4 2 24.68 4.53 3.14 0.014 1.36 3 2 4 33.86 9.22 3.10 0.020 1.50 3 18 3 97.40 50.23 3.08 0.047 1.09 2 14 1 255.69 353.44 3.06 0.124 1.57 8 5 1 34.61 0.82 3.06 0.006 0.92 2 9 1 941.38 763.66 2.97 0.182 2.13 4 18 1 484.28 373.01 2.96 0.127 1.10 3 10 3 30.59 7.05 2.95 0.017 1.44 1 13 1 4199.04 4661.77 2.92 0.449 1.79 2 0 0 2535.66 2232.01 2.83 0.311 3.76 0 10 1 749.88 904.17 2.79 0.198 2.35 3 0 2 128.70 192.80 2.79 0.091 2.09 1 8 4 22.62 3.39 2.72 0.012 1.57 2 3 4 2561.58 2283.28 2.70 0.314 1.65 3 2 6 19.40 1.03 2.64 0.007 1.12 1 12 2 345.19 440.17 2.62 0.138 1.76 7 18 4 -17.95 30.26 2.56 0.036 0.77 5 8 8 -23.64 27.99 2.54 0.035 0.77 4 2 0 3124.78 3460.38 2.51 0.387 1.86 5 8 5 31.03 6.59 2.50 0.017 1.01 5 4 8 39.81 86.39 2.49 0.061 0.79 0 12 3 2612.08 2896.88 2.44 0.354 1.59 3 3 6 1100.87 949.57 2.43 0.203 1.11 0 12 1 4985.19 5424.28 2.40 0.484 1.99 2 15 5 35.73 11.29 2.38 0.022 1.07 6 21 4 9.01 53.03 2.35 0.048 0.78 0 12 4 387.89 479.49 2.35 0.144 1.39 1 11 1 4993.98 5411.54 2.34 0.484 2.07 9 9 2 363.01 479.93 2.34 0.144 0.78 5 2 5 27.26 5.35 2.32 0.015 1.06 1 6 1 4835.13 4464.32 2.31 0.439 3.26 5 6 5 57.65 27.75 2.27 0.035 1.03 7 12 5 34.31 4.69 2.25 0.014 0.81 Bond lengths and angles C1 - Distance Angles C1_$1 1.3652 (0.0044) C2 1.4350 (0.0029) 120.19 (0.12) S1 1.7356 (0.0021) 122.62 (0.07) 117.19 (0.16) C1 - C1_$1 C2 C2 - Distance Angles N1 1.1474 (0.0029) C1 1.4350 (0.0029) 178.51 (0.24) C2 - N1 C11 - Distance Angles N11 1.3537 (0.0026) C12 1.3859 (0.0029) 121.60 (0.20) C11_$1 1.4836 (0.0044) 114.91 (0.12) 123.48 (0.13) C11 - N11 C12 C12 - Distance Angles C11 1.3859 (0.0029) C13 1.3863 (0.0033) 119.24 (0.20) H12 0.9500 120.38 120.38 C12 - C11 C13 C13 - Distance Angles C14 1.3835 (0.0032) C12 1.3863 (0.0033) 118.92 (0.21) H13 0.9500 120.54 120.54 C13 - C14 C12 C14 - Distance Angles C15 1.3804 (0.0031) C13 1.3835 (0.0032) 118.67 (0.21) H14 0.9500 120.66 120.66 C14 - C15 C13 C15 - Distance Angles N11 1.3335 (0.0029) C14 1.3804 (0.0031) 123.04 (0.20) H15 0.9500 118.48 118.48 C15 - N11 C14 N1 - Distance Angles C2 1.1474 (0.0029) N1 - N11 - Distance Angles C15 1.3335 (0.0029) C11 1.3537 (0.0026) 118.51 (0.18) Cu1 2.0229 (0.0018) 126.83 (0.15) 114.65 (0.14) N11 - C15 C11 S1 - Distance Angles C1 1.7356 (0.0021) Cu1 2.2609 (0.0006) 101.67 (0.07) S1 - C1 Cu1 - Distance Angles N11 2.0229 (0.0018) N11_$1 2.0229 (0.0018) 80.87 (0.10) S1 2.2609 (0.0006) 174.00 (0.05) 93.93 (0.05) S1_$1 2.2609 (0.0006) 93.93 (0.05) 174.00 (0.05) 91.41 (0.03) Cu1 - N11 N11_$1 S1 FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -1 -2 2.778 1 2 R1 = 0.0330 for 1608 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.42 at 0.0000 0.1029 0.7500 [ 0.68 A from C1 ] Deepest hole -0.33 at -0.0105 0.0339 0.3130 [ 0.61 A from CU1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1782 / 20160 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0000 -0.1029 0.2500 0.50000 0.05 0.42 0.68 C1 1.89 C2 2.16 S1 3.01 CU1 Q2 1 0.1117 0.0582 0.2923 1.00000 0.05 0.32 0.71 N11 1.33 CU1 1.80 C11 1.82 C15 Q3 1 0.1201 0.1066 0.3198 1.00000 0.05 0.31 0.67 C11 0.69 N11 1.75 C15 1.81 C12 Q4 1 0.1301 0.1516 0.3363 1.00000 0.05 0.31 0.69 C11 0.73 C12 1.49 H12 1.76 N11 Q5 1 0.1723 -0.0004 0.2142 1.00000 0.05 0.29 1.41 CU1 1.57 S1 2.19 N11 2.43 H15 Shortest distances between peaks (including symmetry equivalents) 3 4 1.12 2 3 1.22 2 5 1.63 2 2 1.80 3 3 2.09 2 3 2.28 2 4 2.34 4 4 2.35 3 4 2.48 2 5 2.58 5 5 2.65 3 5 2.79 1 5 2.86 Time profile in seconds ----------------------- 0.07: 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. 3.31: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.46: Structure factors and derivatives 0.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 0.40: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 09:59:37 Total CPU time: 6.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++