+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07rc0001 started at 15:56:32 on 24-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07rc0001 in P-1 CELL 0.71073 5.1231 8.7759 9.2683 62.246 75.259 82.642 ZERR 2.00 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 14 10 2 10 V = 356.60 F(000) = 188.0 Mu = 0.15 mm-1 Cell Wt = 366.24 Rho = 1.705 MERG 2 OMIT -3.00 55.00 OMIT 2 4 0 EXTI 0.06759 SHEL 7 0.77 EQIV $1 -X+1, -Y, -Z-1 HTAB O1 O2 HTAB O3 O2_$1 FMAP 2 PLAN 5 SIZE 0.11 0.24 0.28 ACTA BOND $H WGHT 0.06070 0.10120 L.S. 9 TEMP -153.00 FVAR 2.51851 C1 1 0.063560 0.207384 -0.304093 11.00000 0.01428 0.01404 = 0.01413 -0.00751 -0.00231 0.00125 C2 1 -0.147075 0.309702 -0.376145 11.00000 0.01559 0.01690 = 0.01292 -0.00624 -0.00338 -0.00121 C3 1 -0.318168 0.402114 -0.299099 11.00000 0.01325 0.01933 = 0.01786 -0.00819 -0.00481 0.00387 AFIX 43 H3 2 -0.460583 0.471160 -0.347746 11.00000 -1.20000 AFIX 0 C4 1 -0.280416 0.393066 -0.153650 11.00000 0.01534 0.01837 = 0.01747 -0.01038 -0.00143 0.00254 AFIX 43 H4 2 -0.394980 0.456145 -0.101833 11.00000 -1.20000 AFIX 0 C5 1 -0.071736 0.290074 -0.083191 11.00000 0.01721 0.01648 = 0.01191 -0.00683 -0.00280 -0.00067 C6 1 0.099944 0.197590 -0.155357 11.00000 0.01485 0.01369 = 0.01431 -0.00552 -0.00400 0.00182 AFIX 43 H6 2 0.240662 0.128339 -0.104886 11.00000 -1.20000 AFIX 0 C7 1 0.248415 0.112098 -0.385256 11.00000 0.01462 0.01508 = 0.01513 -0.00702 -0.00365 0.00046 N1 3 -0.031492 0.279502 0.071901 11.00000 0.01915 0.01752 = 0.01477 -0.00849 -0.00258 -0.00006 O1 4 -0.197390 0.325947 -0.518384 11.00000 0.01860 0.02545 = 0.01597 -0.01237 -0.00744 0.00608 AFIX 83 H1 2 -0.085407 0.266216 -0.554622 11.00000 -1.50000 AFIX 0 O2 4 0.236426 0.128916 -0.523615 11.00000 0.02211 0.02575 = 0.01681 -0.01420 -0.00676 0.00696 O3 4 0.421367 0.010291 -0.298788 11.00000 0.01913 0.02051 = 0.01696 -0.01118 -0.00603 0.00887 AFIX 83 H3A 2 0.519604 -0.039446 -0.352061 11.00000 -1.50000 AFIX 0 O4 4 -0.189707 0.358484 0.138452 11.00000 0.02714 0.02605 = 0.01920 -0.01635 -0.00251 0.00384 O5 4 0.156945 0.191231 0.129751 11.00000 0.02809 0.03440 = 0.02126 -0.01596 -0.01309 0.00980 HKLF 4 Covalent radii and connectivity table for 07rc0001 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 C7 C2 - O1 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 N1 C6 - C5 C1 C7 - O2 O3 C1 N1 - O5 O4 C5 O1 - C2 O2 - C7 O3 - C7 O4 - N1 O5 - N1 Operators for generating equivalent atoms: $1 -x+1, -y, -z-1 7399 Reflections read, of which 7 rejected -6 =< h =< 6, -11 =< k =< 11, -12 =< l =< 12, Max. 2-theta = 54.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 -7 1 0.23 0.18 4 1.36 1 Inconsistent equivalents 1635 Unique reflections, of which 0 suppressed R(int) = 0.0295 R(sigma) = 0.0283 Friedel opposites merged Maximum memory for data reduction = 1171 / 16547 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 = 1473 / 151991 wR2 = 0.1055 before cycle 1 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51839 0.00941 -0.013 OSF 2 0.06793 0.02056 0.017 EXTI Mean shift/esd = 0.040 Maximum = -0.108 for U33 C1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 2 for 1635 data and 119 / 119 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51802 0.00941 -0.039 OSF 2 0.06792 0.02058 0.000 EXTI Mean shift/esd = 0.014 Maximum = -0.039 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 3 for 1635 data and 119 / 119 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 -0.002 OSF 2 0.06789 0.02057 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 4 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 0.001 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y C7 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 5 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51801 0.00941 0.000 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for O5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 6 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 0.000 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C6 Max. dU = 0.000 for C4 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 7 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 0.000 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for O2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 8 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 0.000 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C6 Max. dU = 0.000 for C3 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1473 / 151991 wR2 = 0.1055 before cycle 9 for 1635 data and 119 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.51800 0.00941 0.000 OSF 2 0.06789 0.02057 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H6 Max. dU = 0.000 for O3 Largest correlation matrix elements -0.642 U23 O4 / U22 O4 -0.598 U23 O1 / U22 O1 -0.563 U23 C5 / U22 C5 -0.621 U23 O2 / U22 O2 -0.592 U23 O5 / U33 O5 -0.558 U23 C7 / U22 C7 -0.620 U23 O4 / U33 O4 -0.589 U23 C4 / U22 C4 -0.550 U23 C2 / U22 C2 0.618 EXTI / OSF -0.576 U23 O1 / U33 O1 -0.546 U23 C3 / U22 C3 -0.607 U23 O3 / U22 O3 -0.570 U23 C4 / U33 C4 -0.539 U23 N1 / U33 N1 -0.605 U23 O5 / U22 O5 -0.569 U23 C1 / U22 C1 -0.534 U23 C7 / U33 C7 -0.604 U23 O2 / U33 O2 -0.567 U23 N1 / U22 N1 -0.533 U23 C3 / U33 C3 -0.600 U23 O3 / U33 O3 -0.566 U23 C6 / U22 C6 -0.530 U23 C2 / U33 C2 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.4606 0.4712 -0.3478 43 0.950 0.000 C3 C4 C2 H4 -0.3950 0.4561 -0.1018 43 0.950 0.000 C4 C3 C5 H6 0.2406 0.1283 -0.1049 43 0.950 0.000 C6 C5 C1 H1 -0.0854 0.2662 -0.5546 83 0.840 0.000 O1 C2 H1 H3A 0.5196 -0.0394 -0.3521 83 0.840 0.000 O3 C7 H3A 07rc0001 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.06356 0.20739 -0.30411 1.00000 0.01425 0.01397 0.01405 -0.00746 -0.00229 0.00121 0.01394 0.00163 0.00023 0.00015 0.00015 0.00000 0.00056 0.00057 0.00057 0.00047 0.00044 0.00043 0.00028 C2 -0.14707 0.30970 -0.37614 1.00000 0.01555 0.01683 0.01288 -0.00622 -0.00334 -0.00123 0.01515 0.00162 0.00024 0.00015 0.00015 0.00000 0.00057 0.00058 0.00056 0.00047 0.00044 0.00043 0.00028 C3 -0.31817 0.40212 -0.29911 1.00000 0.01323 0.01927 0.01781 -0.00817 -0.00479 0.00385 0.01698 0.00174 0.00024 0.00016 0.00015 0.00000 0.00056 0.00061 0.00060 0.00049 0.00044 0.00043 0.00029 H3 -0.46058 0.47117 -0.34776 1.00000 0.02038 0.00000 0.00000 C4 -0.28041 0.39306 -0.15364 1.00000 0.01532 0.01831 0.01742 -0.01035 -0.00141 0.00253 0.01682 0.00173 0.00024 0.00016 0.00015 0.00000 0.00058 0.00060 0.00060 0.00050 0.00045 0.00044 0.00028 H4 -0.39498 0.45612 -0.10182 1.00000 0.02018 0.00000 0.00000 C5 -0.07172 0.29007 -0.08319 1.00000 0.01718 0.01646 0.01183 -0.00680 -0.00278 -0.00071 0.01503 0.00162 0.00024 0.00015 0.00014 0.00000 0.00059 0.00059 0.00057 0.00047 0.00045 0.00044 0.00028 C6 0.09993 0.19759 -0.15536 1.00000 0.01481 0.01364 0.01426 -0.00548 -0.00398 0.00181 0.01461 0.00164 0.00024 0.00015 0.00015 0.00000 0.00056 0.00056 0.00058 0.00046 0.00043 0.00043 0.00028 H6 0.24064 0.12833 -0.10489 1.00000 0.01754 0.00000 0.00000 C7 0.24840 0.11210 -0.38525 1.00000 0.01457 0.01503 0.01507 -0.00699 -0.00362 0.00046 0.01481 0.00164 0.00023 0.00015 0.00015 0.00000 0.00056 0.00056 0.00056 0.00047 0.00043 0.00043 0.00028 N1 -0.03150 0.27950 0.07189 1.00000 0.01912 0.01748 0.01471 -0.00846 -0.00257 -0.00005 0.01688 0.00142 0.00021 0.00013 0.00013 0.00000 0.00054 0.00052 0.00052 0.00041 0.00039 0.00039 0.00027 O1 -0.19738 0.32595 -0.51839 1.00000 0.01858 0.02540 0.01592 -0.01234 -0.00743 0.00609 0.01864 0.00122 0.00018 0.00012 0.00011 0.00000 0.00046 0.00049 0.00046 0.00039 0.00035 0.00035 0.00025 H1 -0.08539 0.26621 -0.55462 1.00000 0.02796 0.00000 0.00000 O2 0.23642 0.12891 -0.52362 1.00000 0.02208 0.02569 0.01678 -0.01416 -0.00676 0.00694 0.01988 0.00126 0.00018 0.00012 0.00011 0.00000 0.00047 0.00051 0.00046 0.00039 0.00035 0.00036 0.00025 O3 0.42137 0.01030 -0.29880 1.00000 0.01911 0.02049 0.01691 -0.01117 -0.00602 0.00887 0.01822 0.00119 0.00017 0.00011 0.00010 0.00000 0.00047 0.00047 0.00045 0.00038 0.00034 0.00034 0.00025 H3A 0.51960 -0.03944 -0.35208 1.00000 0.02733 0.00000 0.00000 O4 -0.18971 0.35849 0.13845 1.00000 0.02714 0.02599 0.01916 -0.01632 -0.00249 0.00383 0.02256 0.00126 0.00019 0.00012 0.00011 0.00000 0.00053 0.00052 0.00048 0.00042 0.00038 0.00039 0.00026 O5 0.15694 0.19122 0.12976 1.00000 0.02806 0.03435 0.02125 -0.01593 -0.01310 0.00980 0.02598 0.00135 0.00020 0.00013 0.00012 0.00000 0.00054 0.00057 0.00050 0.00044 0.00040 0.00041 0.00027 Final Structure Factor Calculation for 07rc0001 in P-1 Total number of l.s. parameters = 119 Maximum vector length = 511 Memory required = 1354 / 22995 wR2 = 0.1055 before cycle 10 for 1635 data and 0 / 119 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0607 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0388 for 1445 Fo > 4sig(Fo) and 0.0443 for all 1635 data wR2 = 0.1055, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0159 0.0148 0.0112 C1 0.0178 0.0150 0.0127 C2 0.0220 0.0178 0.0112 C3 0.0202 0.0193 0.0109 C4 0.0175 0.0164 0.0112 C5 0.0170 0.0149 0.0119 C6 0.0155 0.0148 0.0141 C7 0.0198 0.0176 0.0132 N1 0.0293 0.0151 0.0116 O1 0.0314 0.0172 0.0110 O2 0.0293 0.0153 0.0100 O3 0.0311 0.0265 0.0100 O4 0.0419 0.0223 0.0136 O5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.039 0.060 0.082 0.105 0.132 0.170 0.223 0.328 1.000 Number in group 164. 163. 172. 166. 152. 164. 165. 165. 161. 163. GooF 1.003 0.974 1.112 1.121 1.114 1.005 1.062 0.977 0.979 1.101 K 1.348 0.981 0.945 0.960 0.981 0.989 1.002 1.022 1.024 1.021 Resolution(A) 0.77 0.80 0.83 0.86 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 168. 160. 167. 162. 163. 161. 163. 167. 161. 163. GooF 1.003 0.999 1.076 1.021 0.914 0.930 0.899 1.067 1.061 1.405 K 1.034 1.040 1.019 1.019 1.034 1.016 1.038 1.040 1.031 0.994 R1 0.077 0.085 0.072 0.055 0.040 0.041 0.033 0.033 0.033 0.034 Recommended weighting scheme: WGHT 0.0599 0.1035 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 2 1 2.38 0.60 4.52 0.018 2.04 3 -3 3 26.06 38.67 3.91 0.149 1.20 4 -1 3 26.55 37.82 3.91 0.147 1.18 2 -2 3 2.63 5.52 3.84 0.056 1.60 -2 5 5 2.13 4.82 3.69 0.053 1.18 3 -6 4 6.68 11.34 3.38 0.081 0.83 -1 1 3 28.04 37.54 3.29 0.147 2.30 3 0 3 19.63 26.72 3.20 0.124 1.57 1 2 2 16.45 22.62 3.17 0.114 3.37 0 3 3 102.39 128.68 3.15 0.272 2.51 2 1 1 158.15 196.19 3.08 0.335 2.52 -2 -6 4 7.94 13.20 3.06 0.087 0.83 2 4 9 76.96 97.15 3.00 0.236 1.02 5 -6 1 59.55 42.36 2.98 0.156 0.77 1 -1 1 226.67 276.86 2.86 0.398 3.61 -2 6 5 42.06 53.66 2.86 0.175 1.10 4 -4 4 1.48 3.80 2.80 0.047 0.90 2 2 2 13.63 9.79 2.79 0.075 2.32 0 5 11 23.12 14.11 2.77 0.090 0.81 -4 -4 4 7.57 12.29 2.76 0.084 0.80 1 1 5 95.01 78.33 2.75 0.212 1.77 2 3 10 10.47 15.20 2.75 0.093 0.91 2 4 10 0.27 1.40 2.68 0.028 0.92 4 -3 7 16.68 11.22 2.67 0.080 0.80 -2 8 9 2.00 4.36 2.66 0.050 0.78 -2 2 4 1.99 0.75 2.66 0.021 1.48 -4 5 7 3.60 6.84 2.66 0.063 0.78 1 3 1 176.33 211.71 2.65 0.348 2.59 2 4 8 0.43 1.56 2.63 0.030 1.13 -1 1 2 0.63 0.04 2.63 0.005 2.96 3 -1 1 12.99 9.61 2.56 0.074 1.62 6 -1 2 8.10 12.02 2.54 0.083 0.83 2 3 5 84.19 70.29 2.54 0.201 1.65 4 9 3 3.05 5.54 2.53 0.056 0.79 4 -2 2 9.17 6.57 2.53 0.061 1.15 1 2 10 4.66 7.20 2.52 0.064 0.89 0 -1 5 73.33 60.98 2.52 0.187 1.44 3 -5 3 78.95 96.47 2.48 0.235 0.98 -1 3 4 60.40 73.09 2.44 0.205 1.79 2 1 3 60.22 50.16 2.44 0.170 2.19 4 4 2 0.74 0.02 2.44 0.004 1.14 -4 6 4 27.14 20.74 2.43 0.109 0.86 -5 1 5 11.64 16.09 2.39 0.096 0.78 4 4 10 8.11 5.29 2.38 0.055 0.83 -1 4 1 4.32 6.39 2.36 0.061 1.90 5 -2 6 2.47 4.54 2.35 0.051 0.82 1 2 7 59.49 71.26 2.34 0.202 1.30 -3 -6 2 0.28 1.16 2.33 0.026 0.89 -3 1 3 27.59 22.28 2.32 0.113 1.31 -4 6 2 25.75 33.94 2.32 0.140 0.90 Bond lengths and angles C1 - Distance Angles C6 1.3996 (0.0016) C2 1.4059 (0.0017) 119.62 (0.11) C7 1.4772 (0.0016) 119.85 (0.11) 120.53 (0.11) C1 - C6 C2 C2 - Distance Angles O1 1.3466 (0.0014) C3 1.4052 (0.0017) 116.55 (0.11) C1 1.4059 (0.0017) 123.58 (0.11) 119.87 (0.11) C2 - O1 C3 C3 - Distance Angles C4 1.3749 (0.0017) C2 1.4052 (0.0017) 120.30 (0.11) H3 0.9500 119.85 119.85 C3 - C4 C2 C4 - Distance Angles C3 1.3749 (0.0017) C5 1.3944 (0.0017) 119.12 (0.11) H4 0.9500 120.44 120.44 C4 - C3 C5 C5 - Distance Angles C6 1.3794 (0.0017) C4 1.3944 (0.0017) 122.13 (0.11) N1 1.4625 (0.0015) 118.56 (0.11) 119.31 (0.10) C5 - C6 C4 C6 - Distance Angles C5 1.3794 (0.0017) C1 1.3996 (0.0016) 118.97 (0.11) H6 0.9500 120.52 120.52 C6 - C5 C1 C7 - Distance Angles O2 1.2376 (0.0014) O3 1.3105 (0.0014) 123.84 (0.11) C1 1.4772 (0.0016) 121.60 (0.11) 114.56 (0.10) C7 - O2 O3 N1 - Distance Angles O5 1.2267 (0.0014) O4 1.2320 (0.0014) 123.36 (0.10) C5 1.4625 (0.0015) 118.25 (0.10) 118.38 (0.10) N1 - O5 O4 O1 - Distance Angles C2 1.3466 (0.0014) H1 0.8400 109.47 O1 - C2 O2 - Distance Angles C7 1.2376 (0.0014) O2 - O3 - Distance Angles C7 1.3105 (0.0014) H3A 0.8400 109.47 O3 - C7 O4 - Distance Angles N1 1.2320 (0.0014) O4 - O5 - Distance Angles N1 1.2267 (0.0014) O5 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.91 2.6401(12) 144.0 O1-H1...O2 0.84 1.83 2.6704(12) 173.3 O3-H3A...O2_$1 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0443 for 1635 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.0758 0.2046 0.7061 [ 0.12 A from C1 ] Deepest hole -0.32 at 0.3321 0.0581 0.5954 [ 0.65 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1490 / 15009 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1480 0.1777 -0.3405 1.00000 0.05 0.30 0.59 C1 0.90 C7 1.76 C6 1.78 C2 Q2 1 -0.2144 0.3156 -0.1049 1.00000 0.05 0.27 0.72 C4 0.78 C5 1.45 H4 1.79 C3 Q3 1 -0.0401 0.2606 -0.3403 1.00000 0.05 0.27 0.70 C1 0.70 C2 1.84 O1 1.84 C6 Q4 1 0.0041 0.2532 -0.1160 1.00000 0.05 0.23 0.59 C5 0.79 C6 1.52 H6 1.78 C4 Q5 1 -0.2380 0.4230 -0.2509 1.00000 0.05 0.22 0.77 C3 0.79 C4 1.53 H3 1.55 H4 Shortest distances between peaks (including symmetry equivalents) 1 3 1.13 2 4 1.18 2 5 1.27 4 5 1.98 3 5 2.01 3 4 2.12 2 3 2.38 1 4 2.39 1 5 3.00 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. 0.33: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.28: Structure factors and derivatives 0.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.13: 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 +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07rc0001 finished at 15:56:34 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++