+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0029p21m started at 15:55:52 on 09-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0029p21m in P2(1)/m CELL 0.71073 8.1472 6.4965 9.0107 90.000 97.401 90.000 ZERR 2.00 0.0007 0.0005 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 16 24 4 8 V = 472.95 F(000) = 212.0 Mu = 0.11 mm-1 Cell Wt = 400.39 Rho = 1.406 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x+1, y, z HTAB O4B O1A_$1 HTAB N21 O1A_$1 EQIV_$2 x+1, y, z-1 HTAB N23 O1B_$2 FMAP 2 PLAN 10 SIZE 0.01 0.06 0.12 ACTA BOND $H WGHT 0.03250 0.26620 L.S. 8 TEMP -153.00 FVAR 1.45709 MOLE 1 C1 1 0.077109 0.250000 0.646708 10.50000 0.01414 0.02103 = 0.01835 0.00000 0.00256 0.00000 C2 1 0.233122 0.250000 0.571032 10.50000 0.01533 0.03026 = 0.01593 0.00000 0.00324 0.00000 AFIX 23 H2A 2 0.231398 0.127091 0.505897 10.50000 -1.20000 H2B 2 0.231398 0.372909 0.505897 10.50000 -1.20000 AFIX 0 C3 1 0.393533 0.250000 0.676576 10.50000 0.01380 0.02620 = 0.01529 0.00000 0.00375 0.00000 AFIX 23 H3A 2 0.397163 0.373215 0.741567 10.50000 -1.20000 H3B 2 0.397163 0.126785 0.741567 10.50000 -1.20000 AFIX 0 C4 1 0.542972 0.250000 0.593372 10.50000 0.01521 0.02056 = 0.01629 0.00000 0.00273 0.00000 O1A 4 -0.058453 0.250000 0.556824 10.50000 0.01186 0.04186 = 0.01810 0.00000 0.00261 0.00000 O1B 4 0.085413 0.250000 0.785051 10.50000 0.01806 0.03617 = 0.01489 0.00000 0.00443 0.00000 O4A 4 0.536512 0.250000 0.458721 10.50000 0.01840 0.04527 = 0.01573 0.00000 0.00288 0.00000 O4B 4 0.683133 0.250000 0.686214 10.50000 0.01283 0.04018 = 0.01773 0.00000 0.00349 0.00000 AFIX 83 H4 2 0.763711 0.250000 0.636688 10.50000 0.04968 AFIX 0 MOLE 2 C22 1 1.002495 0.250000 0.145181 10.50000 0.02600 0.01847 = 0.01801 0.00000 0.00536 0.00000 C24 1 0.742131 0.250000 0.039007 10.50000 0.02214 0.03165 = 0.02136 0.00000 0.00537 0.00000 AFIX 43 H24 2 0.648122 0.250000 -0.035271 10.50000 -1.20000 AFIX 0 C25 1 0.741110 0.250000 0.187712 10.50000 0.02364 0.02636 = 0.02226 0.00000 0.00705 0.00000 AFIX 43 H25 2 0.646190 0.250000 0.238882 10.50000 -1.20000 AFIX 0 C26 1 1.185558 0.250000 0.163420 10.50000 0.02826 0.03265 = 0.02309 0.00000 0.00339 0.00000 AFIX 33 H26A 2 1.223837 0.250000 0.064676 10.50000 -1.50000 H26B 2 1.227057 0.126831 0.218833 10.50000 -1.50000 H26C 2 1.227057 0.373169 0.218834 10.50000 -1.50000 AFIX 0 N21 3 0.903596 0.250000 0.252027 10.50000 0.02991 0.02592 = 0.01451 0.00000 0.00479 0.00000 AFIX 43 H21 2 0.937124 0.250000 0.348852 10.50000 0.04786 AFIX 0 N23 3 0.905662 0.250000 0.014573 10.50000 0.02388 0.02727 = 0.01591 0.00000 0.00597 0.00000 AFIX 43 H23 2 0.940622 0.250000 -0.073850 10.50000 0.05303 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0029p21m in P2(1)/m C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - N23 N21 C26 C24 - C25 N23 C25 - C24 N21 C26 - C22 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 x+1, y, z $2 x+1, y, z-1 h k l Fo^2 Sigma Why rejected 0 7 0 68.92 17.20 observed but should be systematically absent 6276 Reflections read, of which 21 rejected -10 =< h =< 10, -8 =< k =< 8, -11 =< l =< 11, Max. 2-theta = 54.95 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 3 2 2.17 0.67 7 3.61 1 Inconsistent equivalents 1184 Unique reflections, of which 0 suppressed R(int) = 0.0545 R(sigma) = 0.0450 Friedel opposites merged Maximum memory for data reduction = 1540 / 11605 Special position constraints for C1 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C2 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C3 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C4 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1A y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1B y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O4A y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O4B y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C22 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C24 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C25 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C26 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N21 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N23 y = 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 = 1868 / 117023 wR2 = 0.1076 before cycle 1 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U33 O1A Max. shift = 0.000 A for C24 Max. dU = 0.000 for H23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 2 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U33 O1A Max. shift = 0.000 A for C4 Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 3 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O4A Max. dU = 0.000 for H4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 4 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for N21 Max. dU = 0.000 for H23 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 5 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for C2 Max. dU = 0.000 for H23 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 6 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for C25 Max. dU = 0.000 for H23 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 7 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for C24 Max. dU = 0.000 for H23 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1868 / 117023 wR2 = 0.1076 before cycle 8 for 1184 data and 88 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45708 0.00464 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for C25 Max. dU = 0.000 for H4 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.2314 0.1271 0.5059 23 0.990 0.000 C2 C3 C1 H2B 0.2314 0.3729 0.5059 23 0.990 0.000 C2 C3 C1 H3A 0.3972 0.3732 0.7416 23 0.990 0.000 C3 C4 C2 H3B 0.3972 0.1268 0.7416 23 0.990 0.000 C3 C4 C2 H4 0.7637 0.2500 0.6367 83 0.840 0.000 O4B C4 H4 H24 0.6481 0.2500 -0.0353 43 0.950 0.000 C24 C25 N23 H25 0.6462 0.2500 0.2389 43 0.950 0.000 C25 C24 N21 H26A 1.2238 0.2500 0.0647 33 0.980 0.000 C26 C22 H26A H26B 1.2271 0.1268 0.2188 33 0.980 0.000 C26 C22 H26A H26C 1.2271 0.3732 0.2188 33 0.980 0.000 C26 C22 H26A H21 0.9371 0.2500 0.3489 43 0.880 0.000 N21 C22 C25 H23 0.9406 0.2500 -0.0738 43 0.880 0.000 N23 C22 C24 06skc0029p21m in P2(1)/m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.07711 0.25000 0.64671 0.50000 0.01414 0.02103 0.01835 0.00000 0.00256 0.00000 0.01780 0.00332 0.00027 0.00000 0.00025 0.00000 0.00117 0.00116 0.00107 0.00000 0.00087 0.00000 0.00048 C2 0.23312 0.25000 0.57103 0.50000 0.01533 0.03026 0.01593 0.00000 0.00324 0.00000 0.02040 0.00336 0.00027 0.00000 0.00024 0.00000 0.00117 0.00130 0.00105 0.00000 0.00086 0.00000 0.00051 H2A 0.23140 0.12709 0.50590 0.50000 0.02448 0.00000 0.00000 H2B 0.23140 0.37291 0.50590 0.50000 0.02448 0.00000 0.00000 C3 0.39353 0.25000 0.67658 0.50000 0.01380 0.02620 0.01529 0.00000 0.00375 0.00000 0.01827 0.00331 0.00027 0.00000 0.00023 0.00000 0.00110 0.00123 0.00103 0.00000 0.00083 0.00000 0.00049 H3A 0.39716 0.37321 0.74157 0.50000 0.02192 0.00000 0.00000 H3B 0.39716 0.12679 0.74157 0.50000 0.02192 0.00000 0.00000 C4 0.54297 0.25000 0.59337 0.50000 0.01521 0.02056 0.01629 0.00000 0.00273 0.00000 0.01729 0.00324 0.00027 0.00000 0.00023 0.00000 0.00116 0.00115 0.00107 0.00000 0.00087 0.00000 0.00049 O1A -0.05845 0.25000 0.55682 0.50000 0.01186 0.04186 0.01809 0.00000 0.00261 0.00000 0.02388 0.00233 0.00019 0.00000 0.00017 0.00000 0.00084 0.00105 0.00080 0.00000 0.00061 0.00000 0.00041 O1B 0.08541 0.25000 0.78505 0.50000 0.01806 0.03617 0.01489 0.00000 0.00443 0.00000 0.02284 0.00234 0.00020 0.00000 0.00017 0.00000 0.00087 0.00099 0.00079 0.00000 0.00063 0.00000 0.00040 O4A 0.53651 0.25000 0.45872 0.50000 0.01840 0.04527 0.01573 0.00000 0.00288 0.00000 0.02641 0.00239 0.00020 0.00000 0.00017 0.00000 0.00090 0.00112 0.00081 0.00000 0.00063 0.00000 0.00043 O4B 0.68313 0.25000 0.68621 0.50000 0.01283 0.04018 0.01773 0.00000 0.00349 0.00000 0.02344 0.00229 0.00019 0.00000 0.00017 0.00000 0.00083 0.00105 0.00081 0.00000 0.00065 0.00000 0.00041 H4 0.76371 0.25000 0.63669 0.50000 0.04967 0.00000 0.00964 C22 1.00250 0.25000 0.14518 0.50000 0.02600 0.01847 0.01801 0.00000 0.00536 0.00000 0.02061 0.00350 0.00029 0.00000 0.00024 0.00000 0.00133 0.00115 0.00112 0.00000 0.00094 0.00000 0.00052 C24 0.74213 0.25000 0.03901 0.50000 0.02214 0.03165 0.02136 0.00000 0.00537 0.00000 0.02482 0.00376 0.00030 0.00000 0.00026 0.00000 0.00133 0.00139 0.00118 0.00000 0.00095 0.00000 0.00055 H24 0.64812 0.25000 -0.03527 0.50000 0.02979 0.00000 0.00000 C25 0.74111 0.25000 0.18771 0.50000 0.02364 0.02636 0.02226 0.00000 0.00705 0.00000 0.02373 0.00365 0.00031 0.00000 0.00025 0.00000 0.00131 0.00127 0.00119 0.00000 0.00095 0.00000 0.00053 H25 0.64619 0.25000 0.23888 0.50000 0.02847 0.00000 0.00000 C26 1.18556 0.25000 0.16342 0.50000 0.02826 0.03265 0.02309 0.00000 0.00339 0.00000 0.02799 0.00378 0.00031 0.00000 0.00027 0.00000 0.00142 0.00146 0.00123 0.00000 0.00099 0.00000 0.00058 H26A 1.22384 0.25000 0.06468 0.50000 0.04199 0.00000 0.00000 H26B 1.22706 0.12683 0.21883 0.50000 0.04199 0.00000 0.00000 H26C 1.22706 0.37317 0.21883 0.50000 0.04199 0.00000 0.00000 N21 0.90360 0.25000 0.25203 0.50000 0.02991 0.02592 0.01451 0.00000 0.00479 0.00000 0.02328 0.00304 0.00025 0.00000 0.00021 0.00000 0.00120 0.00108 0.00096 0.00000 0.00082 0.00000 0.00047 H21 0.93712 0.25000 0.34885 0.50000 0.04787 0.00000 0.00920 N23 0.90566 0.25000 0.01457 0.50000 0.02388 0.02727 0.01591 0.00000 0.00597 0.00000 0.02205 0.00292 0.00024 0.00000 0.00021 0.00000 0.00111 0.00110 0.00094 0.00000 0.00080 0.00000 0.00046 H23 0.94062 0.25000 -0.07385 0.50000 0.05302 0.00000 0.00979 Final Structure Factor Calculation for 06skc0029p21m in P2(1)/m Total number of l.s. parameters = 88 Maximum vector length = 511 Memory required = 1780 / 22995 wR2 = 0.1076 before cycle 9 for 1184 data and 0 / 88 parameters GooF = S = 1.091; Restrained GooF = 1.091 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0325 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0480 for 918 Fo > 4sig(Fo) and 0.0687 for all 1184 data wR2 = 0.1076, GooF = S = 1.091, Restrained GooF = 1.091 for all data Occupancy sum of asymmetric unit = 7.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0210 0.0184 0.0140 C1 0.0303 0.0168 0.0142 C2 0.0262 0.0163 0.0123 C3 0.0206 0.0166 0.0148 C4 0.0419 0.0181 0.0117 O1A 0.0362 0.0190 0.0133 O1B 0.0453 0.0185 0.0155 O4A 0.0402 0.0180 0.0122 O4B 0.0265 0.0185 0.0169 C22 0.0317 0.0241 0.0188 C24 0.0266 0.0264 0.0182 C25 0.0326 0.0283 0.0231 C26 0.0300 0.0259 0.0140 N21 0.0273 0.0248 0.0141 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.022 0.036 0.049 0.066 0.086 0.107 0.142 0.196 1.000 Number in group 133. 109. 116. 118. 120. 114. 118. 120. 118. 118. GooF 1.257 0.984 1.277 1.016 1.126 1.030 1.006 0.971 0.963 1.193 K 6.529 1.419 1.604 1.104 0.991 1.014 1.001 0.996 1.009 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.98 1.05 1.15 1.33 1.69 inf Number in group 119. 123. 115. 117. 120. 117. 117. 119. 119. 118. GooF 0.953 1.054 1.157 1.072 0.909 0.972 0.899 1.134 1.089 1.535 K 1.042 1.114 1.057 1.071 0.978 0.998 1.005 1.001 1.031 0.978 R1 0.179 0.167 0.130 0.125 0.065 0.062 0.035 0.043 0.032 0.037 Recommended weighting scheme: WGHT 0.0325 0.2661 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) 0 0 3 17.09 4.66 6.13 0.033 2.98 0 3 6 13.36 0.16 6.00 0.006 1.23 -1 1 1 602.13 722.45 3.99 0.409 4.57 -2 0 2 203.66 245.01 3.35 0.238 3.21 0 1 2 3745.40 4281.53 3.24 0.995 3.68 3 0 0 23.27 12.56 3.18 0.054 2.69 2 1 5 6.61 12.68 3.05 0.054 1.52 4 1 0 358.84 309.92 3.04 0.268 1.93 2 0 2 34.23 24.07 2.96 0.075 2.82 8 2 3 7.04 0.59 2.82 0.012 0.89 -6 0 3 6.74 1.63 2.80 0.019 1.29 -3 3 5 2.44 0.02 2.73 0.002 1.28 0 1 6 0.05 3.38 2.72 0.028 1.45 1 0 1 1788.23 2053.72 2.70 0.689 5.64 -1 0 3 90.85 74.30 2.68 0.131 2.92 2 6 6 20.00 9.87 2.61 0.048 0.84 -7 5 2 7.64 0.08 2.60 0.004 0.86 -3 1 5 6.13 2.83 2.58 0.026 1.54 -7 0 5 15.26 24.79 2.58 0.076 1.03 -8 2 8 -0.74 5.30 2.53 0.035 0.78 -5 3 9 10.99 17.87 2.37 0.064 0.83 -7 2 9 139.17 114.20 2.34 0.162 0.78 -2 1 1 7.59 4.13 2.34 0.031 3.33 -8 0 5 61.82 80.41 2.28 0.136 0.93 0 4 3 4.42 1.74 2.27 0.020 1.43 2 1 4 31.25 24.14 2.27 0.075 1.78 -2 5 8 15.44 7.36 2.26 0.041 0.85 3 0 3 204.84 176.40 2.25 0.202 1.88 3 7 0 3.96 0.24 2.25 0.007 0.88 4 5 4 6.63 2.38 2.24 0.023 0.96 -6 1 5 23.61 31.07 2.22 0.085 1.13 -10 2 4 56.79 34.75 2.21 0.090 0.77 -7 1 4 125.28 145.96 2.20 0.184 1.07 1 0 10 1.89 6.50 2.20 0.039 0.88 0 3 5 22.79 17.10 2.19 0.063 1.38 2 2 10 4.26 0.01 2.18 0.002 0.82 8 1 1 29.63 39.27 2.18 0.095 0.98 -9 2 3 25.72 14.30 2.17 0.057 0.86 1 3 0 251.73 281.08 2.16 0.255 2.09 -2 1 3 200.90 178.78 2.15 0.203 2.38 6 4 1 5.20 1.44 2.15 0.018 1.02 -8 0 7 9.11 0.00 2.14 0.001 0.85 -3 2 5 20.08 14.76 2.13 0.058 1.43 -5 5 5 8.74 15.41 2.13 0.060 0.91 5 4 3 64.32 52.77 2.09 0.110 1.04 8 4 0 18.95 8.39 2.08 0.044 0.86 4 1 1 62.30 51.92 2.07 0.110 1.84 -3 5 7 38.07 28.77 2.07 0.082 0.89 3 1 7 811.87 740.36 2.06 0.414 1.08 7 0 7 15.20 6.96 2.06 0.040 0.81 Bond lengths and angles C1 - Distance Angles O1B 1.2397 (0.0026) O1A 1.2827 (0.0027) 124.47 (0.20) C2 1.5179 (0.0030) 120.75 (0.19) 114.78 (0.19) C1 - O1B O1A C2 - Distance Angles C3 1.5140 (0.0031) C1 1.5179 (0.0030) 115.01 (0.18) H2A 0.9900 108.52 108.52 H2B 0.9900 108.52 108.52 107.52 C2 - C3 C1 H2A C3 - Distance Angles C4 1.5098 (0.0029) C2 1.5140 (0.0031) 111.97 (0.18) H3A 0.9900 109.22 109.22 H3B 0.9900 109.22 109.22 107.91 C3 - C4 C2 H3A C4 - Distance Angles O4A 1.2077 (0.0025) O4B 1.3258 (0.0026) 123.81 (0.20) C3 1.5098 (0.0029) 124.42 (0.20) 111.76 (0.18) C4 - O4A O4B O1A - Distance Angles C1 1.2827 (0.0027) O1A - O1B - Distance Angles C1 1.2397 (0.0026) O1B - O4A - Distance Angles C4 1.2077 (0.0025) O4A - O4B - Distance Angles C4 1.3258 (0.0026) H4 0.8400 109.47 O4B - C4 C22 - Distance Angles N23 1.3297 (0.0030) N21 1.3327 (0.0029) 107.12 (0.21) C26 1.4793 (0.0034) 124.96 (0.20) 127.92 (0.21) C22 - N23 N21 C24 - Distance Angles C25 1.3410 (0.0031) N23 1.3781 (0.0031) 106.87 (0.21) H24 0.9500 126.57 126.57 C24 - C25 N23 C25 - Distance Angles C24 1.3410 (0.0031) N21 1.3750 (0.0031) 106.95 (0.20) H25 0.9500 126.52 126.52 C25 - C24 N21 C26 - Distance Angles C22 1.4793 (0.0034) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B N21 - Distance Angles C22 1.3327 (0.0029) C25 1.3750 (0.0031) 109.53 (0.19) H21 0.8800 125.23 125.23 N21 - C22 C25 N23 - Distance Angles C22 1.3297 (0.0030) C24 1.3781 (0.0031) 109.52 (0.19) H23 0.8800 125.24 125.24 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.70 2.535(2) 173.0 O4B-H4...O1A_$1 0.88 1.87 2.724(2) 163.2 N21-H21...O1A_$1 0.88 1.84 2.684(2) 159.3 N23-H23...O1B_$2 FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0685 for 1184 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.1608 0.2500 0.6106 [ 0.73 A from C2 ] Deepest hole -0.24 at 0.8386 0.2054 0.1401 [ 0.99 A from C25 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1816 / 12751 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1608 0.2500 0.6106 0.50000 0.05 0.28 0.73 C2 0.79 C1 1.41 H2A 1.41 H2B Q2 1 1.4003 0.2500 0.2356 0.50000 0.05 0.28 1.61 H26B 1.61 H26C 1.61 H26B 1.61 H26C Q3 1 0.0002 0.2500 0.8236 0.50000 0.05 0.27 0.82 O1B 1.10 H23 1.79 C1 1.97 N23 Q4 1 0.4400 0.2500 0.3969 0.50000 0.05 0.23 0.90 O4A 1.86 C4 2.22 H2A 2.22 H2B Q5 1 0.4671 0.2500 0.6319 0.50000 0.05 0.22 0.75 C4 0.76 C3 1.44 H3A 1.44 H3B Q6 1 1.2357 0.2500 -0.0987 0.50000 0.05 0.21 1.49 H26A 1.51 O1B 2.22 H3A 2.22 H3B Q7 1 0.8771 0.2500 0.7376 0.50000 0.05 0.20 1.21 H4 1.59 O4B 1.70 O1B 1.71 H23 Q8 1 1.3122 0.2500 0.3595 0.50000 0.05 0.20 1.58 H26B 1.58 H26C 1.58 H26B 1.58 H26C Q9 1 0.6737 0.2500 0.4394 0.50000 0.05 0.20 1.15 O4A 1.79 H25 1.83 H4 1.85 C4 Q10 1 0.0970 0.2500 0.9223 0.50000 0.05 0.19 1.23 O1B 1.28 H23 1.54 H26A 1.86 N23 Shortest distances between peaks (including symmetry equivalents) 4 8 1.05 3 10 1.11 6 10 1.17 3 7 1.19 2 8 1.40 2 4 1.45 4 9 1.89 3 6 1.96 4 5 2.10 7 10 2.28 1 3 2.46 1 5 2.48 5 9 2.57 1 6 2.61 5 8 2.61 2 9 2.70 1 7 2.71 1 8 2.71 1 10 2.92 8 9 2.94 7 9 2.97 Time profile in seconds ----------------------- 0.06: 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 0.02: Analyse other restraints etc. 0.28: 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 0.33: Structure factors and derivatives 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0029p21m finished at 15:55:53 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++