+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0817 started at 17:33:27 on 12-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0817 in P-1 CELL 0.71073 5.7619 6.3796 11.6206 92.684 98.060 114.750 ZERR 1.00 0.0002 0.0002 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H B N O UNIT 4 20 6 2 14 V = 381.43 F(000) = 200.0 Mu = 0.16 mm-1 Cell Wt = 385.08 Rho = 1.676 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV $1 X-1, Y, Z EQIV $2 X, Y+1, Z EQIV $3 -X, -Y+1, -Z+2 EQIV $4 -X+1, -Y, -Z+2 EQIV $5 -X, -Y+1, -Z+1 EQIV $6 -X+1, -Y+1, -Z+1 HTAB O4 O7_$1 HTAB O5 O7_$2 HTAB O6 O1_$3 HTAB O7 O2_$4 HTAB N11 O4_$5 HTAB N11 O5_$6 FMAP 2 PLAN 5 SIZE 0.03 0.05 0.08 ACTA BOND $H WGHT 0.01940 0.37080 L.S. 8 TEMP -153.00 FVAR 1.56392 MOLE 1 B1 3 0.057120 0.276526 0.765017 11.00000 0.01441 0.01259 = 0.01046 0.00086 0.00187 0.00729 B2 3 0.181945 0.294758 0.983192 11.00000 0.01239 0.01399 = 0.01350 0.00298 0.00269 0.00641 B3 3 0.296383 0.060821 0.854575 11.00000 0.01087 0.01185 = 0.01311 0.00129 0.00287 0.00434 O1 5 0.064506 0.353670 0.889639 11.00000 0.01610 0.01587 = 0.01086 0.00144 0.00223 0.01020 O2 5 0.302020 0.147179 0.968077 11.00000 0.01681 0.01584 = 0.01131 0.00173 0.00158 0.01044 O3 5 0.184167 0.116859 0.759924 11.00000 0.01572 0.01525 = 0.01045 0.00109 0.00224 0.00976 O4 5 -0.209766 0.160942 0.703662 11.00000 0.01353 0.01651 = 0.01331 0.00313 0.00237 0.00708 AFIX 147 H4 2 -0.302572 0.071832 0.746648 11.00000 -1.50000 AFIX 0 O5 5 0.192319 0.476276 0.705018 11.00000 0.01887 0.01275 = 0.01310 0.00112 0.00447 0.00723 AFIX 147 H5 2 0.244860 0.598806 0.751002 11.00000 -1.50000 AFIX 0 O6 5 0.193075 0.371162 1.095910 11.00000 0.02271 0.02156 = 0.01176 0.00152 0.00173 0.01607 AFIX 147 H6 2 0.112359 0.454309 1.097145 11.00000 -1.50000 AFIX 0 O7 5 0.414840 -0.084456 0.840397 11.00000 0.01615 0.01552 = 0.01100 0.00108 0.00049 0.00989 AFIX 147 H7 2 0.493968 -0.091166 0.905556 11.00000 -1.50000 AFIX 0 MOLE 2 C11 1 0.595621 0.747717 0.498501 11.00000 0.01745 0.01373 = 0.01513 0.00070 0.00035 0.00726 AFIX 23 H11A 2 0.482280 0.784595 0.544344 11.00000 -1.20000 H11B 2 0.717485 0.894086 0.473789 11.00000 -1.20000 AFIX 0 C12 1 0.252728 0.355879 0.425807 11.00000 0.01429 0.01432 = 0.01584 0.00072 0.00114 0.00613 AFIX 23 H12A 2 0.153170 0.247393 0.354209 11.00000 -1.20000 H12B 2 0.128118 0.380115 0.469144 11.00000 -1.20000 AFIX 0 N11 4 0.433982 0.581589 0.393140 11.00000 0.01615 0.01516 = 0.01162 0.00292 0.00219 0.00924 AFIX 23 H11C 2 0.340180 0.645618 0.349228 11.00000 -1.20000 H11D 2 0.540728 0.556376 0.347881 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src0817 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O4 O5 O3 O1 B2 - O1 O6 O2 B3 - O3 O7 O2 O1 - B2 B1 O2 - B3 B2 O3 - B3 B1 O4 - B1 O5 - B1 O6 - B2 O7 - B3 C11 - N11 C12_$6 C12 - N11 C11_$6 N11 - C12 C11 Operators for generating equivalent atoms: $1 x-1, y, z $2 x, y+1, z $3 -x, -y+1, -z+2 $4 -x+1, -y, -z+2 $5 -x, -y+1, -z+1 $6 -x+1, -y+1, -z+1 7332 Reflections read, of which 20 rejected -7 =< h =< 7, -8 =< k =< 8, -15 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1746 Unique reflections, of which 0 suppressed R(int) = 0.0440 R(sigma) = 0.0370 Friedel opposites merged Maximum memory for data reduction = 1626 / 17920 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 = 1964 / 156448 wR2 = 0.0941 before cycle 1 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56392 0.00334 -0.001 OSF Mean shift/esd = 0.003 Maximum = -0.008 for U33 O2 Max. shift = 0.000 A for H4 Max. dU = 0.000 for O5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0941 before cycle 2 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.003 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for O5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0941 before cycle 3 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H6 Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0940 before cycle 4 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H5 Max. dU = 0.000 for N11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0940 before cycle 5 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H5 Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0941 before cycle 6 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for B1 Max. dU = 0.000 for O3 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0940 before cycle 7 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H6 Max. dU = 0.000 for N11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1964 / 156448 wR2 = 0.0941 before cycle 8 for 1746 data and 122 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56391 0.00334 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O6 Max. shift = 0.000 A for H6 Max. dU = 0.000 for O2 Largest correlation matrix elements 0.606 U12 O6 / U22 O6 0.572 U12 O1 / U11 O1 0.547 U12 C12 / U22 C12 0.586 U12 O6 / U11 O6 0.571 U12 O3 / U22 O3 0.542 U12 B1 / U11 B1 0.582 U12 O2 / U22 O2 0.565 U12 O7 / U11 O7 0.541 U12 O5 / U11 O5 0.581 U12 O1 / U22 O1 0.560 U12 N11 / U11 N11 0.541 U12 C12 / U11 C12 0.579 U12 N11 / U22 N11 0.552 U12 O4 / U11 O4 0.536 U12 C11 / U22 C11 0.577 U12 O3 / U11 O3 0.550 U12 O4 / U22 O4 0.529 U12 C11 / U11 C11 0.576 U12 O2 / U11 O2 0.550 U12 O5 / U22 O5 0.528 U12 B2 / U11 B2 0.573 U12 O7 / U22 O7 0.550 U12 B1 / U22 B1 0.527 U12 B3 / U11 B3 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 -0.3026 0.0718 0.7466 147 0.840 0.000 O4 B1 H4 H5 0.2449 0.5988 0.7510 147 0.840 0.000 O5 B1 H5 H6 0.1124 0.4543 1.0971 147 0.840 0.000 O6 B2 H6 H7 0.4940 -0.0912 0.9056 147 0.840 0.000 O7 B3 H7 H11A 0.4823 0.7846 0.5443 23 0.990 0.000 C11 N11 C12_$6 H11B 0.7175 0.8941 0.4738 23 0.990 0.000 C11 N11 C12_$6 H12A 0.1532 0.2474 0.3542 23 0.990 0.000 C12 N11 C11_$6 H12B 0.1281 0.3801 0.4691 23 0.990 0.000 C12 N11 C11_$6 H11C 0.3402 0.6456 0.3492 23 0.920 0.000 N11 C12 C11 H11D 0.5407 0.5564 0.3479 23 0.920 0.000 N11 C12 C11 2008src0817 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.05712 0.27653 0.76502 1.00000 0.01441 0.01258 0.01046 0.00086 0.00188 0.00729 0.01202 0.00426 0.00037 0.00032 0.00016 0.00000 0.00090 0.00087 0.00082 0.00066 0.00067 0.00074 0.00037 B2 0.18194 0.29476 0.98319 1.00000 0.01238 0.01399 0.01350 0.00297 0.00269 0.00640 0.01295 0.00433 0.00037 0.00032 0.00016 0.00000 0.00088 0.00089 0.00088 0.00070 0.00069 0.00075 0.00037 B3 0.29638 0.06082 0.85458 1.00000 0.01086 0.01185 0.01311 0.00129 0.00287 0.00434 0.01205 0.00420 0.00035 0.00032 0.00016 0.00000 0.00087 0.00085 0.00085 0.00066 0.00068 0.00073 0.00036 O1 0.06451 0.35367 0.88964 1.00000 0.01610 0.01587 0.01086 0.00144 0.00223 0.01020 0.01314 0.00266 0.00023 0.00020 0.00010 0.00000 0.00060 0.00059 0.00056 0.00044 0.00045 0.00051 0.00026 O2 0.30202 0.14718 0.96808 1.00000 0.01681 0.01584 0.01130 0.00173 0.00158 0.01044 0.01356 0.00264 0.00023 0.00020 0.00010 0.00000 0.00061 0.00059 0.00057 0.00045 0.00046 0.00051 0.00026 O3 0.18417 0.11686 0.75992 1.00000 0.01572 0.01525 0.01045 0.00109 0.00224 0.00976 0.01276 0.00264 0.00022 0.00020 0.00010 0.00000 0.00061 0.00059 0.00055 0.00044 0.00045 0.00051 0.00026 O4 -0.20977 0.16094 0.70366 1.00000 0.01353 0.01651 0.01331 0.00313 0.00237 0.00708 0.01418 0.00268 0.00023 0.00021 0.00010 0.00000 0.00060 0.00061 0.00058 0.00046 0.00046 0.00050 0.00027 H4 -0.30257 0.07183 0.74665 1.00000 0.02127 0.00000 0.00000 O5 0.19232 0.47628 0.70502 1.00000 0.01887 0.01274 0.01310 0.00112 0.00447 0.00723 0.01459 0.00275 0.00024 0.00020 0.00010 0.00000 0.00063 0.00058 0.00057 0.00044 0.00047 0.00051 0.00027 H5 0.24486 0.59881 0.75100 1.00000 0.02189 0.00000 0.00000 O6 0.19308 0.37116 1.09591 1.00000 0.02271 0.02156 0.01176 0.00152 0.00173 0.01607 0.01656 0.00284 0.00025 0.00022 0.00010 0.00000 0.00067 0.00066 0.00058 0.00047 0.00048 0.00056 0.00028 H6 0.11236 0.45431 1.09715 1.00000 0.02484 0.00000 0.00000 O7 0.41484 -0.08446 0.84040 1.00000 0.01614 0.01552 0.01100 0.00108 0.00049 0.00989 0.01337 0.00267 0.00023 0.00020 0.00010 0.00000 0.00061 0.00060 0.00055 0.00045 0.00045 0.00051 0.00026 H7 0.49396 -0.09117 0.90556 1.00000 0.02006 0.00000 0.00000 C11 0.59562 0.74772 0.49850 1.00000 0.01745 0.01372 0.01513 0.00070 0.00035 0.00726 0.01554 0.00387 0.00034 0.00029 0.00015 0.00000 0.00085 0.00081 0.00081 0.00063 0.00065 0.00070 0.00035 H11A 0.48228 0.78460 0.54434 1.00000 0.01865 0.00000 0.00000 H11B 0.71749 0.89409 0.47379 1.00000 0.01865 0.00000 0.00000 C12 0.25273 0.35588 0.42581 1.00000 0.01429 0.01432 0.01583 0.00072 0.00114 0.00613 0.01502 0.00383 0.00033 0.00029 0.00015 0.00000 0.00083 0.00081 0.00082 0.00064 0.00065 0.00070 0.00035 H12A 0.15317 0.24739 0.35421 1.00000 0.01803 0.00000 0.00000 H12B 0.12812 0.38012 0.46914 1.00000 0.01803 0.00000 0.00000 N11 0.43398 0.58159 0.39314 1.00000 0.01615 0.01516 0.01162 0.00292 0.00219 0.00924 0.01342 0.00318 0.00028 0.00024 0.00012 0.00000 0.00072 0.00071 0.00066 0.00053 0.00054 0.00061 0.00030 H11C 0.34018 0.64562 0.34923 1.00000 0.01610 0.00000 0.00000 H11D 0.54073 0.55638 0.34788 1.00000 0.01610 0.00000 0.00000 Final Structure Factor Calculation for 2008src0817 in P-1 Total number of l.s. parameters = 122 Maximum vector length = 511 Memory required = 1842 / 24017 wR2 = 0.0941 before cycle 9 for 1746 data and 0 / 122 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0194 * P )^2 + 0.37 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0416 for 1479 Fo > 4sig(Fo) and 0.0525 for all 1746 data wR2 = 0.0941, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0150 0.0109 0.0101 B1 0.0150 0.0124 0.0114 B2 0.0136 0.0122 0.0104 B3 0.0185 0.0109 0.0101 O1 0.0190 0.0117 0.0099 O2 0.0178 0.0108 0.0097 O3 0.0169 0.0134 0.0122 O4 0.0193 0.0133 0.0111 O5 0.0273 0.0119 0.0105 O6 0.0188 0.0118 0.0096 O7 0.0196 0.0139 0.0131 C11 0.0172 0.0144 0.0135 C12 0.0175 0.0128 0.0100 N11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.029 0.044 0.060 0.080 0.104 0.133 0.170 0.240 1.000 Number in group 175. 176. 187. 163. 178. 178. 165. 174. 174. 176. GooF 1.091 1.121 1.187 1.150 1.092 1.108 1.057 0.957 0.940 1.199 K 2.471 1.190 1.073 0.982 0.974 1.002 0.986 1.002 1.011 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 180. 171. 177. 174. 173. 172. 174. 175. 178. 172. GooF 1.192 1.201 1.133 0.984 0.984 1.090 0.923 0.916 0.988 1.427 K 1.053 1.028 1.018 1.010 1.004 0.992 0.998 0.999 1.013 0.998 R1 0.121 0.104 0.105 0.073 0.068 0.049 0.032 0.035 0.027 0.028 Recommended weighting scheme: WGHT 0.0193 0.3707 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) -4 1 9 5.74 0.11 3.47 0.005 1.02 -3 3 1 619.55 536.60 3.41 0.361 1.69 -1 -3 14 0.85 7.75 3.35 0.043 0.78 -3 -3 6 4.78 0.51 3.23 0.011 1.01 -2 2 2 10.82 5.15 3.18 0.035 2.38 -1 0 4 56.28 74.88 3.17 0.135 2.71 -1 1 1 5.07 1.61 3.13 0.020 4.76 -2 2 3 420.06 367.86 3.06 0.299 2.18 0 1 1 2342.49 2555.70 3.05 0.787 4.91 1 6 4 56.76 81.46 3.03 0.141 0.81 0 1 3 1011.06 1118.10 3.01 0.521 3.02 1 -2 3 20.64 31.15 2.92 0.087 2.45 -4 -4 1 18.16 7.74 2.88 0.043 0.81 3 -4 8 41.53 56.44 2.87 0.117 1.00 -1 0 2 2253.22 2474.64 2.84 0.775 4.21 2 2 11 29.07 42.57 2.84 0.102 0.81 -3 6 0 7.65 3.27 2.80 0.028 1.05 1 -1 3 1953.18 2127.26 2.78 0.718 2.95 6 0 1 12.01 50.40 2.66 0.111 0.85 -2 1 14 10.30 4.59 2.64 0.033 0.81 -2 -4 10 10.18 3.64 2.64 0.030 0.85 5 -4 9 41.60 25.96 2.63 0.079 0.79 -4 -2 2 -1.32 1.69 2.62 0.020 1.04 -1 3 0 446.50 401.40 2.59 0.312 2.12 -7 5 3 3.52 11.72 2.57 0.053 0.79 -4 5 2 25.77 35.74 2.56 0.093 1.12 -1 7 4 6.41 14.18 2.54 0.059 0.81 -1 1 0 545.67 603.44 2.53 0.382 5.07 -3 0 7 2.36 0.00 2.50 0.001 1.30 -4 6 9 0.19 3.40 2.49 0.029 0.79 1 -1 13 7.54 3.06 2.46 0.027 0.86 -6 3 2 2.59 8.75 2.41 0.046 0.96 -3 -1 13 7.10 2.55 2.41 0.025 0.82 -3 8 3 77.81 53.92 2.39 0.114 0.77 -2 0 3 120.97 100.69 2.38 0.156 2.33 1 0 1 1341.68 1447.61 2.38 0.592 4.41 2 5 4 7.97 1.85 2.37 0.021 0.83 -1 0 1 16.34 23.50 2.36 0.075 5.04 3 -4 12 10.88 4.56 2.35 0.033 0.79 -2 -5 8 3.54 10.41 2.34 0.050 0.83 -1 -6 8 13.69 24.23 2.32 0.077 0.80 -3 -1 14 4.29 0.21 2.32 0.007 0.78 4 -6 8 15.96 7.87 2.31 0.044 0.82 -1 2 12 11.33 18.32 2.30 0.067 0.91 3 1 5 5.33 10.08 2.30 0.049 1.15 -2 4 1 138.23 116.34 2.27 0.168 1.56 0 -2 12 34.91 25.09 2.26 0.078 0.94 2 -1 3 1015.11 939.15 2.23 0.477 2.15 -1 1 2 470.50 517.45 2.23 0.354 3.93 -3 -5 3 90.64 72.04 2.23 0.132 0.82 Bond lengths and angles B1 - Distance Angles O4 1.4528 (0.0022) O5 1.4564 (0.0022) 107.42 (0.13) O3 1.4859 (0.0021) 109.99 (0.14) 108.78 (0.13) O1 1.4966 (0.0021) 110.12 (0.14) 110.32 (0.13) 110.16 (0.13) B1 - O4 O5 O3 B2 - Distance Angles O1 1.3513 (0.0021) O6 1.3594 (0.0022) 123.75 (0.15) O2 1.4000 (0.0022) 120.59 (0.15) 115.67 (0.15) B2 - O1 O6 B3 - Distance Angles O3 1.3366 (0.0021) O7 1.3780 (0.0021) 119.22 (0.15) O2 1.3961 (0.0021) 122.39 (0.15) 118.38 (0.15) B3 - O3 O7 O1 - Distance Angles B2 1.3513 (0.0021) B1 1.4966 (0.0021) 124.38 (0.13) O1 - B2 O2 - Distance Angles B3 1.3961 (0.0021) B2 1.4000 (0.0022) 118.72 (0.13) O2 - B3 O3 - Distance Angles B3 1.3366 (0.0021) B1 1.4859 (0.0021) 123.69 (0.13) O3 - B3 O4 - Distance Angles B1 1.4528 (0.0022) H4 0.8400 109.47 O4 - B1 O5 - Distance Angles B1 1.4564 (0.0022) H5 0.8400 109.47 O5 - B1 O6 - Distance Angles B2 1.3594 (0.0022) H6 0.8400 109.47 O6 - B2 O7 - Distance Angles B3 1.3780 (0.0021) H7 0.8400 109.47 O7 - B3 C11 - Distance Angles N11 1.4906 (0.0021) C12_$6 1.5154 (0.0023) 110.46 (0.13) H11A 0.9900 109.56 109.56 H11B 0.9900 109.56 109.56 108.11 C11 - N11 C12_$6 H11A C12 - Distance Angles N11 1.4871 (0.0021) C11_$6 1.5154 (0.0023) 109.82 (0.14) H12A 0.9900 109.70 109.70 H12B 0.9900 109.70 109.70 108.19 C12 - N11 C11_$6 H12A N11 - Distance Angles C12 1.4871 (0.0021) C11 1.4906 (0.0021) 111.59 (0.13) H11C 0.9200 109.30 109.30 H11D 0.9200 109.30 109.30 107.96 N11 - C12 C11 H11C Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.02 2.8312(17) 162.8 O4-H4...O7_$1 0.84 2.00 2.8258(16) 169.5 O5-H5...O7_$2 0.84 1.91 2.7453(16) 176.4 O6-H6...O1_$3 0.84 1.89 2.7179(16) 167.0 O7-H7...O2_$4 0.92 1.78 2.6786(18) 163.3 N11-H11C...O4_$5 0.92 1.82 2.7182(19) 165.0 N11-H11D...O5_$6 FMAP and GRID set by program FMAP 2 1 18 GRID -3.333 -2 -2 3.333 2 2 R1 = 0.0525 for 1746 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.3386 0.3292 0.4723 [ 0.75 A from C12 ] Deepest hole -0.32 at 0.0443 0.2448 0.6996 [ 0.76 A from B1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1924 / 15588 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3386 0.3292 0.4723 1.00000 0.05 0.30 0.75 C12 0.80 C11 1.38 H12B 1.51 H11B Q2 1 0.4085 0.1137 1.0055 1.00000 0.05 0.22 0.81 O2 1.15 H7 1.75 B3 1.96 H7 Q3 1 0.3041 0.1253 0.9182 1.00000 0.05 0.22 0.59 O2 0.82 B3 1.72 B2 1.86 O3 Q4 1 -0.2049 0.0290 0.6478 1.00000 0.05 0.20 1.05 O4 1.41 H4 1.91 H12A 1.96 B1 Q5 1 0.2950 0.7476 0.3135 1.00000 0.05 0.20 0.89 H11C 0.92 O4 1.36 H4 1.79 N11 Shortest distances between peaks (including symmetry equivalents) 2 3 1.13 4 5 1.77 2 2 2.13 1 1 2.18 1 4 2.38 2 3 2.77 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.08: Structure factors and derivatives 0.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0817 finished at 17:33:42 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++