+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0583pbcn started at 09:32:05 on 22-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL pbcn in Pbcn CELL 0.71073 39.9227 8.3170 12.9213 90.000 90.000 90.000 ZERR 16.00 0.0015 0.0003 0.0005 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 O UNIT 192 208 16 32 V = 4290.35 F(000) = 1728.0 Mu = 0.09 mm-1 Cell Wt = 3251.74 Rho = 1.259 MERG 2 OMIT -3.00 55.00 omit 23 7 0 SHEL 7 0.77 EQIV $1 -x, -y, -z+1 EQIV $2 x, -y, z+1/2 HTAB O1 O2_$1 HTAB O21 N1_$2 FMAP 2 PLAN 5 SIZE 0.04 0.14 0.16 ACTA BOND $H WGHT 0.00780 7.50150 L.S. 12 TEMP -153.00 FVAR 0.23670 MOLE 1 C1 1 0.025129 0.035149 0.376212 11.00000 0.01973 0.02220 = 0.02440 0.00417 -0.00196 -0.00061 C2 1 0.043470 0.062903 0.278056 11.00000 0.01986 0.02332 = 0.02070 0.00325 0.00174 0.00018 C3 1 0.048124 0.221742 0.244514 11.00000 0.02092 0.02001 = 0.02150 -0.00250 0.00027 0.00295 AFIX 43 H3 2 0.039973 0.309870 0.283930 11.00000 -1.20000 AFIX 0 C4 1 0.064868 0.245929 0.152721 11.00000 0.01749 0.01986 = 0.02144 0.00056 -0.00065 0.00289 C5 1 0.076921 0.115394 0.095952 11.00000 0.01706 0.02408 = 0.02117 -0.00131 -0.00001 0.00173 C6 1 0.072433 -0.041689 0.127658 11.00000 0.02658 0.01996 = 0.02873 -0.00372 0.00451 0.00220 AFIX 43 H6 2 0.080669 -0.129368 0.087998 11.00000 -1.20000 AFIX 0 C7 1 0.055380 -0.066020 0.219921 11.00000 0.02788 0.01878 = 0.03176 0.00234 0.00172 -0.00064 AFIX 43 H7 2 0.051762 -0.172602 0.243881 11.00000 -1.20000 AFIX 0 C8 1 0.073854 0.397101 0.093856 11.00000 0.02300 0.01790 = 0.02086 0.00103 -0.00020 0.00189 C9 1 0.093110 0.322551 0.004199 11.00000 0.02301 0.02519 = 0.02046 0.00167 -0.00393 0.00249 C10 1 0.110444 0.419965 -0.075288 11.00000 0.04179 0.03339 = 0.02433 0.00442 0.00805 0.00023 AFIX 137 H10A 2 0.129858 0.473442 -0.044149 11.00000 -1.50000 H10B 2 0.095003 0.501080 -0.102678 11.00000 -1.50000 H10C 2 0.117951 0.349881 -0.131674 11.00000 -1.50000 AFIX 0 C11 1 0.096445 0.511272 0.155335 11.00000 0.02842 0.02128 = 0.02611 -0.00096 -0.00099 0.00074 AFIX 137 H11A 2 0.083610 0.559389 0.212084 11.00000 -1.50000 H11B 2 0.104731 0.596368 0.109545 11.00000 -1.50000 H11C 2 0.115449 0.451107 0.183712 11.00000 -1.50000 AFIX 0 C12 1 0.042689 0.486070 0.054267 11.00000 0.02758 0.02775 = 0.03247 0.00730 -0.00250 0.00270 AFIX 137 H12A 2 0.029144 0.412897 0.012045 11.00000 -1.50000 H12B 2 0.049617 0.578327 0.012223 11.00000 -1.50000 H12C 2 0.029413 0.523774 0.113265 11.00000 -1.50000 AFIX 0 N1 3 0.094009 0.166892 0.005095 11.00000 0.02272 0.02620 = 0.02012 -0.00012 0.00056 0.00181 O1 4 0.018987 -0.114829 0.399681 11.00000 0.03185 0.02665 = 0.02979 0.00561 0.00856 -0.00012 AFIX 147 H1 2 0.007088 -0.118646 0.453240 11.00000 -1.50000 AFIX 0 O2 4 0.016265 0.149647 0.431650 11.00000 0.03266 0.02791 = 0.02433 0.00049 0.00511 -0.00040 MOLE 2 C21 1 0.142283 0.127467 0.379110 11.00000 0.02491 0.02421 = 0.02621 0.00329 0.00155 0.00049 C22 1 0.158751 0.205099 0.287947 11.00000 0.01976 0.01884 = 0.02359 0.00222 0.00184 0.00045 C23 1 0.175060 0.352809 0.302509 11.00000 0.02067 0.02538 = 0.02201 -0.00284 -0.00055 0.00336 AFIX 43 H23 2 0.176774 0.399272 0.369465 11.00000 -1.20000 AFIX 0 C24 1 0.188557 0.429036 0.217269 11.00000 0.01665 0.01905 = 0.02761 -0.00041 0.00083 0.00251 C25 1 0.186296 0.360388 0.119007 11.00000 0.01677 0.02193 = 0.02375 0.00295 0.00138 0.00192 C26 1 0.171143 0.212186 0.103843 11.00000 0.02285 0.02501 = 0.02168 -0.00183 -0.00112 0.00204 AFIX 43 H26 2 0.170246 0.164390 0.037125 11.00000 -1.20000 AFIX 0 C27 1 0.157277 0.135698 0.189715 11.00000 0.02059 0.01864 = 0.02805 0.00149 -0.00085 0.00110 AFIX 43 H27 2 0.146622 0.034420 0.181223 11.00000 -1.20000 AFIX 0 C28 1 0.206287 0.588450 0.205687 11.00000 0.02015 0.02083 = 0.03106 0.00135 0.00080 0.00032 C29 1 0.211382 0.588004 0.088611 11.00000 0.02177 0.02900 = 0.03095 0.00736 -0.00174 -0.00249 C30 1 0.227536 0.723393 0.032512 11.00000 0.04214 0.03947 = 0.04092 0.01157 -0.00466 -0.01670 AFIX 137 H30A 2 0.230407 0.694368 -0.040457 11.00000 -1.50000 H30B 2 0.249474 0.745764 0.063343 11.00000 -1.50000 H30C 2 0.213377 0.819315 0.037663 11.00000 -1.50000 AFIX 0 C31 1 0.240058 0.592113 0.263402 11.00000 0.02649 0.02904 = 0.03428 0.00085 -0.00155 -0.00300 AFIX 137 H31A 2 0.236096 0.582980 0.338020 11.00000 -1.50000 H31B 2 0.251567 0.693650 0.248689 11.00000 -1.50000 H31C 2 0.253989 0.502038 0.240201 11.00000 -1.50000 AFIX 0 C32 1 0.184283 0.729550 0.240466 11.00000 0.03140 0.02152 = 0.05915 -0.00193 0.00354 -0.00063 AFIX 137 H32A 2 0.162953 0.726529 0.202976 11.00000 -1.50000 H32B 2 0.195798 0.831043 0.225678 11.00000 -1.50000 H32C 2 0.180032 0.721266 0.314973 11.00000 -1.50000 AFIX 0 N21 3 0.200426 0.461159 0.041359 11.00000 0.02471 0.03162 = 0.02594 0.00797 -0.00143 -0.00413 O21 4 0.128821 -0.013777 0.356760 11.00000 0.03944 0.02502 = 0.02901 0.00316 0.00947 -0.00867 AFIX 147 H21 2 0.118564 -0.049055 0.408780 11.00000 -1.50000 AFIX 0 O22 4 0.141003 0.188825 0.464674 11.00000 0.05588 0.03727 = 0.02619 -0.00289 0.01035 -0.01183 HKLF 4 1.0 0.00 0.00 1.00 1.00 0.00 0.00 0.00 1.00 0.00 Covalent radii and connectivity table for pbcn in Pbcn C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 O1 C2 C2 - C7 C3 C1 C3 - C4 C2 C4 - C3 C5 C8 C5 - C6 C4 N1 C6 - C5 C7 C7 - C6 C2 C8 - C4 C9 C11 C12 C9 - N1 C10 C8 C10 - C9 C11 - C8 C12 - C8 N1 - C9 C5 O1 - C1 O2 - C1 C21 - O22 O21 C22 C22 - C27 C23 C21 C23 - C24 C22 C24 - C23 C25 C28 C25 - C26 C24 N21 C26 - C25 C27 C27 - C26 C22 C28 - C24 C29 C32 C31 C29 - N21 C30 C28 C30 - C29 C31 - C28 C32 - C28 N21 - C29 C25 O21 - C21 O22 - C21 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x, -y, z+1/2 h k l Fo^2 Sigma Why rejected 7 0 11 5.85 1.37 observed but should be systematically absent 35 0 0 6.42 1.57 observed but should be systematically absent 24263 Reflections read, of which 1912 rejected -51 =< h =< 51, -9 =< k =< 10, -16 =< l =< 16, Max. 2-theta = 54.97 2 Systematic absence violations 0 Inconsistent equivalents 4862 Unique reflections, of which 0 suppressed R(int) = 0.0637 R(sigma) = 0.0543 Friedel opposites merged Maximum memory for data reduction = 2878 / 48210 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 = 3670 / 347751 wR2 = 0.1452 before cycle 1 for 4862 data and 279 / 279 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23668 0.00043 -0.054 OSF Mean shift/esd = 0.096 Maximum = -0.629 for U12 C5 Max. shift = 0.004 A for H10A Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 2 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 -0.068 OSF Mean shift/esd = 0.037 Maximum = -0.270 for U12 C5 Max. shift = 0.002 A for H10A Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 3 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 -0.002 OSF Mean shift/esd = 0.004 Maximum = -0.026 for U12 C5 Max. shift = 0.000 A for H10A Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 4 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.005 for tors H10A Max. shift = 0.000 A for H10B Max. dU = 0.000 for C11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 5 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H10A Max. shift = 0.000 A for H10B Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 6 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for C12 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 7 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H30C Max. dU = 0.000 for C30 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 8 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H30A Max. dU = 0.000 for C12 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 9 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H32C Max. dU = 0.000 for C29 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 10 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C24 Max. shift = 0.000 A for C24 Max. dU = 0.000 for O1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 11 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H12C Max. dU = 0.000 for C28 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3670 / 347751 wR2 = 0.1450 before cycle 12 for 4862 data and 279 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23665 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O21 Max. shift = 0.000 A for H10C Max. dU = 0.000 for C30 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.0399 0.3098 0.2839 43 0.950 0.000 C3 C4 C2 H6 0.0807 -0.1293 0.0880 43 0.950 0.000 C6 C5 C7 H7 0.0517 -0.1726 0.2438 43 0.950 0.000 C7 C6 C2 H10A 0.1298 0.4740 -0.0441 137 0.980 0.000 C10 C9 H10A H10B 0.0949 0.5007 -0.1030 137 0.980 0.000 C10 C9 H10A H10C 0.1181 0.3498 -0.1315 137 0.980 0.000 C10 C9 H10A H11A 0.0836 0.5595 0.2120 137 0.980 0.000 C11 C8 H11A H11B 0.1047 0.5963 0.1095 137 0.980 0.000 C11 C8 H11A H11C 0.1154 0.4510 0.1838 137 0.980 0.000 C11 C8 H11A H12A 0.0291 0.4130 0.0121 137 0.980 0.000 C12 C8 H12A H12B 0.0496 0.5783 0.0122 137 0.980 0.000 C12 C8 H12A H12C 0.0294 0.5240 0.1133 137 0.980 0.000 C12 C8 H12A H1 0.0071 -0.1187 0.4533 147 0.840 0.000 O1 C1 H1 H23 0.1768 0.3993 0.3695 43 0.950 0.000 C23 C24 C22 H26 0.1703 0.1644 0.0371 43 0.950 0.000 C26 C25 C27 H27 0.1466 0.0345 0.1812 43 0.950 0.000 C27 C26 C22 H30A 0.2305 0.6943 -0.0404 137 0.980 0.000 C30 C29 H30A H30B 0.2495 0.7458 0.0634 137 0.980 0.000 C30 C29 H30A H30C 0.2134 0.8193 0.0375 137 0.980 0.000 C30 C29 H30A H31A 0.2361 0.5825 0.3380 137 0.980 0.000 C31 C28 H31A H31B 0.2516 0.6936 0.2488 137 0.980 0.000 C31 C28 H31A H31C 0.2540 0.5020 0.2401 137 0.980 0.000 C31 C28 H31A H32A 0.1629 0.7265 0.2031 137 0.980 0.000 C32 C28 H32A H32B 0.1958 0.8310 0.2255 137 0.980 0.000 C32 C28 H32A H32C 0.1801 0.7214 0.3150 137 0.980 0.000 C32 C28 H32A H21 0.1187 -0.0493 0.4089 147 0.840 0.000 O21 C21 H21 pbcn in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.02512 0.03498 0.37621 1.00000 0.01972 0.02222 0.02441 0.00416 -0.00190 -0.00021 0.02212 0.00413 0.00006 0.00029 0.00019 0.00000 0.00110 0.00127 0.00125 0.00103 0.00094 0.00097 0.00051 C2 0.04347 0.06295 0.27806 1.00000 0.01972 0.02248 0.02093 0.00325 0.00168 0.00017 0.02105 0.00412 0.00006 0.00029 0.00018 0.00000 0.00112 0.00125 0.00121 0.00096 0.00091 0.00096 0.00051 C3 0.04811 0.22173 0.24451 1.00000 0.02076 0.01937 0.02178 -0.00247 0.00023 0.00319 0.02064 0.00405 0.00006 0.00029 0.00018 0.00000 0.00113 0.00118 0.00119 0.00097 0.00092 0.00094 0.00049 H3 0.03994 0.30982 0.28394 1.00000 0.02476 0.00000 0.00000 C4 0.06487 0.24611 0.15272 1.00000 0.01757 0.01999 0.02132 0.00053 -0.00065 0.00302 0.01963 0.00400 0.00005 0.00028 0.00018 0.00000 0.00106 0.00120 0.00119 0.00095 0.00089 0.00094 0.00049 C5 0.07691 0.11538 0.09595 1.00000 0.01708 0.02413 0.02111 -0.00130 -0.00003 0.00084 0.02077 0.00401 0.00006 0.00029 0.00018 0.00000 0.00107 0.00124 0.00119 0.00098 0.00089 0.00096 0.00049 C6 0.07244 -0.04161 0.12765 1.00000 0.02657 0.02009 0.02867 -0.00376 0.00455 0.00145 0.02511 0.00427 0.00006 0.00029 0.00019 0.00000 0.00124 0.00124 0.00134 0.00104 0.00102 0.00102 0.00054 H6 0.08069 -0.12927 0.08802 1.00000 0.03013 0.00000 0.00000 C7 0.05536 -0.06604 0.21991 1.00000 0.02793 0.01895 0.03164 0.00235 0.00171 -0.00041 0.02617 0.00435 0.00006 0.00030 0.00020 0.00000 0.00129 0.00125 0.00142 0.00104 0.00105 0.00104 0.00056 H7 0.05171 -0.17263 0.24382 1.00000 0.03141 0.00000 0.00000 C8 0.07385 0.39717 0.09385 1.00000 0.02295 0.01791 0.02083 0.00105 -0.00020 0.00115 0.02057 0.00407 0.00006 0.00028 0.00018 0.00000 0.00115 0.00114 0.00119 0.00094 0.00092 0.00095 0.00049 C9 0.09311 0.32267 0.00420 1.00000 0.02301 0.02512 0.02047 0.00171 -0.00393 0.00183 0.02287 0.00417 0.00006 0.00030 0.00019 0.00000 0.00117 0.00130 0.00120 0.00100 0.00092 0.00100 0.00051 C10 0.11043 0.42003 -0.07529 1.00000 0.04148 0.03249 0.02459 0.00434 0.00799 0.00013 0.03285 0.00504 0.00007 0.00034 0.00020 0.00000 0.00156 0.00150 0.00136 0.00116 0.00114 0.00125 0.00063 H10A 0.12977 0.47405 -0.04407 1.00000 0.04928 0.00000 0.00000 H10B 0.09495 0.50071 -0.10299 1.00000 0.04928 0.00000 0.00000 H10C 0.11806 0.34984 -0.13147 1.00000 0.04928 0.00000 0.00000 C11 0.09642 0.51125 0.15534 1.00000 0.02831 0.02118 0.02613 -0.00094 -0.00108 0.00111 0.02521 0.00416 0.00006 0.00030 0.00019 0.00000 0.00124 0.00126 0.00132 0.00103 0.00102 0.00106 0.00054 H11A 0.08358 0.55945 0.21203 1.00000 0.03781 0.00000 0.00000 H11B 0.10474 0.59629 0.10955 1.00000 0.03781 0.00000 0.00000 H11C 0.11541 0.45105 0.18380 1.00000 0.03781 0.00000 0.00000 C12 0.04269 0.48617 0.05427 1.00000 0.02747 0.02706 0.03272 0.00719 -0.00243 0.00281 0.02908 0.00468 0.00006 0.00032 0.00021 0.00000 0.00127 0.00137 0.00144 0.00114 0.00109 0.00112 0.00058 H12A 0.02913 0.41297 0.01213 1.00000 0.04363 0.00000 0.00000 H12B 0.04962 0.57834 0.01216 1.00000 0.04363 0.00000 0.00000 H12C 0.02943 0.52401 0.11328 1.00000 0.04363 0.00000 0.00000 N1 0.09402 0.16696 0.00510 1.00000 0.02276 0.02643 0.02001 -0.00014 0.00056 0.00126 0.02307 0.00350 0.00005 0.00025 0.00015 0.00000 0.00100 0.00113 0.00103 0.00086 0.00079 0.00086 0.00045 O1 0.01899 -0.11492 0.39968 1.00000 0.03182 0.02640 0.02985 0.00560 0.00851 -0.00046 0.02936 0.00323 0.00004 0.00021 0.00014 0.00000 0.00099 0.00096 0.00101 0.00078 0.00077 0.00079 0.00042 H1 0.00709 -0.11873 0.45325 1.00000 0.04404 0.00000 0.00000 O2 0.01628 0.14962 0.43165 1.00000 0.03253 0.02748 0.02449 0.00050 0.00514 -0.00055 0.02816 0.00308 0.00004 0.00021 0.00013 0.00000 0.00097 0.00096 0.00092 0.00077 0.00075 0.00080 0.00041 C21 0.14230 0.12748 0.37911 1.00000 0.02484 0.02411 0.02625 0.00326 0.00152 0.00100 0.02507 0.00439 0.00006 0.00030 0.00019 0.00000 0.00122 0.00129 0.00133 0.00105 0.00100 0.00106 0.00053 C22 0.15877 0.20507 0.28795 1.00000 0.01986 0.01925 0.02340 0.00220 0.00188 0.00069 0.02084 0.00412 0.00006 0.00029 0.00018 0.00000 0.00112 0.00119 0.00122 0.00097 0.00093 0.00095 0.00050 C23 0.17506 0.35283 0.30251 1.00000 0.02051 0.02450 0.02229 -0.00277 -0.00054 0.00326 0.02243 0.00416 0.00006 0.00029 0.00019 0.00000 0.00112 0.00127 0.00121 0.00101 0.00094 0.00099 0.00051 H23 0.17675 0.39935 0.36945 1.00000 0.02692 0.00000 0.00000 C24 0.18858 0.42904 0.21727 1.00000 0.01656 0.01874 0.02774 -0.00037 0.00087 0.00253 0.02101 0.00407 0.00006 0.00028 0.00019 0.00000 0.00109 0.00118 0.00130 0.00098 0.00093 0.00093 0.00050 C25 0.18627 0.36040 0.11901 1.00000 0.01679 0.02215 0.02368 0.00293 0.00138 0.00204 0.02087 0.00412 0.00006 0.00029 0.00018 0.00000 0.00106 0.00122 0.00121 0.00099 0.00090 0.00096 0.00049 C26 0.17115 0.21221 0.10385 1.00000 0.02265 0.02421 0.02199 -0.00186 -0.00111 0.00208 0.02295 0.00416 0.00006 0.00029 0.00019 0.00000 0.00115 0.00124 0.00122 0.00103 0.00096 0.00101 0.00051 H26 0.17028 0.16437 0.03714 1.00000 0.02754 0.00000 0.00000 C27 0.15727 0.13574 0.18971 1.00000 0.02042 0.01810 0.02827 0.00151 -0.00082 0.00090 0.02226 0.00416 0.00006 0.00029 0.00019 0.00000 0.00115 0.00120 0.00131 0.00101 0.00096 0.00096 0.00051 H27 0.14658 0.03454 0.18120 1.00000 0.02672 0.00000 0.00000 C28 0.20627 0.58844 0.20568 1.00000 0.02012 0.02084 0.03105 0.00138 0.00081 0.00088 0.02400 0.00431 0.00006 0.00030 0.00020 0.00000 0.00114 0.00123 0.00134 0.00105 0.00099 0.00098 0.00053 C29 0.21137 0.58808 0.08861 1.00000 0.02184 0.02951 0.03072 0.00742 -0.00170 -0.00207 0.02736 0.00453 0.00006 0.00032 0.00020 0.00000 0.00122 0.00138 0.00140 0.00113 0.00103 0.00107 0.00056 C30 0.22755 0.72342 0.03251 1.00000 0.04222 0.03965 0.04089 0.01160 -0.00469 -0.01704 0.04092 0.00508 0.00007 0.00036 0.00024 0.00000 0.00162 0.00169 0.00169 0.00141 0.00134 0.00139 0.00073 H30A 0.23047 0.69430 -0.04043 1.00000 0.06138 0.00000 0.00000 H30B 0.24948 0.74584 0.06345 1.00000 0.06138 0.00000 0.00000 H30C 0.21339 0.81935 0.03754 1.00000 0.06138 0.00000 0.00000 C31 0.24006 0.59196 0.26340 1.00000 0.02639 0.02845 0.03450 0.00081 -0.00153 -0.00285 0.02978 0.00441 0.00006 0.00032 0.00021 0.00000 0.00132 0.00137 0.00148 0.00117 0.00108 0.00110 0.00059 H31A 0.23610 0.58254 0.33801 1.00000 0.04468 0.00000 0.00000 H31B 0.25156 0.69358 0.24884 1.00000 0.04468 0.00000 0.00000 H31C 0.25400 0.50201 0.24005 1.00000 0.04468 0.00000 0.00000 C32 0.18431 0.72955 0.24047 1.00000 0.03141 0.02171 0.05904 -0.00196 0.00359 -0.00125 0.03739 0.00508 0.00007 0.00032 0.00025 0.00000 0.00140 0.00137 0.00195 0.00133 0.00134 0.00117 0.00068 H32A 0.16295 0.72645 0.20314 1.00000 0.05608 0.00000 0.00000 H32B 0.19581 0.83101 0.22551 1.00000 0.05608 0.00000 0.00000 H32C 0.18011 0.72143 0.31502 1.00000 0.05608 0.00000 0.00000 N21 0.20042 0.46105 0.04136 1.00000 0.02473 0.03153 0.02586 0.00788 -0.00142 -0.00369 0.02738 0.00370 0.00005 0.00026 0.00016 0.00000 0.00106 0.00122 0.00112 0.00097 0.00087 0.00094 0.00048 O21 0.12882 -0.01382 0.35676 1.00000 0.03961 0.02543 0.02879 0.00317 0.00946 -0.00874 0.03128 0.00312 0.00005 0.00022 0.00014 0.00000 0.00105 0.00097 0.00099 0.00079 0.00082 0.00084 0.00043 H21 0.11865 -0.04932 0.40889 1.00000 0.04692 0.00000 0.00000 O22 0.14099 0.18883 0.46467 1.00000 0.05589 0.03715 0.02623 -0.00293 0.01041 -0.01248 0.03976 0.00341 0.00005 0.00024 0.00015 0.00000 0.00128 0.00115 0.00101 0.00089 0.00091 0.00100 0.00050 Final Structure Factor Calculation for pbcn in Pbcn Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 3391 / 22995 wR2 = 0.1450 before cycle 13 for 4862 data and 0 / 279 parameters GooF = S = 1.103; Restrained GooF = 1.103 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0078 * P )^2 + 7.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0711 for 3702 Fo > 4sig(Fo) and 0.1007 for all 4862 data wR2 = 0.1450, GooF = S = 1.103, Restrained GooF = 1.103 for all data Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0279 0.0202 0.0182 C1 0.0253 0.0202 0.0176 C2 0.0243 0.0216 0.0160 C3 0.0220 0.0214 0.0154 C4 0.0247 0.0206 0.0170 C5 0.0327 0.0251 0.0176 C6 0.0326 0.0274 0.0185 C7 0.0232 0.0212 0.0173 C8 0.0263 0.0254 0.0169 C9 0.0449 0.0335 0.0201 C10 0.0290 0.0257 0.0209 C11 0.0376 0.0293 0.0203 C12 0.0268 0.0225 0.0199 N1 0.0403 0.0286 0.0192 O1 0.0350 0.0276 0.0219 O2 0.0293 0.0241 0.0218 C21 0.0251 0.0191 0.0183 C22 0.0277 0.0212 0.0184 C23 0.0278 0.0204 0.0148 C24 0.0265 0.0200 0.0161 C25 0.0267 0.0213 0.0209 C26 0.0285 0.0207 0.0175 C27 0.0313 0.0212 0.0195 C28 0.0380 0.0228 0.0213 C29 0.0638 0.0370 0.0220 C30 0.0351 0.0300 0.0243 C31 0.0596 0.0311 0.0215 C32 0.0382 0.0239 0.0201 N21 0.0469 0.0303 0.0166 O21 0.0650 0.0314 0.0228 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.010 0.016 0.022 0.028 0.035 0.045 0.060 0.087 1.000 Number in group 573. 403. 545. 478. 449. 484. 499. 472. 469. 490. GooF 1.197 1.148 1.160 1.160 1.119 1.092 1.091 0.998 0.901 1.109 K 7.263 1.811 1.336 1.138 1.077 1.047 1.021 0.999 1.001 0.995 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 495. 486. 485. 493. 479. 480. 487. 486. 483. 488. GooF 1.198 1.292 1.233 1.108 1.164 1.061 0.997 0.824 0.921 1.143 K 1.144 1.112 1.060 1.038 1.030 1.001 0.988 0.999 1.021 0.995 R1 0.238 0.248 0.210 0.183 0.140 0.096 0.063 0.047 0.049 0.033 Recommended weighting scheme: WGHT 0.0001 7.3905 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) 18 9 7 1170.50 2354.48 6.02 0.115 0.77 25 8 2 171.25 521.98 5.09 0.054 0.86 4 0 14 -22.32 319.91 5.07 0.042 0.92 30 8 2 13.75 251.13 5.06 0.037 0.81 25 5 0 178.11 492.17 4.84 0.052 1.15 24 8 3 -3.75 124.68 3.74 0.026 0.86 27 9 1 7.68 177.09 3.73 0.031 0.78 38 4 5 115.07 0.80 3.53 0.002 0.88 8 9 7 116.50 0.22 3.50 0.001 0.82 3 1 3 3477.08 4179.02 3.45 0.153 3.68 0 0 2 262.67 466.10 3.36 0.051 6.46 38 6 0 763.73 1265.68 3.32 0.084 0.84 37 4 1 237.13 76.15 3.24 0.021 0.96 28 8 3 90.89 267.76 3.23 0.039 0.82 30 3 12 92.58 5.52 3.15 0.006 0.80 11 2 13 193.68 36.80 3.11 0.014 0.93 45 2 1 332.65 154.65 3.08 0.029 0.87 15 4 13 874.90 539.37 3.05 0.055 0.85 0 8 11 194.99 58.49 3.04 0.018 0.78 36 1 9 -25.82 53.74 3.03 0.017 0.87 46 3 4 247.58 16.10 3.02 0.009 0.80 34 2 11 335.20 158.72 2.99 0.030 0.81 11 2 15 134.46 315.63 2.99 0.042 0.82 45 4 1 155.89 8.97 2.99 0.007 0.81 4 3 5 16027.09 14290.92 2.98 0.282 1.86 18 6 3 47.26 2.47 2.98 0.004 1.13 18 2 15 218.39 85.30 2.96 0.022 0.79 28 1 9 68.37 9.27 2.95 0.007 1.00 13 4 14 465.47 236.74 2.93 0.036 0.81 14 1 15 283.08 26.37 2.92 0.012 0.82 23 8 2 -8.21 70.84 2.91 0.020 0.88 19 8 6 -24.11 63.80 2.90 0.019 0.86 9 4 10 73.77 12.29 2.90 0.008 1.07 27 2 10 110.47 0.73 2.86 0.002 0.95 6 0 16 -36.07 163.80 2.81 0.030 0.80 46 2 0 -47.70 60.36 2.78 0.018 0.85 15 6 4 2599.42 3152.02 2.78 0.133 1.15 3 0 6 2970.16 2473.04 2.78 0.117 2.13 5 7 7 282.17 458.84 2.77 0.051 0.99 48 3 3 156.88 27.75 2.73 0.012 0.78 22 9 5 123.39 9.53 2.73 0.007 0.78 2 0 2 10893.76 12197.66 2.71 0.261 6.15 39 5 3 117.27 260.62 2.71 0.038 0.85 27 0 6 983.20 718.80 2.70 0.063 1.22 41 3 6 91.75 16.58 2.70 0.010 0.85 21 6 1 249.59 438.57 2.70 0.049 1.12 6 3 14 60.27 170.42 2.70 0.031 0.87 1 9 1 252.30 126.54 2.70 0.027 0.92 2 1 1 6692.60 7568.07 2.69 0.205 6.60 0 4 2 2023.40 1649.63 2.68 0.096 1.98 Bond lengths and angles C1 - Distance Angles O2 1.2438 (0.0029) O1 1.3062 (0.0029) 123.00 (0.22) C2 1.4829 (0.0032) 120.83 (0.22) 116.16 (0.21) C1 - O2 O1 C2 - Distance Angles C7 1.3931 (0.0033) C3 1.4022 (0.0033) 120.90 (0.21) C1 1.4829 (0.0032) 120.58 (0.22) 118.52 (0.21) C2 - C7 C3 C3 - Distance Angles C4 1.3767 (0.0032) C2 1.4022 (0.0033) 117.99 (0.22) H3 0.9500 121.01 121.01 C3 - C4 C2 C4 - Distance Angles C3 1.3767 (0.0032) C5 1.3970 (0.0032) 120.34 (0.22) C8 1.5119 (0.0032) 132.15 (0.22) 107.51 (0.19) C4 - C3 C5 C5 - Distance Angles C6 1.3801 (0.0034) C4 1.3970 (0.0032) 122.40 (0.22) N1 1.4242 (0.0030) 126.28 (0.22) 111.31 (0.21) C5 - C6 C4 C6 - Distance Angles C5 1.3801 (0.0034) C7 1.3883 (0.0034) 117.19 (0.22) H6 0.9500 121.41 121.41 C6 - C5 C7 C7 - Distance Angles C6 1.3883 (0.0034) C2 1.3931 (0.0033) 121.18 (0.23) H7 0.9500 119.41 119.41 C7 - C6 C2 C8 - Distance Angles C4 1.5119 (0.0032) C9 1.5222 (0.0033) 99.47 (0.18) C11 1.5310 (0.0033) 113.17 (0.20) 110.48 (0.19) C12 1.5351 (0.0032) 112.09 (0.19) 110.61 (0.20) 110.55 (0.20) C8 - C4 C9 C11 C9 - Distance Angles N1 1.2955 (0.0031) C10 1.4796 (0.0034) 122.70 (0.23) C8 1.5222 (0.0033) 114.47 (0.21) 122.80 (0.22) C9 - N1 C10 C10 - Distance Angles C9 1.4796 (0.0034) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles C8 1.5310 (0.0033) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C8 H11A H11B C12 - Distance Angles C8 1.5351 (0.0032) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C8 H12A H12B N1 - Distance Angles C9 1.2955 (0.0031) C5 1.4242 (0.0030) 107.16 (0.20) N1 - C9 O1 - Distance Angles C1 1.3062 (0.0029) H1 0.8400 109.47 O1 - C1 O2 - Distance Angles C1 1.2438 (0.0029) O2 - C21 - Distance Angles O22 1.2187 (0.0030) O21 1.3245 (0.0030) 123.50 (0.23) C22 1.4954 (0.0033) 123.55 (0.23) 112.94 (0.21) C21 - O22 O21 C22 - Distance Angles C27 1.3954 (0.0034) C23 1.4032 (0.0033) 120.25 (0.22) C21 1.4954 (0.0033) 121.29 (0.22) 118.44 (0.22) C22 - C27 C23 C23 - Distance Angles C24 1.3805 (0.0033) C22 1.4032 (0.0033) 118.45 (0.22) H23 0.9500 120.78 120.78 C23 - C24 C22 C24 - Distance Angles C23 1.3805 (0.0033) C25 1.3951 (0.0034) 120.83 (0.22) C28 1.5097 (0.0033) 131.70 (0.22) 107.45 (0.21) C24 - C23 C25 C25 - Distance Angles C26 1.3864 (0.0033) C24 1.3951 (0.0034) 121.41 (0.22) N21 1.4236 (0.0030) 126.58 (0.22) 112.01 (0.21) C25 - C26 C24 C26 - Distance Angles C25 1.3864 (0.0033) C27 1.3938 (0.0033) 117.80 (0.22) H26 0.9500 121.10 121.10 C26 - C25 C27 C27 - Distance Angles C26 1.3938 (0.0033) C22 1.3954 (0.0034) 121.23 (0.22) H27 0.9500 119.39 119.39 C27 - C26 C22 C28 - Distance Angles C24 1.5097 (0.0033) C29 1.5264 (0.0036) 99.15 (0.20) C32 1.5325 (0.0035) 112.06 (0.20) 111.63 (0.22) C31 1.5416 (0.0034) 112.22 (0.20) 111.27 (0.20) 110.14 (0.22) C28 - C24 C29 C32 C29 - Distance Angles N21 1.2962 (0.0033) C30 1.4866 (0.0036) 122.28 (0.24) C28 1.5264 (0.0036) 115.06 (0.22) 122.66 (0.24) C29 - N21 C30 C30 - Distance Angles C29 1.4866 (0.0036) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C29 H30A H30B C31 - Distance Angles C28 1.5416 (0.0034) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C28 H31A H31B C32 - Distance Angles C28 1.5325 (0.0035) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C28 H32A H32B N21 - Distance Angles C29 1.2962 (0.0033) C25 1.4236 (0.0030) 106.32 (0.21) N21 - C29 O21 - Distance Angles C21 1.3245 (0.0030) H21 0.8400 109.47 O21 - C21 O22 - Distance Angles C21 1.2187 (0.0030) O22 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.77 2.611(2) 173.4 O1-H1...O2_$1 0.84 1.86 2.688(3) 167.1 O21-H21...N1_$2 FMAP and GRID set by program FMAP 2 1 45 GRID -0.595 -2 -1 0.595 2 1 R1 = 0.1006 for 4862 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.0692 0.3207 0.1295 [ 0.71 A from C4 ] Deepest hole -0.32 at 0.0181 0.0199 0.4240 [ 0.69 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3256 / 33345 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0692 0.3207 0.1295 1.00000 0.05 0.29 0.71 C4 0.81 C8 1.79 C5 1.88 C9 Q2 1 0.0738 0.1831 0.1333 1.00000 0.05 0.26 0.68 C4 0.75 C5 1.80 C3 1.85 N1 Q3 1 0.0317 0.0426 0.3165 1.00000 0.05 0.26 0.70 C2 0.82 C1 1.77 O1 1.81 C7 Q4 1 0.0874 0.4413 0.1169 1.00000 0.05 0.25 0.72 C8 0.85 C11 1.42 H11C 1.47 H11B Q5 1 -0.0028 0.1400 0.4738 1.00000 0.05 0.25 0.94 O2 0.97 H1 1.77 O1 1.90 C1 Shortest distances between peaks (including symmetry equivalents) 1 2 1.16 1 4 1.25 2 4 2.22 5 5 2.44 3 5 2.59 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 6.79: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.36: Structure factors and derivatives 6.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.22: Apply other restraints 1.80: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0583pbcn finished at 09:32:41 Total CPU time: 21.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++